Pre-Construction Background Air Monitoring Quality Assurance Project Plan (QAPP)

Pre-Construction Background Air Monitoring Quality Assurance Project Plan (QAPP)
Air Monitoring Program
Quality Assurance Project Plan
Area 1, Phase 1 Development
Version 1
Baltimore Works Site
Baltimore, Maryland
March 2014
By:
Environmental Resources Management Inc.
Harbor Point Development LLC
For:
U.S. Environmental Protection Agency – Region III
Maryland Department of the Environment
APPROVAL AND SIGNATURE PAGE FOR THE AIR MONITORING PROGRAM
QUALITY ASSURANCE PROJECT PLAN AREA 1, PHASE I DEVELOPMENT,
VERSION 1, FEBRUARY 24, 2014.
Approval
Date
Project Manager
(Harbor Point Development LLC)
Jonathan Flesher
Project Manager
(Honeywell International)
Chris French
Project Manager
(ERM, Inc.)
Darren Quillen, P.E.
Project Quality Assurance Manager
(ERM, Inc.)
Larry Hottenstein
Partner-in-Charge
(ERM, Inc.)
Leonard Rafalko
A signed copy of this Air Monitoring Program Quality Assurance Project Plan is stored in
the Harbor Point Development office. Please see the contact in the Acknowledgement
Section.
i
REVISION HISTORY FOR THE AIR MONITORING PROGRAM QUALITY
ASSURANCE PROJECT PLAN AREA 1, PHASE I DEVELOPMENT, VERSION 1,
FEBRUARY 24, 2014
Date
Revision Description
ii
Initials
TABLE OF CONTENTS
TABLE OF CONTENTS
III
1.0
PROJECT MANAGEMENT
1
1.1
ROLES AND RESPONSIBILITIES
1
1.2
PROJECT BACKGROUND, OVERVIEW, AND INTENDED USE OF DATA
5
1.3
DATA QUALITY OBJECTIVES
1.3.1 State the Problem
1.3.2 Identify the Decision
1.3.3 Identify Inputs to the Decision
1.3.4 Define the Site Boundaries
1.3.5 Develop a Decision Rule
1.3.6 Specify Limits on Decision Errors
1.3.7 Optimize the Sampling Design
6
7
7
8
11
12
13
14
1.4
MEASUREMENT PERFORMANCE CRITERIA
15
2.0
SPECIAL TRAINING REQUIREMENTS AND CERTIFICATION
17
2.1
DOCUMENTATION AND RECORDS REQUIREMENTS
17
3.0
DATA ACQUISITION
19
3.1
SAMPLE COLLECTION PROCEDURES, DESIGN, & SAMPLING TASKS
OVERVIEW
3.1.1 Pre-Construction Air Monitoring
3.1.2 Construction Air Monitoring
19
19
22
3.2
SAMPLING PROCEDURES AND REQUIREMENTS
26
3.3
SAMPLING HANDLING, CUSTODY PROCEDURES, AND
DOCUMENTATION
27
3.4
ANALYTICAL METHOD REQUIREMENTS
30
3.5
FIELD QUALITY CONTROL REQUIREMENTS
30
3.6
FIELD INSTRUMENT/EQUIPMENT CALIBRATION AND MAINTENANCE
REQUIREMENTS
30
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3.7
LABORATORY QUALITY CONTROL REQUIREMENTS
33
3.8
DATA MANAGEMENT REQUIREMENTS
34
4.0
ASSESSMENTS
4.1.1 Sampling Program Design Execution
4.1.2 Sample Collection Procedures
4.1.3 Sample Handling
4.1.4 Quantitative Field Data
4.2.1 Laboratory Data Review and Reduction
4.2.2 Laboratory Data Review and Validation
36
36
36
37
37
37
38
4.3
AUDITS OF DATA QUALITY
4.3.1 Performance Audits
4.3.2 System Audits
38
39
40
4.4
SURVEILLANCE OF OPERATIONS
41
4.5
ASSESSMENT OF DATA QUALITY
4.5.1 Field Data Quality
4.5.2 Laboratory Data Reduction
42
42
44
4.6
QUALITATIVE AND QUANTITATIVE COMPARISONS TO ACCEPTANCE
CRITERIA
4.6.1 Precision
4.6.2 Accuracy
4.6.3 Representativeness
4.6.4 Comparability
4.6.5 Completeness
4.6.6 Sensitivity (Method Detection Limit)
45
45
46
46
47
47
47
4.7
INTERIM ASSESSMENTS OF DATA QUALITY
48
5
REVIEW, EVALUATION OF USABILITY AND REPORTING REQUIREMENTS49
5.1
DATA VERIFICATION AND VALIDATION TARGETS AND METHODS
49
5.3
POTENTIAL LIMITATIONS ON DATA INTERPRETATION
52
5.4
RECONCILIATION WITH PROJECT REQUIREMENTS
5.4.1 Conduct Preliminary Data Review
5.4.2 Draw Conclusions from the Data
53
53
53
5.5
REPORTS TO MANAGEMENT
5.5.1 Daily Data Summary Tables
53
53
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5.5.2
5.5.3
5.5.4
5.5.5
Event Logs
Data Quality Assessment Reports
Performance Evaluation and Audit Reports
Summary Data Reports
53
54
54
54
LIST OF TABLES
1
Roles and Responsibilities
2
Measurement Quality Objectives
3.
Records and Storage Locations
4
Pre-construction Monitoring Samples
5
Construction Monitoring Samples
6
Field Calibration, Testing, and Inspection
7
Field Equipment Maintenance, Testing, and Inspection
LIST OF FIGURES
1
Project Organization
2
Project Area
3
Pre-construction Air Monitoring Locations
4
Construction Air Monitoring Locations
5
Data Management Process
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LIST OF APPENDICES
A
Sampling and Analysis Plans (Pre-construction SAP attached;
Construction SAP to be prepared and amended to the QAPP)
B
Field Sampling Method SOP
B1.
Field Sampling Protocol and Standard Operating Procedure –
Real-Time Air Sampling for Total Particulate Matter in Ambient Air
B2.
Field Sampling Protocol and Standard Operating Procedure –
Sampling of Hexavalent Chromium in Ambient Air
C
Laboratory Analytical Method SOP
D
Standard Operating Procedure for Response Actions and Notifications
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LIST OF ACRONYMS
BTV – Background Threshold Value
CFR – Code of Federal Regulations
CL – Confidence Limit
COC – Chain of Custody
CrVI – Hexavalent Chromium
° C – Degrees Celsius
° F – Degrees Fahrenheit
DQO – Data Quality Objectives
EPA – U.S. Environmental Protection Agency
ERG – Eastern Research Group
ERS – Environmental Remediation System
IDC - Initial Demonstration of Capability
Lpm – Liters per Minute
M3 – Cubic Meters
MDE – Maryland Department of the Environment
µg - Microgram
mg – Milligram
ŋg – Nanogram
PAM - Perimeter Air Monitoring
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LIST OF ACRONYMS (continued)
PM – Particulate Matter
QA – Quality Assurance
QAPP - Quality Assurance Project Plan
QC – Quality Control
SAP – Sampling and Analysis Plan
SOP – Standard Operating Procedures
SSO – Site Safety Officer
Total PM – Total Particulate Matter
µg – Microgram
µm - Micron
USL – Upper Simultaneous Limit
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DOCUMENT DISTRIBUTION LIST
QAPP Recipient
Project Role
Organization
Address / E-mail / Phone
Russell Fish
Project Coordinator
EPA Region 3
Office of Remediation 3LC20
1650 Arch Street
Philadelphia, PA 19103-2029
[email protected]
(215) 814-3226
Ruth Prince
Technical Lead
EPA Region 3
Office of Technical and
Administrative Support 3LC10
1650 Arch Street
Philadelphia, PA 19103-2029
[email protected]
(215) 814-3118
Edward Dexter
Project Coordinator
MDE
Solid Waste Program
1800 Washington Boulevard,
Suite 605
Baltimore, MD 21230-1719
[email protected]
(410) 537-3315
Mark Mank
Technical Lead
MDE
Jonathan Flesher
Project Manager
Harbor Point
Development
LLC (HPD)
Chris French
Project Manager
Honeywell
International
Julie Swift
Laboratory Program
Manager
Eastern Research
Group. Inc.
(ERG)
Darren Quillen
Project Manager
Environmental
Resources
Management,
AIR MONITORING PROGRAM, QUALITY ASSURANCE PROJECT PLAN
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Solid Waste Program
1800 Washington Boulevard,
Suite 605
Baltimore, MD 21230-1719
[email protected]
(410) 537-3437
1300 Thames Street
Suite 10
Baltimore, MD 21231
[email protected]
(410) 332-1100
101 Columbia Road
Morristown, NJ 07960
[email protected]
(973) 455-4131
601 Keystone Park Drive
Suite 700
Morrisville, NC 27560
[email protected]
(919) 468-7924
200 Harry S Truman Parkway,
Suite 400
Annapolis, Maryland 21401
[email protected]
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Inc. (ERM)
Larry Hottenstein
Quality Assurance
Manager
ERM
Jeff Boggs
Technical Lead
ERM
AIR MONITORING PROGRAM, QUALITY ASSURANCE PROJECT PLAN
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HARBOR POINT DEVELOPMENT LLC
(410) 972-0234
2875 Michelle Drive
Suite 200
Irvine, CA 92606
[email protected]
(949) 623-4685
75 Valley Stream Parkway
Suite 200
Malvern, PA 19355
[email protected]
(443) 803-8495
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1.0
PROJECT MANAGEMENT
The project consists of air monitoring before and during construction at
the Harbor Point Area 1, Phase1 Development site. The QAPP outline
and format are consistent with the policies and guidance specified in the
EPA Guidance on Quality Assurance Project Plans (CIO 2106-G-05 QAPP),
EPA, 2012. The QAPP presents the rationale and scope of work
associated with field activities (e.g., sample types, sample locations), the
project data quality objectives, protocols for collecting samples, field and
laboratory analytical procedures, quality assurance/quality control
(QA/QC) procedures, data quality evaluation criteria, and procedures for
documenting field and laboratory methods so that data are technically
and legally defensible.
1.1
ROLES AND RESPONSIBILITIES
The project team will consist of personnel from HPD, ERM, and Eastern
Research Group (ERG). ERG has been selected to perform the hexavalent
chromium (CrVI) analysis. An independent third-party data validator,
Laboratory Data Consultants, Inc. (LDC), will validate the data collection,
including 40% raw data re-calculation. The following paragraphs describe
the major positions and responsibilities of the team along with the
approach to quality assurance management. The EPA is the lead
regulatory agency for this program with key input from the MDE’s Air
and Radiation Program. Key project personnel and regulatory personnel
and their responsibilities for QA activities are described below. The
Project Organization chart (Figure 1) presents the lines of communication
and data flow between the individuals listed below on Table 1.
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Table 1. Roles and Responsibilities
Name
Jonathan
Flesher
Lenny Rafalko
Darren
Quillen
Title/Role
Project
Manager
Partner-inCharge
Project
Manager
Organizational
Affiliation
HPD
ERM
ERM
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Responsibilities
•
Oversees all project activities.
•
Directs the scope of work to the
ERM PM.
•
Reviews and approves all
documents and coordinate
transmittal of documents to
appropriate parties for review.
•
Communicates with stakeholders
regarding project activities.
•
Oversees entire program for ERM.
•
Reviews all final deliverables and
invoices.
•
Seeks HPD feedback on
performance of project managers.
•
Addresses program-level issues.
•
Reports to ERM Partner-in-Charge
(Leonard Rafalko) and HPD
(Jonathan Flesher)
•
Directs ERM Field Manager and
subcontractors.
•
Communicates questions or issues
to Agency leads (Ed Dexter, MDE
and Russell Fish, EPA)
•
Ensures that assigned staff has
been trained in SOP
implementation.
•
Ensures that all key decisions and
project deliverables are subjected
to independent technical review
by qualified personnel within the
time frame of the project schedule.
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Name
Larry
Hottenstein
Title/Role
QA/QC
Manager
Organizational
Affiliation
ERM
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Responsibilities
•
Monitor subcontractor (CrVI
analysis) for compliance with both
project and data quality
requirements records, costs, and
progress of the work and re-plan
and re-schedule work tasks as
appropriate.
•
Ensure and document that QC
checks on field equipment are
performed according to schedule
and meet acceptance criteria, and
the QA/QC
•
Resolves field QA/QC issues.
•
Audit sample preservation,
handling, transport, and custody
procedures throughout the project.
•
Review and approve all data
reduction and reporting
procedures for inclusion in
deliverables.
•
Conduct Field audits.
•
Review and respond to field audit
assessment findings, determine
the root cause for any
nonconformance, confer with the
ERM PM and Partner in Charge
on the steps to be taken for
correction, and ensure that
procedures are modified to reflect
the corrective action and are
distributed to all field personnel,
including subcontractors.
•
Report QA and any procedural
problems to the ERM PM and
Partner in Charge
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Name
Jeff Boggs
Charles
McClellan
Title/Role
Technical
Lead/ Field
Manager
Field
Engineer
Organizational
Affiliation
ERM
ERM
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Responsibilities
•
Provide technical support to
ERM’s PM, QA Manager, and
Field Engineer as needed.
•
Reports to ERM PM.
•
Prepares and implements this
QAPP and deliverables.
•
Ensures data collection activities
are consistent with approved SAP,
SOP and QAPP requirements.
•
Oversees evaluation of data
received from the laboratory in
accordance with the project
requirements.
•
Prepares or oversees the
preparation of portions of the
reports that summarize data
results and present conclusions.
•
Performs monitoring and collects
samples according to project
approved SAPs, SOPs and this
QAPP.
•
Reports to ERM Field Manager (if
Field Manager not available,
report to ERM PM).
•
Communicates any problems or
deviations from project plans to
ERM Field Manager.
•
Ensures that all data collection and
handling activities comply with
applicable SOPs, including audits
conducted in the presence of
Agency personnel.
•
Prepares and maintains field
forms, notebooks, and equipment.
•
Implements technical procedures
applicable to tasks.
•
Inspects and accepts supplies and
consumables.
•
Coordinates and schedules sample
shipment to analytical laboratory
to meet holding times and
analytical procedure
specifications.
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Name
Julie Swift
1.2
Title/Role
Project
Manager
Organizational
Affiliation
ERG
Responsibilities
•
Reviews and implements
analytical laboratory elements of
this QAPP with regards to the
CrVI analysis.
•
Manages analytical chemists to
complete the sample analyses
selected in this QAPP, according
to the approved methods.
•
Monitors, reviews, and documents
the quality of all analytical
chemistry work performed by
ERG under this QAPP.
•
Oversees management of
analytical data.
•
Transmits completed data
packages to the ERM Quality
Manager
•
Promptly informs the ERM’s
Quality Manager of any laboratory
analytical problems, data quality
issues, or delays in sample
analysis.
•
Promptly responds to any data
quality issues identified through
the independent data validation
process.
PROJECT BACKGROUND, OVERVIEW, AND INTENDED USE OF
DATA
The Harbor Point, Area 1, Phase 1 Development will occur at a location
(the site) that was formerly a chromium chemical manufacturing facility.
The site is located on a peninsula on the northeast shore of the Patapsco
River of the Inner Harbor, in the Fells Point section of Baltimore City,
Maryland. The historical manufacturing processes at the site resulted in
chromium impacts to soil and groundwater. The original buildings and
associated infrastructure have been removed from the site, and a number of
remedial actions are on-going. An Environmental Remediation System
(ERS) is maintained and operated by Honeywell International Inc.
(Honeywell) to contain CrVI -impacted ground water and control the
potential for human exposure to affected soil in “Area 1” of the site
(Figure 2). Area 1 was the principal site of Honeywell’s Baltimore Works
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Facility where chromium ore was processed from 1845 to 1985. The ERS
consists of a Multimedia cap (MMC), Hydraulic barrier, Head
Maintenance System (HMS), a ground water storage and transfer system,
and Outboard Embankment. The HMS maintains an inward ground
water gradient to mitigate the migration of chromium-impacted ground
water from the site.
The primary concern addressed by this Air Monitoring Program QAPP is
the potential for particulates containing CrVI to be distributed on-site and
off-site during the period of construction that involves the disturbance of
contaminated materials below the MMC. CrVI is considered by the EPA
to be a known human carcinogen by the inhalation route of exposure
(EPA 2013). Inhalation of CrVI dusts is also associated with non-cancer
toxicity.
Because of the dynamic nature of dust-disturbing activities during
construction, providing real time information on concentration levels of
particulates to project personnel during construction is necessary in order
that dust-generating activities on site can be appropriately controlled.
Real-time instrumentation is available to measure ambient concentrations
of total particulate matter (Total PM), but such instrumentation is not
available for measuring CrVI concentrations in real-time. Air samples for
measuring CrVI concentrations require laboratory analysis.
To address the data objectives, data will be collected prior to construction,
and then throughout the construction period that involves disturbance of
the surface immediately below the synthetic layers of the existing MMC in
Area 1. The intended use of the air monitoring data is to 1) obtain
empirical pre-construction data to establish the Total PM action level and
CrVI background concentration and 2) to measure/monitor Total PM and
CrVI during construction to ensure the efficiency of on-going dustsuppression activities such that dust control measures can be
supplemented, as appropriate.
The pre-construction air monitoring study will be conducted in March
2014. Construction monitoring will be performed for approximately six
(6) months commencing in April 2014.
1.3
DATA QUALITY OBJECTIVES
Data quality objectives (DQOs) are an integrated set of qualitative and
quantitative decision statements that define data quality requirements
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based on the end use of the data. The EPA has developed a seven-step
process (shown in bold italics below) to clarify study objectives, define the
appropriate type of data, and specify tolerable levels of potential decision
errors that will be used as the basis for establishing the quality and
quantity of data needed to support decisions. The DQO process is
described in detail in the EPA guidance document, Guidance on Systematic
Planning Using the Data Quality Objectives Process EPA QA/G-4 (February
2006).
1.3.1
State the Problem
The problem being addressed is to ensure that representative and accurate
real-time particulate and airborne CrVI data are collected to define the
pre-construction particulate population reflective of routine background
conditions. This data will be used to generate Background Threshold
Values (BTVs) that in turn will be used to ensure that the site perimeter
and work zones are accurately monitored during construction to control
any potential release in a timely manner.
1.3.2
Identify the Decision
Is the pre-construction dataset (real-time Total PM and airborne CrVI
concentrations) accurate and representative of routine city traffic
conditions?
1. Possible Outcome – Collected data shows acceptable variability
and expected airborne concentrations.
a. No Action.
2. Possible Outcome - Collected pre-construction data shows
extreme concentration variability.
a. Possible Actions –
i. Option - Accept data as representative of urban setting.
ii. Option – Confirm the precision estimate between
duplicate instruments/ co-located samplers meet the
established RPD precision criteria.
iii.
Option - Review field logs to determine if there were any
conditions (unusual traffic, extreme weather, etc.) that
could explain the variability.
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iv.
v.
Option – Conduct 100% raw data validation.
Option - Use additional statistical analysis to remove
significant outliers and evaluate the influence on data.
3. Possible Outcome - Collected pre-construction data shows
unexpected elevated airborne concentrations.
a. Possible Actions –
1.3.3
i.
Option - Accept data as representative of urban setting.
ii.
Option – Confirm the precision estimate between
duplicate instruments/ co-located samplers meet the
established RPD precision criteria.
iii.
Option - Review field logs to determine if there were any
conditions (unusual traffic, extreme weather, etc.) that
could explain the unexpected elevated airborne
concentrations.
iv.
Option – Conduct 100% raw data validation.
v.
Option - Use additional statistical analysis to remove
significant outliers and evaluate the influence on data.
Identify Inputs to the Decision
This section summarizes the variables to be measured, the quality
assurance/quality control mechanisms in place, measurement quality
objectives, data validation and audit results, and statistical analyses to be
performed to resolve the decision (Section 1.3.2, above).
Variables to be Measured
Variables to be measured include:
•
24-hour Total PM concentrations;
•
24-hour particulate CrVI concentrations; and
•
Observations of ambient conditions and activities in the
vicinity of each monitoring station.
Quality Assurance/Quality Control Mechanisms
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Quality assurance/quality control (QA/QC) mechanisms are
described in detail in Sections 2.5 through 2.7. QA/QC
mechanisms include:
•
Accuracy, precision, and sensitivity of analysis – review the
MQOs are met;
•
Representativeness and comparability of field data;
•
Sample documentation (including field and laboratory
records);
•
Maintenance and calibration of field and laboratory
equipment;
•
Analytical procedures for CrVI that comply with ASTM
Standard Test Method D7614-12 Determination of Total
Suspended Particulate (TSP) Hexavalent Chromium in
Ambient Air Analyzed by Ion Chromatography and
Spectrophotometric Measurements; and all of the associated
QA/QC requirements of the method (Laboratory SOP is
included as Appendix C).
•
Review of field and laboratory data by qualified personnel.
Measurement Quality Objectives (MQOs)
MQOs are designed to evaluate and control various phases of the
measurement process to ensure that total measurement uncertainty
is with a range that will meet the DQO requirements. The MQOs
(provided in Table 2) can be defined in terms of the following data
quality indicators. A more detailed description of these MQOs and
how they will be used to control and assess measurement
uncertainty will be described in the following elements of the
QAPP.
•
Precision – a measure of mutual agreement among
individual measurement of the same property usually under
prescribed similar conditions. This is the random
component of error.
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•
Bias – the systematic or persistent distortion of a
measurement process which causes error in one direction.
Bias is determined by estimating the positive and negative
deviation from the true value as a percentage of the true
value.
•
Representativeness – a measure of the degree to which data
accurately and precisely represent a characteristic of
population, parameter variations at a sampling point, a
process condition, or an environmental condition.
•
Detectability – the determination of the low range critical
value of a characteristic that a method-specific procedure
can reliably discern.
•
Completeness – a measure of the amount of valid data
obtained from a measurement system compared to the
amount that was expected to be obtained under correct,
normal conditions.
•
Comparability – a measure of the level of confidence with
which one data set can be compared to another.
Data Validation and Audits
Data validation is discussed in detail in Section 4.1. Audits are discussed
in detail in Section 3.0.
Data validation will include the following:
•
The laboratory will review and reduce the data internally
prior to submitting the data to ERM. Laboratory SOPs for
internal data review procedures are included in the
laboratory’s QAPP.
•
Laboratory data will be reviewed by ERM.
•
ERM will review precision of the DustTrak 8533 data by
assessing results of duplicate monitors at PAM-1.
•
Following receipt of the laboratory report, ERM will send
the sample group QC package data to Laboratory Data
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Consultants, Inc. (LDC), an independent third-party
validator, to perform Level II validation, as described in
EPA’s Guidance on Environmental Data Verification and Data
Validation (2002). The validation process is described in
detail in Section 4.1.
Auditing procedures will include the following:
•
Field performance procedure audits will be conducted
during pre-construction and construction air monitoring by
the ERM QA/QC Manager. Specific attention will be given
to field instrumentation QC, sampling methods, data
collection, sample preservation, and decontamination to
demonstrate compliance with required procedures. Field
instrumentation QC procedures will also be verified,
including measure of co-located precision for DustTrak 8533.
•
Internal laboratory audits should be performed by the
Laboratory QA Manager, Laboratory PM, or qualified
designee annually. Laboratory systems audits may also be
conducted by the ERM QA/QC Officer or qualified
designee. This auditor, in conjunction with the Laboratory
QA Manager, may conduct the systems startup audit to
ensure that all instruments proposed or in use are
appropriate for the given methods and functioning properly.
Laboratory performance may be audited through PE check
samples that contain certified concentrations of target
analytes. Audit procedures are described in detail in Section
3.0.
Statistical Analysis
Laboratory statistics will be performed to assure precision,
accuracy, and sensitivity of the collected CrVI data. These
measures and statistics are discussed in Section 3.4.
1.3.4
Define the Site Boundaries
The target media is air at the site perimeter and at off-site locations
representative of urban conditions. The site physical boundary is the
project property as bounded by the perimeter air monitoring (PAM)
stations as shown on Figure 4. Total PM will be provided real-time at
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1-minute intervals. Particulate CrVI samples will be collected over a
24-hour interval.
The primary practical constraints include:
•
Methods to measure particulate CrVI are limited to analytical
laboratory methods. Particulate CrVI cannot be determined
real-time in the field.
•
Severe weather would create a safety concern and may also
damage equipment and influence the monitoring results.
Sample collection may be delayed if severe weather is
encountered.
•
Samples for particulate CrVI must be stored at 0°C or less.
•
Monitoring locations will require electric power to operate
instruments and sampling pumps.
•
Monitoring locations must have safe access for personnel and
security for instruments and sampling pumps.
The scale of decision for this site is air at the site property boundaries and
urban area vicinity.
1.3.5
Develop a Decision Rule
For this project, the decision is whether the data collected meet quality
requirements and therefore can be accepted as valid representations of
airborne Total PM and particulate CrVI concentrations during preconstruction and during construction. The parameters of interest are the
concentrations of Total PM and particulate CrVI in the air shed at the site
perimeter and in the vicinity of the project. The decision making scale
during pre-construction is a sufficient period of sampling to ensure air
samples representative of various ambient conditions in the vicinity of the
project are collected. The decision making scale during construction is a
rapid response (within 15 minutes) to elevated Total PM concentrations in
the immediate, on-site work area at or above a dust action level (the BTV)
such that construction generated dust will not migrate off site at
concentrations above the BTV.
The expected outcome for pre-construction monitoring is the collection of
valid, representative data with which to calculate BTVs. The outcome of
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the construction monitoring is the collection of valid, representative data
of construction conditions demonstrating that concentrations are at or
below the BTVs and are representative of pre-construction conditions.
Specifically, the project will:
•
Collect Total PM and particulate CrVI data using accurate
methods, including data quality review. Ensure that the
samples are collected using calibrated equipment. Analyze
CrVI concentrations in an EPA-certified laboratory. Ensure that
samples are collected over a range of times when construction
will occur to account for diurnal cycles in urban sources.
Ensure that samples are taken for multiple days to account for
daily variation in weather patterns, urban sources, etc. Ensure
that appropriate quality assurance/quality control measures are
followed to confirm data accuracy and precision; and
•
Collect and analyze Total PM and particulate CrVI using the
same method during construction as for pre-construction
monitoring. Collect real-time Total PM data from locations as
close as safely possible to construction activities and from
locations on the perimeter of the site to ensure any increases in
total PM above the BTV are identified immediately and
corrective measures are implemented.
Hypotheses and decision error is discussed in the following section.
1.3.6
Specify Limits on Decision Errors
The problem statement is to ensure that representative and accurate realtime particulate and airborne CrVI data is collected to define the preconstruction particulate population reflective of routine background
conditions. Collection of acceptable pre-construction total PM and
particulate CrVI concentrations is an estimation problem, as defined in the
EPA guidance document, Guidance on Systematic Planning Using the Data
Quality Objectives Process EPA QA/G-4 (February 2006). For estimation
problems, performance metrics and acceptable levels of uncertainty are
used in place of statistical hypothesis testing and decision errors.
For all data collection, data will be required to meet all the field and
laboratory procedures and quality control requirements in order to be
accepted. For pre-construction, if the data meets all quality goals, it is
considered acceptable. For construction, all data must meet the same
quality goals for pre-construction in order to be acceptable.
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During the construction phase, use of the BTVs to determine whether
particulate CrVI concentrations exceed ambient conditions is a decision
making problem, as defined in the EPA guidance document, Guidance on
Systematic Planning Using the Data Quality Objectives Process EPA QA/G-4
(February 2006). The hypotheses and associated decision errors are:
•
Ho: Total PM concentration is greater than the BTV
o Type II error (false acceptance): Total PM concentration is
identified as greater than the BTV, but is actually less
than or equal to the BTV
•
Ha: Total PM concentration is less than or equal to the BTV
o Type I error (false rejection): Total PM concentration is
identified as less than or equal to the BTV, but is actually
greater than the BTV
Quantitation limits of the error, parameter range, grey region, and
acceptable error levels cannot be determined until the BTV for
background total PM and particulate CrVI concentrations have been
determined.
Collected data must meet all EPA quality requirements and will be
validated according to the guidance provided in EPA Contract Laboratory
Program National Functional Guidelines for Inorganic Superfund Data Review
(January 2010) and ASTM Standard Test Method D7614-12. Air
monitoring data collected during the pre-construction and construction
phases will be validated. Appropriate calibration of equipment during
field activities and during laboratory analysis will be performed (see
Sections 2.6 and 2.7 and Appendices B and C). Limits on decision errors
based on use of the action limit during construction (i.e., addressing false
positives) will be established by the project team during development of
the Construction Air Monitoring Plan.
1.3.7
Optimize the Sampling Design
Air quality data for establishing pre-construction concentrations for total
PM and particulate CrVI will be collected for the range of meteorological
conditions present during a 15-day sampling period at three, fixed
locations. One location will include a duplicate real-time instrument for
Total data and co-located samplers for CrVI (60 CrVI samples collected in
total). Air monitoring during construction will be used to assess on-site
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and off-site Total PM and particulate CrVI concentrations at six (6), fixed
locations (6 CrVI samples per day).
During standard construction hours/days, a minimum of two additional
real-time monitors, only, will be placed in the Work Zone immediately
adjacent to and upwind of construction intrusive activities. The Work
Zone monitors will be set to sound an audible alarm in the event the Total
PM action level is exceeded, providing immediate feedback to workers as
to when dust levels might require additional controls. Work Zone
monitoring will occur on all work days.
1.4
MEASUREMENT PERFORMANCE CRITERIA
The quality of the collected air sampling data must be evaluated and
controlled to ensure that data quality is maintained within the established
acceptance criteria. Measurement quality objectives for the data apply to
both collection of the data (e.g., trip and field blanks) and the analysis
procedures (e.g. lab blanks). The measurement objectives for this project
are as described in the best practice analytical method included as
Appendix C. The analytical method meets specific criteria for precision,
bias, representativeness, minimum detection limits, comparability and
completeness as shown on Table 2. EPA’s definitions for these terms are
provided below (EPA 2009).
Precision - a measure of the agreement among repeated measurements of
the same constituent, usually under prescribed similar conditions
(uncertainty is driven by random error).
Bias - the systematic or persistent distortion of a measurement process
which causes error in one direction (uncertainty is driven by systematic
error).
Representativeness - a measure of the degree to which an observation or a
sample represents the population from which it was drawn.
Detectability - the determination of the low range critical value of a
characteristic that a method-specific procedure can reliably discern.
Completeness - a measure of the amount of valid data obtained from a
measurement system compared to the amount taken.
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Table 2. Measurement Quality Objectives
Compound
Reporting
Units
Precision
(RPD)*
Bias*
Representativeness
Comparability/
Method Selection
Completeness
Method
Detection
Limit
Total
Particulate
Matter
µg/M3
Duplicate
instruments
at one
location
Acceptance
criteria:
RPD < 40%
NA
Pre-construction – air
shed surrounding site
vicinity; Construction
– air shed at perimeter
& surrounding site
vicinity
Direct Read
Instrument
DustTrak 8533;
factory and field
calibrated
Average daily
Total PM
concentration
measurement for
24-hour sampling
day at each
location for 15
monitoring days
1.0 µg/M3
Hexavalent
Chromium
(CrVI)
ng/ M3
Co-located
sample
collection
Acceptance
criteria:
RPD < 20%
25%
Pre-construction – air
shed surrounding site
vicinity; Construction
– air shed at perimeter
& surrounding site
vicinity
ERG-specific
method ERGMOR-063 based
on ASTM Test
Method D7614-12
90% of proposed
samples
0.0078
ng/ml
(0.0036 ng/
M3 based
on 21.6 M3
sample
volume)
Pre-construction
= 4 samples per
24-hour sampling
day for 15
sampling days.
Construction = 6
samples per 24hour sampling
day.
* = These are estimates. The methods do not state the precision or bias.
RPD = Relative percent difference
ASTM = American Society for Testing and Materials
µg/M3 = Micrograms per cubic meter
ng/M3 = Nanograms per cubic meter
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2.0
SPECIAL TRAINING REQUIREMENTS AND CERTIFICATION
Each analyst analyzing samples under this project will have an Initial
Demonstration of Capability (IDC) on file for the analysis of Cr(VI) in
ambient air at the laboratory that is available for inspection upon request.
The personnel performing the field tasks will be able to demonstrate by
training records and documented experience that they can operate,
troubleshoot and maintain the equipment and perform QC checks.
2.1
DOCUMENTATION AND RECORDS REQUIREMENTS
Documentation and records anticipated to be generated during the project
are listed below, along with their storage location:
Table 3. Records and Storage Locations
Record
Storage Location
Sample Collection and Handling Records
Daily per-sample field data sheets
Field (hard copy); Faxed copies scanned
(including DustTrak 8533 readings) (see
and stored weekly in ERM’s office
Section 2.2. & Appendix B for field sheet
(ERM’s Annapolis, Maryland office)
contents; info collected will include field
project file (electronic copy).
equipment maintenance information, see
Sections 2.2 & 2.3)
Field Notebooks
Field (hard copy); Scanned and stored
in ERM’s office project file at the
conclusion of the field work.
Sample COC sheets
Field (hard copy); Faxed copies weekly
scanned and stored in ERM’s office
project file
Sample receipt acknowledgement from the
Electronic copies stored weekly in
laboratory
ERM’s office project file
Field Audit & Corrective Action Reports
Field (hard copy); ERM’s Office project
file (electronic copy)
Field SOPs
Field (hard copy); ERM’s Office project
file (electronic copy)
Analytical Records
Laboratory Sample Management Records
ERG (hard copy & electronic)
Test method raw data & reported results
ERG (hard & electronic), ERM project
file (electronic)
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QA/QC reports (general QC records, MDL
ERG (hard & electronic), ERM project
info, calibration, etc.)
file (electronic)
Test Method SOP
ERG (hard & electronic), ERM project
file (electronic)
DustTrak 8533 data logs
Upload data logs to field computer once
per day (electronic), Backup to ERM’s
Office project within 36 hours of field
upload (electronic) and upload to
project website during construction
within 36 hours of field upload.
Data Assessment Records
Data validation reports
ERM receives electronic copy from third
party data validator & stores electronic
copy
All electronic versions/copies of data and reports will be initially stored
on ERM’s secure server.
Data and reports will be transmitted to HPD, and HPD will supply
records to Honeywell, EPA, and MDE as required.
The results of air sampling during construction will be posted to the
project website (after validation) per agreement between HPD and EPA
and MDE.
The URL for the project website is: http://harborpointbaltimore.info.
Data will be retained on file at ERM for a minimum of one year after the
cessation of air monitoring, and will be readily available for audits and
data verification activities. After one year, hardcopy records and
computer backup electronic media will be discarded.
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3.0
DATA ACQUISITION
This section describes how the project data will be obtained, including the
rationale for the sample design and all field quality controls procedures.
The Sampling and Analysis Plans (Appendix A) and the Standard
Operation Procedures (SOPs) for field sampling methods are provided in
Appendix B. The laboratory SOP is provided in Appendix C.
3.1
SAMPLE COLLECTION PROCEDURES, DESIGN, & SAMPLING
TASKS OVERVIEW
Sample collection is based on a judgmental design (rather than
probability-based). As described in Section 3, sample collection will occur
in two phases – pre-construction and during construction.
3.1.1
Pre-Construction Air Monitoring
Pre-construction air monitoring is intended to provide information on
pre-construction air concentrations of Total PM and CrVI in the area of the
site. As such, one on-site air monitoring location (PAM-1) and two off-site
air monitoring locations (OAM-1 and OAM-2) were selected for sampling,
as shown on Figure 3. OAM-1 will be located approximately 0.5 miles
west of the site at the Baltimore National Aquarium and will be
representative of Baltimore Inner Harbor waterfront background air
conditions. OAM – 2 will be located approximately 1.0 miles north of the
site at the Old Town monitoring station established by MDE and will be
representative of the urban background air conditions. Sampling
equipment at OAM-1 and OAM-2 will be secured within a sturdy
waterproof case with a locking mechanism. A padlock will be used to
secure each case.
Duplicate real-time instruments and co-located CrVI samplers will be
placed at PAM-1 to allow for collection of field duplicate data. The siting
requirements of 40 CFR Part 58, Appendix E will be used as guidance.
Sampler inlets will be placed not less than 2 meters above ground level
and have unrestricted air flow for at least 270 degrees around each
sampler. The initial monitoring location selection will be verified by EPA
and MDE personnel in the field.
Table 4 summarizes the number of samples and analytical methods to be
used for the pre-construction and construction sampling. The goal of preconstruction real-time monitoring and sample collection is to collect
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samples for 15 consecutive calendar days. In the event that samples
cannot be collected (e.g. equipment malfunction, severe weather
conditions, etc.), an extra sampling day(s) will be added to the schedule to
make up for the collection of lost data and samples to achieve 15 days of
sampling. Samples for real-time Total PM and daily average particulate
CrVI concentrations will be collected each day at the three monitoring
locations and one co-located station for 15 sampling days, yielding 60
primary samples and 30 quality assurance samples for laboratory analysis
by laboratory-specific method ERG-MOR-063, which is modified from
ASTM Method D7614-12. No potential dust generating activities may
occur on the site during pre-construction air monitoring.
A meteorological monitoring station will be sited following EPA siting
guidance in EPA-454/B-08-002 Quality Assurance Handbook for Air
Pollution Measurement Systems Volume IV: Meteorological
Measurements Version 2.0 (Final), March 2008. The wind speed and
direction sensors for the meteorological monitoring system will be
situated approximately 10 meters above ground, on the Transfer Station
Mechanical Room rooftop during the pre-construction and construction
air monitoring. The meteorological sensors will be calibrated on-site
during installation following the guidance of EPA-454/B-08-002.
Table 4. Pre-construction Monitoring Samples
Sampling
Location
Sample
Methods
Sample
Equipment
Sampling
Duration
PAM-1
CrVI:
Laboratoryspecific
method ERGMOR-063
(2) BGI Model
PQ-100 pumps
with NaHCO3impregnated
Whatman 541
filter cassettes
15 days, 24hours per
primary
samples
QA/QC Events
Check filter for foreign
matter, tears, or
pinholes
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
1 field duplicate:
co-located BGI
sampler
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Real-time
total PM:
Equipmentspecific
method1
(2) DustTrak
Model
8533monitors
15 days, 24hour
continuous
monitoring
Zero check calibration
before first use
Clean inlet every 2
weeks
Replace internal filters
every 2 weeks or
sooner if error
message noted
1 field duplicate:
DustTrak DRX 8533
connected to same
intake port via a “T”
connector
OAM-1
CrVI:
Laboratoryspecific
method ERGMOR-063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
15 days, 24hours per
primary
samples
Check filter for foreign
matter, tears, or
pinholes
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
OAM-2
Real-time
total PM:
Equipmentspecific
method1
(1) DustTrak
DRX 8533
monitor
CrVI:
Laboratoryspecific
method ERGMOR-063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
15 days, 24hour
continuous
monitoring
Zero check calibration
before first use
Clean inlet every 4
weeks
Replace internal filters
every 2 weeks or
sooner if error
message noted
15 days, 24hours per
primary
sample
Check filter for foreign
matter, tears, or
pinholes
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
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Real-time
total PM:
Equipmentspecific
method1
1 The
(1) DustTrak
DRX 8533
monitor
15 days, 24hour
continuous
monitoring
Zero check calibration
before first use
Clean inlet every 4
weeks
Replace internal filters
every 2 weeks or
sooner if error
message noted
real-time data is collected continuously including one co-located station, see details provided
in the Preconstruction SAP in Appendix A. Daily 24-hour average Total PM concentration results
will be used in the statistical analyses as described in Appendix D.
One trip blank will be included in the daily shipments of CrVI filters to the laboratory. Trip blanks
are unopened filters.
One field blank will be collected per day of CrVI sample collection. Field blanks will be sent to the
field, opened, and then packaged like the primary samples, but not placed on the sampling devices.
One field performance audit will be performed for all three sampling locations.
3.1.2
Construction Air Monitoring
During construction, dust levels will be assessed at locations adjacent to
intrusive activities (Work Zone sampling), at the perimeter of the site, and
off-site. Final monitoring locations will be determined upon completion
of the pre-construction sampling event. It is expected that there will be
four perimeter monitoring locations at the property boundary of the
development (Figure 4, PAM-1 through PAM-4) and two off-site locations
(OAM-1 and OAM-2). Note that locations PAM-1, OAM-1, and OAM-2
will also be used during Pre-construction monitoring.
It is anticipated that these perimeter and off-site locations will be operated
continuously, 24-hours per day, during “intrusive” construction work
days. In addition, each day during construction hours, a minimum of two
additional real-time monitors will be placed in the Work Zone
immediately adjacent to and upwind of construction intrusive activities.
The Work Zone monitors will be set to sound an audible alarm in the
event the Total PM action level is exceeded, providing immediate
feedback to workers as to when dust levels might require additional
controls. Work Zone monitoring will occur on all work days. Table 5
summarizes the number of samples and analytical methods used for
construction sampling.
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Table 5. Construction Monitoring Samples
Sampling
Location
Sample
Methods
Sample
Equipment
Sampling
Duration
PAM-1
CrVI:
Laboratory
-specific
method
ERG-MOR063
(2) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
Duration of
construction,
24-hours per
primary
samples
QA/QC Events
Check filter for foreign
matter, tears, or pinholes
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Co-located
Confirm sample
operation within time
parameters
PAM-2
Real-time
total PM:
Equipment
-specific
method
(2) DustTrak
Model 8533
CrVI:
Laboratory
-specific
method
ERG-MOR063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
Duplicate
Duration of
construction,
24-hour
continuous
monitoring
Zero check calibration
before first use
Duration of
construction,
24-hours per
primary
samples
Check filter for foreign
matter, tears, or pinholes
Clean inlet every 2 weeks
Replace internal filters
every 2 weeks or sooner if
error message noted
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
PAM-3
Real-time
total PM:
Equipment
-specific
method
(1) DustTrak
DRX 8533
CrVI:
Laboratory
-specific
method
ERG-MOR063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
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Duration of
construction,
24-hour
continuous
monitoring
Duration of
construction,
24-hours per
primary
samples
Zero check calibration
before first use
Clean inlet every 4 weeks
Replace internal filters
every 2 weeks or sooner if
error message noted
Check filter for foreign
matter, tears, or pinholes
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
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Sampling
Location
Sample
Methods
Sample
Equipment
Sampling
Duration
QA/QC Events
flow rates within ±10%
Confirm sample
operation within time
parameters
PAM-4
Real-time
total PM:
Equipment
-specific
method
(1) DustTrak
Model 8533
CrVI:
Laboratory
-specific
method
ERG-MOR063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
Duration of
construction,
24-hour
continuous
monitoring
Zero check calibration
before first use
Duration of
construction,
24-hours per
primary
samples
Check filter for foreign
matter, tears, or pinholes
Clean inlet every 2 weeks
Replace internal filters
every 2 weeks or sooner if
error message noted
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
OAM-1
Real-time
total PM:
Equipment
-specific
method
(1) DustTrak
Model 8533
CrVI:
Laboratory
-specific
method
ERG-MOR063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
Duration of
construction,
24-hour
continuous
monitoring
Zero check calibration
before first use
Duration of
construction,
24-hours per
primary
samples
Check filter for foreign
matter, tears, or pinholes
Clean inlet every 2 weeks
Replace internal filters
every 2 weeks or sooner if
error message noted
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
Real-time
total PM:
(1) DustTrak
Model 8533
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Sampling
Location
Sample
Methods
Sample
Equipment
Equipment
-specific
method
OAM-2
CrVI:
Laboratory
-specific
method
ERG-MOR063
(1) BGI Model
PQ-100 pump
with NaHCO3impregnated
Whatman 541
filter cassettes
Sampling
Duration
QA/QC Events
24-hour
continuous
monitoring
Clean inlet every 2 weeks
Duration of
construction,
24-hours per
primary
samples
Check filter for foreign
matter, tears, or pinholes
Replace internal filters
every 2 weeks or sooner if
error message noted
Flow rate calibration at
beginning and end of
sample collection
Confirm start and stop
flow rates within ±10%
Confirm sample
operation within time
parameters
Real-time
total PM:
Equipment
-specific
method
(1) DustTrak
Model 8533
Duration of
construction,
24-hour
continuous
monitoring
Zero check calibration
before first use
Clean inlet every 2 weeks
Replace internal filters
every 2 weeks or sooner if
error message noted
Each perimeter and off-site air monitoring location will be sited in
accordance with EPA monitor siting guidelines established in 40 CFR Part
58, Appendix E, to provide representative data for the area. This guidance
ensures monitoring locations and equipment will be sited, to the extent
possible, away from trees, buildings, roadways, or other obstacles that
may cause undue influence on the measured concentrations. Sampler
inlets will be placed not less than 2 meters above ground level and have
unrestricted air flow for at least 270 degrees around each sampler. The
monitoring location selection will be verified by EPA and MDE personnel
in the field.
A meteorological monitoring station will be sited following EPA siting
guidance in EPA-454/B-08-002 Quality Assurance Handbook for Air Pollution
Measurement Systems Volume IV: Meteorological Measurements Version 2.0
(Final), March 2008. The wind speed and direction sensors for the
meteorological monitoring system will be situated approximately 10
meters above ground, on the Transfer Station Mechanical Room rooftop
during the pre-construction and construction air monitoring. The
meteorological sensors will be calibrated on-site during installation
following the guidance of EPA-454/B-08-002.
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3.2
SAMPLING PROCEDURES AND REQUIREMENTS
Details of sample collection procedures are provided in the Sampling and
Analysis Plans (Appendix A). Sample start time, end time, beginning and
ending flow rate (see Section 4.6), and total sample volumes will be
recorded on the field forms (Appendix B) along with any other pertinent
information regarding sample collection.
In addition to the field forms, field information will also be recorded in
field notebooks that are sequentially pre-numbered; the field notebooks
will be bound, have a water-resistant cover, and be assigned to individual
field personnel for the duration of field activities. Entries will be as
detailed and as descriptive as practical so that a particular situation can be
recalled without relying solely on the sampler’s memory. Field log entries
will be dated and signed. Information entered in the field notebook will
include, at a minimum, the following items:
• Project name and number;
• Dates and times of entries;
• Weather conditions;
• Names of personnel performing the activities;
• A description of sample locations, including sample name and
type;
• Field instrument calibration information;
• Field instrument readings; and
• Health and safety information.
Information recorded in the field notebook should be neat, legible,
completed in dark, permanent ink, and signed and dated by the person
completing the entry.
Copies of the field notebook will be provided to the PM, and the data will
be summarized for reporting purposes and retained in the appropriate
project file.
Field notebooks will be stored in ERM’s project file when not in use.
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Corrections to field documentation will be made by striking out the
incorrect entry, entering the corrected value or text, and dating and
initialing the document; the original entry will remain visible.
3.3
SAMPLING HANDLING, CUSTODY PROCEDURES, AND
DOCUMENTATION
CrVI samples will be stored in an on-site freezer and shipped to the
laboratory daily during pre-construction monitoring and twice per week
during construction monitoring. CrVI samples have a holding time of 10
days, providing they are kept frozen. Sample coolers will be refreshed
with ice packs as necessary to ensure a temperature of less than 0oC is
maintained until receipt by the laboratory. Samples will be stored in the
laboratory freezer until extraction and sample analysis immediately
thereafter.
CrVI samples are collected on specific, laboratory-prepared filters that are
loaded by the laboratory into cassettes. In the field, the cassettes are
loaded into the sample pump for collection of primary samples. Filters
will be considered invalid if any of the following occur:
•
Filter has been dropped or contaminated with any foreign
matter (such as dirt, finger marks, ink, liquids, etc.);
•
Filter with tears or pinholes;
•
The start and stop flow rates differ more than ±10%; or
•
Filter sample operates less than 23 hours or more than 25 hours.
The sample date and time collected, project name and number, and
unique sampling number associated with the filter will be recorded on the
sample label. CrVI samples will be placed in a cooler with ice packs
immediately after removing filter cassettes from the sample pump, as
CrVI samples must arrive at the lab at 0ºC.
The COC of the physical sample and its corresponding documentation
will be maintained throughout the handling of the sample. All samples
must be identified, labeled, logged in a COC form, and recorded in the
field notebook as a part of the procedure to ensure the integrity of the
resulting data. Information required on the COC form includes the
following:
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•
Project name, location, and number;
•
Name of ERM PM;
•
Sampler name and signature;
•
Location and time of sampling;
•
Total volume of air that passed through the filter, including
both the calculated total volume and the total volume reported
by the BGI PQ-100 sampler;
•
Unique sampling number associated with the filter;
•
Sample type and matrix;
•
Requested analytical parameters or methods;
•
Laboratory name and contact information;
•
Signature of person relinquishing samples;
•
Date and time of relinquishing;
•
Special instructions, if any;
•
Signature of receiver and date and time samples received
(completed by laboratory upon receipt).
The record of the physical sample (location and time of sampling, total
volume of air that passed through each filter) will be related to the
analytical results through accurate accounting of the sample custody.
Sample custody applies to both field and laboratory operations.
Analytical requests will be identified on the form. The information (for
each sample) provided on the COC form will duplicate the information
provided on the sample label of each sample container. A carbon copy of
the COC form completed by the field team will be submitted to the ERM
QA Manager. The original and carbon copy COC form will be placed in
protective plastic and will be taped to the inside lid of the cooler
containing samples before transport to the laboratory. The COC forms
will be retained in the ERM project job files by the QA Manager.
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Sampling personnel will be responsible for the care and custody of the
samples from the time they are collected until they are transferred to
another individual. A sample is under an individual's custody if one of
the following criteria is met:
•
It is in the sampler’s possession.
•
It is in the sampler's view after being in possession.
•
It is in the sampler's possession and secured to prevent
tampering.
•
It is in a designated secure area.
Sampling personnel will complete the COC form for each sample
shipment. When transferring custody, the individuals relinquishing and
receiving samples will sign, date, and note the time of the exchange on the
record. The COC record will be completed using waterproof ink.
Corrections will be made by drawing a single line through the error and
initialing and dating the correction. Information will not be erased or
rendered unreadable.
When the samples arrive at the laboratory, the laboratory personnel
receiving the sample cooler will evaluate the integrity of the samples and
sign the COC form. The laboratory will assign work order numbers to the
samples for use in its internal tracking system. Damaged sample
containers, sample labeling discrepancies between sample container labels
and the COC form, and analytical request discrepancies will be noted on
the COC form. The laboratory will contact the ERM FM or ERM Quality
Manager by sending the COCs and the sample non-conformance report
electronically within 24 hours of sample receipt. The laboratory will also
provide a sample acknowledgment to ERM indicating field sample
identification, laboratory identification number, and analytical testing
logged for each sample. ERM will review this information for correctness
within 24 hours of receipt and provide feedback to the laboratory. The
status of a sample can be checked at any time by referring to the
laboratory numbers on the COC form and the laboratory work order
numbers in the notebook. Both the laboratory and unique sampling
numbers will be cited when the analytical results are reported. The
laboratory will send the carbon copy of the COC form and the analytical
data package to the PM.
Standard Operating Procedures (SOPs) and data collection forms have
been developed for sample custody, sample labeling, analysis requests,
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and shipping and tracking procedures. Field SOPs are included in
Appendix B. Analytical laboratory sample custody procedures are
included in the laboratory SOP (Appendix C), which identify the roles of
both the sample custodian and the laboratory coordinator.
3.4
ANALYTICAL METHOD REQUIREMENTS
Analytical methods and over-all analytical quality requirements for the
laboratory are provided in Table 2. The laboratory-specific Method ERGMOR-063 (modified ASTM Method D7614-12) is provided in Appendix C.
The required laboratory turn-around time (TAT) will be three (3) business
days from receipt of samples during the pre-construction and the
construction phases unless written approval is received from EPA and
MDE to extend the TAT to 10 business days.
3.5
FIELD QUALITY CONTROL REQUIREMENTS
Field blank filters in sample cassettes will be sent to the field, opened, and
re-packaged as with the sample filter cassettes but not exposed to the air
on a sampling device, and returned to the laboratories along with the
primary samples according to the schedule shown in Tables 4 and 5.
Blank filters will be provided by the laboratories from the same lot as the
filters provided for sample collection. Additionally, a trip blank will be
included in each sample set (2 per week, one in each shipment to the
laboratory). A trip blank is shipped to the field and back to the laboratory,
but never opened. All filters will be maintained at a temperature of less
than 0oC from the time of shipment from the laboratory until the time of
analysis, except during field sampling.
3.6
FIELD INSTRUMENT/EQUIPMENT CALIBRATION AND
MAINTENANCE REQUIREMENTS
Maintenance and calibration of field instruments are included in the field
Standard Operating Procedures in Appendix B. Sampling equipment will
be maintained according to the manufacturer’s specifications. A summary
of the daily field calibration procedures is provided in Table 6 and a
summary of field equipment maintenance procedures is provided in Table
7. Calibration and maintenance procedures for collection of samples for
particulate CrVI and for Total PM are detailed below.
Table 6. Field Calibration, Testing, and Inspection
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Field
Equipment
Calibration Testing
Activity
Activity
BGI Model
PQ-100
Pump flow One point
rate
calibration
using BGI
TetraCal
DustTrak
DRX 8533
Zero
instrument
Inspection
Activity
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Acceptance Criteria
Initial daily Beginning Initial flow rates
flow check and end of ±4%
each sample
Start/stop
Start and stop flow
collection
flow rates
rates ±10%
period
Flow rate at 15
L/min
1-point check Zero value
with zero
filter
Pump flow One point
rate
calibration
using BIOS
Defender 510H
Frequency
Once per
day
Initial daily Once per
flow check day
2 liters per minute,
±5%
±0.001 milligrams
per cubic meter
Start/stop
flow rates
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Table 7. Field Equipment Maintenance, Testing and Inspection
Field
Equipment
Parameter
Maintenance Inspection
Activities
Activity
BGI
Model
PQ-100
Pump flow Replace
diaphragms,
rate
valves, and
bearings after
5000 hours of
use
DustTrak
DRX 8533
Zero
instrument
Clean
instrument
Frequency
Acceptance
Criteria
Check
pump
cumulative
time
Beginning of Less than 4,500
each week cumulative
hours
1-point check Zero value
with zero
filter
Once per day ±0.001 milligra
ms per cubic
meter
Clean inlet
and internal
filters
Factory
cleaning and
calibration
Confirm
that no error
indicators
are present
on
instrument
screen
Check
instrument
screen once
per day;
clean once
every two
weeks
Confirm
maintenance
schedule in
field notebook
Beginning of
Confirm
with rental project
agency that
factory
cleaning has
occurred
CrVI: Air samples will be collected using BGI Model PQ-100 or
equivalent samplers. Sampling will be performed at 15 L/min during the
sampling period. Sampling flow rates will be checked at the beginning
and end of each sampling period, using BGI TetraCal flow standard and
flow rates recorded on the field sampling form (form included in
Appendix B). If the initial daily flow check varies from the pre-set
sampling flow rate by more than 4 percent, a full recalibration will be
performed. The total volume reported by the BGI PQ-100 will be
provided on the field forms with the data reports. For QC comparison,
the average flow rate reported by the BGI PQ-100 will be multiplied by the
exact duration of time the sample was being collected in order that the
total volume can also be calculated for each sample. Note that the
instrument is designed to maintain a steady flow rate. If the beginning
and ending flow rates vary by more than 10%, the filter is invalidated.
Calibration records and the individual air volumes per filter, including all
volume calculations will be documented and provided with data reports.
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The BGI Model PQ-100 instruction manual is provided in the Preconstruction and Construction SAPs found in Appendix A.
DustTrak DRX 8533: The DustTrak Model 8533 monitors Total PM
concentrations and stores 1-minute averages on an internal data logger.
The manufacturer lists daily maintenance and calibration procedures that
will be followed in the field. In addition, other maintenance and
calibration procedures that will be used are as follows:
•
Before each use: perform a zero check according to manual
instructions.
•
Manufacturer instructions recommend cleaning the inlet after
every 350 hr. if total dust concentrations are at 1 mg/M3. As a
practical matter in the field, the inlet will be cleaned every two
(2) weeks and the cleaning date and time recorded in the field
notebook.
•
Manufacturer instructions recommend replacing internal filters
every 350 hr. if total dust concentrations are at 1 mg/M3 or
when indicated by the main screen filter error indicator. As a
practical matter in the field, if no error message has been noted,
the inlet will be cleaned every two (2) weeks and the cleaning
date and time recorded in the field notebook.
Because the DustTrak Model 8533 will be operated in the Total PM mode
rather than size-specific classifications, the factory-set photometric
calibration factor (PCF) of 1.0 and size correction factor (SCF) of 1.0 will be
used. As recommended by the manufacturer, the Ambient Air calibration
factor will be selected to represent outdoor ambient dust. The DustTrak
Model 8533 instruction manual is provided in the Pre-construction and
Construction SAPs, Appendix A.
Laboratory instrument/equipment calibration and maintenance
requirements are provided in Appendix C.
3.7
LABORATORY QUALITY CONTROL REQUIREMENTS
Laboratory records are defined as all written, recorded, and electronic
documentation necessary to reconstruct all laboratory activities that
produce data and include all information relating to the laboratory’s
equipment, analytical test methods, and related activities.
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The laboratory will retain copies of all sample, sample QC and calibration
runs, quantitation reports, injection logs, preparation summary sheets,
corrective action reports, and summary information in a central file
location for 5 years from the date of analysis. Electronic copies of raw data
should also be retained by the laboratory for 5 years from the date of
analysis.
Specific laboratory instrument calibration procedures for various
instruments are described in detail in the method-specific procedures and
laboratory SOPs for the analytical laboratory selected, as provided in
Appendix C.
3.8
DATA MANAGEMENT REQUIREMENTS
This section describes the data management process and methods to
ensure data integrity from data production in the field to final use and
retention. All data will be reviewed and verified for accuracy by the ERM
QA/QC Officer and Field Manager (FM). The ERM FM will ensure that
the field and technical data obtained for the project will provide the end
user with acceptable data. All field and technical data shall be reviewed
by the ERM QA/QC Officer, to ensure that the final data is accurate prior
to the inclusion in the project report. The field data sheets, log books,
COC forms, and DustTrak data are reviewed and submitted (faxed,
electronic, or hard copy) by the ERM FM to the ERM QA/QC Officer
daily.
The analytical data processing procedure is presented on Figure 5 and
summarized as follows:
1. Samples are sent to the laboratory under COC.
2. The laboratory enters the sample information into their tracking
system and performs the analysis.
3. The laboratory electronically submits raw data, sample results,
and their QA information to ERM and to an independent third
party validator, who in turn performs Level II validation, as
described in EPA’s Guidance on Environmental Data Verification
and Data Validation (2002).
4. The third party validator electronically submits their validation
report to ERM.
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5. ERM reviews the data validation report, and, if acceptable,
stores all data into the project files. If unacceptable, ERM may
request re-analysis of the data by the laboratory. Under this
condition, the ERM PM will bring this result to the attention of
EPA and MDE and request their concurrence of ERM’s
recommendation of whether or not to perform the re-analysis.
6. Once the ERM QA/QC Officer completes the accuracy review,
the ERM FM, or their designee, then stores the validated
information electronically into ERM’s project files and uploads
the summary tables to the project website.
Real-time data processing is summarized as follows:
1. The field data sheets (real-time Total PM) and real-time instrument
data logs are submitted (faxed, electronic, or hard copy) by field
personnel to the ERM PM weekly. The ERM PM, or their designee
checks all metadata for accuracy, then stores the information
electronically into ERM’s project files.
2. ERM submits the field data sheets and real-time instrument data
logs to the third party validator.
3. The third party validator electronically submits their validation
report to ERM.
Real-time Total PM concentration data will be provided as hourly
averages based on one (1) minute frequency data collection. The daily
average real-time Total PM concentration data will be used to calculate the
dust action level, i.e., the background threshold value (BTV).
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4.0
ASSESSMENTS
4.1
FIELD DATA REVIEW
The process of reviewing field data will involve evaluating field records
for consistency and completeness assuring that each sample result is fully
supported by accurate metadata, reviewing QC and calibration
information, summarizing deviations and determining their impact on
data quality, summarizing the samples collected, and summary of the
review in the project report.
Field data (provided to the ERM PM by fax, electronically or hard copy)
will be scanned at least weekly and stored electronically as part of the
project database maintained by ERM
4.1.1
Sampling Program Design Execution
Sample collection records (provided to ERM PM by fax, electronically or
hard copy) will be reviewed weekly by the ERM QA/QC Officer/PM or
qualified designee to ensure that samples have been collected according to
the sampling design. Items to be reviewed include the types and numbers
of samples collected, sampling locations and frequencies, and
measurement parameters of interest. Deviations must be reported to
ERM’s PM immediately. Under this condition, the ERM PM will bring this
result to the attention of EPA and MDE and request their concurrence of
ERM’s recommendation of whether or not the identified deviation
requires any additional attention.
4.1.2
Sample Collection Procedures
Sample collection procedures will be reviewed by the ERM FM and the
ERM QA/QC Officer to ensure that the appropriate procedures have been
followed. Items to be reviewed include sampling methods and
equipment, sample type, time, location and sample preservation
requirements. Deviations must be reported to the ERM PM immediately.
The PM will determine whether the samples meet the field quality control
requirements specified in Section 4.5.1. Under this condition, the ERM
PM will bring this result to the attention of EPA and MDE and request
their concurrence of ERM’s recommendation of whether or not the
identified deviation requires any additional attention.
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4.1.3
Sample Handling
Sample handling procedures will be reviewed by the ERM FM and the
ERM QA/QC Officer to ensure that the appropriate procedures have been
followed. Items to be reviewed include sample labeling, COC
documentation, sample preservation and holding times, sample
packaging, and shipment. Deviations from established procedures must
be reported to the PM immediately. Under this condition, the ERM PM
will bring this result to the attention of EPA and MDE and request their
concurrence of ERM’s recommendation of whether or not the identified
deviation requires any additional attention.
4.1.4
Quantitative Field Data
The volume calculations performed in the field will be verified by the
ERM FM and the ERM QA/QC Officer, along with the sample collection
and handling procedures noted above.
4.1.5
Field and Technical Data Reduction
Field and analytical data will be summarized in tables as appropriate.
ERM will perform a 100% check of all data presented on data summary
tables.
4.2
LABORATORY DATA
This section describes the data review, reduction, and verification
processes for laboratory data, as well as who is responsible for executing
each process.
4.2.1
Laboratory Data Review and Reduction
The laboratory will review and reduce the data internally in accordance
with its SOP (Appendix C) and established internal procedures prior to
submitting the data to the ERM FM. The ERG SOP contains all quality
control requirements, as shown in the SOP Tables 24-1 and 24-2.
Laboratory SOPs for internal data review procedures are to be maintained
electronically in the project files. Specifically, the laboratory will review
the data package to ensure the following:
•
Sample preparation information is correct and complete;
•
Holding times have been met;
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•
Analytical information is complete and was generated within
acceptable criteria;
•
Any discrepancies/corrective actions identified during sample
login, preparation or analysis have been addressed and
documented;
•
The appropriate SOPs have been followed;
•
QC samples were within established control limits;
•
Analytical requirements have been met (e.g., the correct analytical
procedures were used as defined by the COC); and
•
Documentation is complete and any QC issues are fully explained
in a detailed case narrative.
An authorized laboratory employee must sign the data package to
indicate the data have been reviewed.
Data will be reduced in the laboratory following method protocols and
reported in standard formats. The data will be peer-reviewed by a
qualified analyst before it is released to ERM. The review will be
documented with a standard checklist that has been initialed and dated by
the peer reviewer. Reporting requirements for analytical data pertain
only to the final data report to be submitted to ERM.
4.2.2
Laboratory Data Review and Validation
Following receipt of the laboratory report, ERM will send the report
(including raw data and all QA/QC information) to the designated thirdparty validator. The third party will perform Level II validation, as
described in EPA’s Guidance on Environmental Data Verification and Data
Validation (2002). Level II validation will include 40% raw data recalculation.
4.3
AUDITS OF DATA QUALITY
A performance audit is defined as a review of the existing procedures and
analytical data (sample and QA) to determine the accuracy of the total
measurement systems, or a component of the system. The analysis of a
project-specific laboratory Performance Evaluation (PE) sample is the
primary method for a performance audit of the laboratory. An equivalent
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evaluation sample audit method is difficult to produce in the field;
therefore, procedure audits will be performed to assess the accuracy and
consistent application of field SOPs.
4.3.1
Performance Audits
4.3.1.1
Field Performance Audits
Performance audits of field activities consist of procedure audits that may
be conducted by the PM or qualified designee. During a procedure audit,
the field auditor observes and reviews actual procedures to verify
conformance with written field procedures as well as sampling and
analysis protocols. Specific attention is given to sampling, data collection,
sample preservation, decontamination, and disposal of waste to
demonstrate compliance with required procedures. Field instrumentation
QC procedures are also verified. The field auditor meets with key field
staff members to evaluate the field program and determine if changes are
necessary to improve data quality. One field performance audit will be
performed during the pre-construction phase of the project.
Audit items are tied to the tasks defined in the field procedures, as well as
in the sampling and analysis protocols, rather than restricted to a specific
list. The field auditor verbally reports the results of each audit to the PM
within one working day to transmit any significant problems with the
field QA program. Any non-conformance identified during the audit will
be reported immediately to the PM and remedied as soon as possible. A
written report will be provided to key personnel and placed in the project
file within 10 working days of each audit. This report should include a
field audit checklist, documentation of on-site meetings, findings, and
program revisions.
4.3.1.2
Laboratory Performance Audits
In a performance audit, a PE sample is submitted to the laboratory and
analyzed for the purpose of evaluating the performance of the
measurement or analytical procedures used by the laboratory. The PE
sample consists of some type of environmental matrix (e.g., air, soil,
water) which contains a known amount of a particular analyte(s). The PE
sample result will be submitted to EPA and MDE prior to initiating the
pre-construction monitoring.
Review of PE sample data will be performed by the third-party reviewer
and includes verifying the following:
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•
Sample analysis was completed following the correct
methodology;
•
Correct identification and quantitation of sample analytes;
•
Accurate and complete reporting of data to meet project
specifications; and
•
Instruments are operating within established precision and
accuracy control limits.
Results that do not fall into the certified limits of acceptability may
indicate a laboratory performance problem and will trigger immediate
corrective actions. All particulate CrVI samples will be analyzed by ERG
for this project.
4.3.2
System Audits
The ERM QA/QC Officer or qualified designee may conduct a laboratory
systems audit. This auditor, in conjunction with the Laboratory QA
Manager, may conduct the systems startup audit to ensure that all
instruments proposed or in use are appropriate for the given methods and
functioning properly. Additional external audits will be performed as
needed. Internal laboratory audits should be performed by the Laboratory
QA Manager, Laboratory PM, or qualified designee annually.
During internal and external audits, the auditor will observe and review
laboratory procedures and analytical results to ensure that they conform
to the operating procedures and reporting requirements. Prior to the
laboratory audit, the auditor will prepare a list of items and procedures to
be audited. Audit items may be tied to the analyses of the samples in
progress rather than be restricted to a specific list. Internal systems audits
will include a review of the following:
•
Sample custody and tracking procedures;
•
Calibration procedures and documentation;
•
Completeness of data forms, notebooks, and other data
reporting documents;
•
Compliance with laboratory SOPs;
•
Data storage, filing, and record-keeping procedures;
•
QC procedures, criteria, and documentation;
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•
Operating conditions of equipment and facilities;
•
Employee training records; and
•
Laboratory information and management system procedures
and security.
External systems audits will include a review of the previous items plus a
review of laboratory internal assessment SOPs and laboratory internal
assessment documentation. The auditor will meet with key staff members
to evaluate the program and determine if corrective actions are necessary
to improve the data quality.
The auditor will submit a report in writing to the ERM QA/QC Officer or
PM within five (5) working days of the audit. The report will include the
documentation of on-site meetings, findings, and proposed revisions. A
written assessment of the laboratory with any suggested changes in
procedures will be provided to the laboratory. Follow-up audits will be
conducted if warranted by the audit findings. If changes in the systems
are necessary, the Laboratory PM or designee will make the changes.
Written confirmation within 10 days will document any corrective actions
the laboratory has implemented to meet requirements of the measurement
system. The letter should be directed to the ERM PM or QA/QC Officer’s
attention.
After the ERM PM has been notified (following the initial systems audit)
that the laboratory systems are all satisfactory, QC measures will be
implemented. After implementation of the plan, all procedures will be
monitored internally by the laboratory to facilitate compliance with the
requirements. Any significant problems within the system will be verbally
reported immediately to the QA/QC Officer. Verbal notification will be
followed by a written report within 10 working days from completion of
the audit and/or the resolution of the change. Written reports should be
retained in the laboratory permanent files, as well as in ERM’s project file.
4.4
SURVEILLANCE OF OPERATIONS
The results of monitoring will be posted to the project-dedicated website
within approximately 24 hours, as practicable, of real-time collection or
receipt of validated laboratory results. In this manner the public will have
ready access to monitoring results. The website will also post any
response actions deemed necessary due to the air monitoring results.
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The Developer’s representative is responsible for all necessary
notifications to both the MDE and EPA representatives. The Developer’s
representative on site will ensure both EPA and MDE’s representatives are
apprised of the air monitoring activities and results on a daily basis. In
this manner, the agencies can assess the need to notify the public of the air
monitoring results and related response actions, as appropriate.
4.5
ASSESSMENT OF DATA QUALITY
4.5.1
Field Data Quality
Data quality assessment criteria for field measurements include the
following parameters:
Precision– Precision of field procedures will be assessed through
the collection of field duplicate real-time data and co-located
samples (Section 2.0). Field duplicate data will be collected for
Total PM by use of second DustTrak monitor (duplicate), which
will be connected to the same inlet. Co-located samples of
particulate CrVI will be collected at a frequency of one per day.
If the relative percent differences (RPDs) for field duplicate data
or co-located sample results are within acceptance criteria, the
original result should be used. However, if the RPDs are not
within acceptance criteria, the more conservative result should
be used. Additional actions to assess and improve precision
may include collecting duplicate total particulate matter
samples for gravimetric analysis for comparison. The DustTrak
Field instrument accuracy and precision will be confirmed
using the QA/QC actions described in Table 4.
Accuracy – Accuracy in the field is a measure of how close the
value is to the true value and will be is assessed by the
Laboratory Control Sample, also known as the Method Spike.
Completeness – Field completeness is a measure of the number of
valid field measurements obtained relative to the total number
of field measurements. The percent of completeness for field
data can be expressed by the following formula:
Percent Completeness = (V/T) x 100
Where:
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V = Number of valid data points
T = Total number of data points
Field completeness is based on the number of samples or field
tests planned and the actual number collected or performed.
The completeness objective for field measurements is 90
percent.
Representativeness – Representativeness in the field will be
ensured by following standard procedures during data
collection. The ERM PM will monitor the sampling program to
ensure that field activities are being conducted consistently
according to the procedures outlined in the QAPP and the SAP.
Additionally, field duplicates will reflect representativeness by
measuring sample homogeneity and precision.
Comparability – Measures to ensure comparability of field data
include field personnel reviewing the QAPP and the SAP.
ERM’s FM and/or QA Manager will routinely verify that
proper field activity procedures are being followed. To facilitate
comparability of field data, ERM field staff will only utilize the
approved SAPs and Field SOPs.
Sensitivity – Sensitivity is the capability of a method or instrument
to discriminate between measurement responses representing
different levels of a variable of interest, or to detect or reliably
measure low levels of a variable of interest. Field sensitivity
basically refers to the smallest value or change in value a field
instrument can reliably measure above background noise. For
the pre-construction and construction phases of this project, this
concept applies to measurement of Total PM. The sensitivity
objectives for the DustTrak include the following specifications:
o Concentration Range = 0.001 to 150 mg/m3
o Resolution = ±0.1% of reading or 0.001 mg/m3,
whichever is greater
o Flow Accuracy = ±5% of factory set point
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4.5.2
Laboratory Data Reduction
Field and analytical data will be summarized in tables as appropriate and
discussed in the text of the data report.
The quality of laboratory data will be evaluated based on precision,
accuracy, representativeness, completeness, and comparability of the data
generated by each type of analysis. These data assessment parameters are
described in the following sections. The specific analytical criteria
including reporting limits and control limits for QC results are provided
in Appendix C.
Blank samples are used to determine contamination arising from
principally four sources: the environment from which the sample was
collected/analyzed, the reagents used in the analysis, the apparatus used,
and the operator/analyst performing the analysis. Three types of blanks
will be implemented in the in this monitoring program:
•
Field blanks - Field blank cassettes will be included for CrVI
samples yielding one filter cassette blank per day that samples
are collected. Blank filter cassettes will be sent to the field,
opened, but not placed on the sampling devices, and then
packaged like the actual samples. Field blank cassettes will be
returned to the laboratories in the same shipment as the
primary samples.
•
Trip blanks - Trip blank cassettes will be included for CrVI
samples yielding one filter cassette blank per sample shipment.
The trip blank is an un-opened, un-handled filter cassette.
• Lab blanks - Laboratory SOP for the ASTM Standard Test
Method D7614-12 (Determination of Total Suspended
Particulate (TSP) Hexavalent Chromium in Ambient Air
Analyzed by Ion Chromatography and Spectrophotometric
Measurements is included with this QAPP in Appendix C. This
SOP includes procedures and criteria for lab blanks, spiked
samples, and duplicate analyses.
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4.6
QUALITATIVE AND QUANTITATIVE COMPARISONS TO
ACCEPTANCE CRITERIA
4.6.1
Precision
Precision is a measure of random error, and describes the degree to which
repeated measurements are similar to one another. It measures the
agreement or reproducibility among individual measurements. Precision
will be measured through the use of field duplicate samples. . Duplicate
samples are ideally expected to contain similar chemical concentrations;
therefore, it is generally assumed that any variability in results is
introduced by inherent field heterogeneity, sampling, handling, or
laboratory procedures.
Precision will be calculated as the RPD as follows:
where:
% 𝑅𝑃𝐷𝑖 =
|𝑂𝑖 − 𝐷𝑖 |
𝑥 100%
(𝑂𝑖 + 𝐷𝑖 )/2
%RPDi
=
compound i
Relative percent difference for
Oi
sample
=
Value of compound i in original
Di
sample
=
Value of compound i in duplicate
The resultant RPD will be compared to acceptance criteria and deviations
from specified limits reported. If the laboratory objective criteria are not
met, the laboratory will supply a justification of why the acceptability
limits were exceeded and implement the appropriate corrective actions.
LDC, the third-party data quality reviewer will assess field and laboratory
RPDs and deviations from the specified limits will be noted and the effect
on reported data commented upon by LDC, as described in Section 4.0.
The data review will be provided to the ERM FM, who will take corrective
actions described in Section 4.0.
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4.6.2
Accuracy
Accuracy is the amount of agreement between a measured value and the
true value. It will be measured as the percent recovery of blank spike
samples and performance evaluation (PE) samples.
Accuracy shall be calculated as percent recovery of spiked analytes as
follows:
% Ri = (Yi ÷ X i ) × 100%
where:
%Ri
=
percent recovery for compound i
=
measured spike concentration in sample i
Yi
(sample concentration with the spike - original sample
concentration)
Xi
=
actual spike amount in sample i
The resultant percent recoveries will be compared to acceptance criteria
(described in Section 4.0) and deviations from specified limits will be
reported. If the objective criteria are not met, the laboratory will supply a
justification of why the acceptability limits were exceeded and implement
the appropriate corrective actions.
LDC, the third-party data quality reviewer will assess laboratory %R and
deviations from the specified limits will be noted and the effect on
reported data commented upon by LDC, as described in Section 4.0. The
data review will be provided to the ERM FM, who will take corrective
actions described in Section 4.0.
4.6.3
Representativeness
Representativeness is a qualitative parameter that expresses the degree to
which sample data accurately and precisely represent a characteristic of a
population, parameter variations at a sampling point, or an environmental
condition. Representativeness of the environmental conditions at the time
of sampling is achieved by selecting sampling locations, methods, and
times so that the data describe the site conditions that the project seeks to
evaluate. Representative samples will also be ensured through following
proper protocols for sample handling (storage, preservation, packaging,
custody, and transportation), sample documentation, and laboratory
sample handling and documentation procedures.
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4.6.4
Comparability
Comparability is a qualitative parameter expressing the confidence with
which one data set can be compared to another. The comparability goal is
achieved by maintaining consistency in sampling conditions, selection of
sampling procedures, sample preservation methods, and analytical
methods.
4.6.5
Completeness
Completeness for usable data is defined as the percentage of usable data
out of the total amount of planned data. The closer the numbers are; the
more complete the measurement system. The target goal for completeness
is 90 percent for all data. Completeness will be calculated as follows:
%C =
A
x100%
I
where:
%C
=
Percent completeness (analytical)
A
=
Number of usable sample results
reported (all results not rejected)
I
=
Total number of results reported
Non-valid data (i.e., data qualified as “R” rejected) will be identified
during the data review and the reasons for rejection explained in the data
review report.
4.6.6
Sensitivity (Method Detection Limit)
Sensitivity is the capability of a method or instrument to discriminate
between measurement responses representing different levels of a
variable of interest, or to detect or reliably measure low levels of a variable
of interest. Sensitivity defines the method detection limit (MDL) as the
minimum concentration of a substance that can be measured and reported
with 99 percent confidence that the concentration is greater than zero. The
MDL for particulate CrVI is provided Section 4.0.
The MDL is determined every year according to the procedure in 40 CFR,
Part 136, Appendix B. A standard is spiked onto at least seven prepared
filters at a concentration one to five times the estimated detection limit.
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These filters are extracted and analyzed according to the method outlined.
The MDL is calculated as follows:
MDL = (t) x (SD)
where:
t
=
Student’s t value for a 99% confidence
level and a standard deviation estimate with n – 1
degrees for freedom [t = 3.14 for seven replicates]
SD
=
analysis
Standard deviation of the replicate
The laboratory will maintain current records of DL studies for each
instrument, and will have established reasonable accuracy (lower control
limits should be 10 percent or greater) and precision goals for the
analytical method utilized. The laboratory should perform DL verification
studies at least annually for each method, as stipulated by National
Environmental Laboratory Accreditation Conference. The concentration of
the standards used to determine the DLs should be no more than five
times the expected DL value. Historical DL studies, accuracy, and
precision limit control charts should be retained in the laboratory archives
for five (5) years.
4.7
INTERIM ASSESSMENTS OF DATA QUALITY
Evaluation of field and laboratory QC data and/or audits conducted for
field operations and/or laboratory operations may indicate the need for a
corrective action. Problems with analytical QC data will be addressed by
the laboratory QC officer. Problems arising during field operations,
however, will be addressed by the Technical Lead through
communication of the identified problem and proposed corrective action
to the ERM Project Manager. The Project Manager and Technical Lead
will discuss the appropriate actions with the MDE and EPA
representatives to obtain concurrence, and then relay this information to
the field personnel for implementation. The field personnel will then
report back to the ERM Project Manager upon successful implementation
of the corrective act.
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5
REVIEW, EVALUATION OF USABILITY AND REPORTING
REQUIREMENTS
5.1
DATA VERIFICATION AND VALIDATION TARGETS AND METHODS
All data will be verified by a review of the completeness and accuracy of
each result’s metadata. Field operations will be fully documented,
reviewed, and audited. All CrVI data will undergo Level II third party
data validation. The precision of the DustTrak particulate data will be
determined by daily duplicate results.
The quality of field and laboratory data will be evaluated based on
precision, accuracy, representativeness, completeness, and comparability
of the data generated by each type of analysis. These data assessment
parameters are described in the following sections. The specific analytical
criteria, including reporting limits and control limits for QC results, are
provided in Appendix C.
5.2
QUANTITATIVE AND QUALITATIVE EVALUATIONS OF USABILITY
When the results of the measurements have been obtained, the ERM
Project Manager, QA Manager and Technical Lead will determine
whether the project QA/QC goals have been achieved. Whether the
overall project QA/QC goals have been met will be assessed by review of
the analytical data quality assessment reports generated using data
verification/validation. All laboratory results will be reviewed by the
ERM FM to verify that the data package is complete. The completeness
check will include a brief screening of six basic elements that should be
included in each data package, including:
•
Verification that sample numbers and analyses match the chainof-custody request.
•
Are all analyses that are requested on the Chain-of-Custody and
any change orders present in the data package?
•
Does the data package include a copy of the Chain-of-Custody
forms?
•
Has the laboratory placed any data qualifier flags on the
analytical results?
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•
Does the laboratory’s case narrative identify problems,
including an explanation of flagged data?
•
Does the data package include reports for all QA/QC samples
(see Table 5)?
• Based on any missing information and/or gross quality control
exceedence, should the laboratory perform additional analytical
work on the samples before holding times have expired or the
leftover sample is discarded?
The completeness, correctness, and conformance/compliance of the data
will be verified and validated against the method, procedural, or
contractual requirements. Guidance for data verification/validation is
provided in EPA’s Guidance on Environmental Data Verification and Data
Validation (EPA 2002b) and EPA’s National Functional Guidelines (EPA
1999; EPA 2004). Laboratory data will be validated in accordance with
ASTM Standard Test Method D7614-12 and the EPA document EPA
Contract Laboratory Program (CLP) National Functional Guidelines for
Inorganic Data Review, October 2004. One hundred percent of laboratory
data will be validated by Laboratory Data Consultants, Inc., a third-party
data reviewer. A Level II data review will be conducted, which consists of
the following elements:
•
Verification that sample numbers and analyses match the chainof-custody request.
•
Verification that sample preservation and holding times are
met.
•
Verification that instrument performance checks were
performed and acceptable.
•
Verification that calibrations were performed at the appropriate
frequency and met method criteria.
•
Verification that field, trip, and laboratory blanks were
performed at the proper frequency and that no analytes were
present in the blanks.
•
Verification that field and laboratory duplicates, matrix spikes,
and laboratory control samples were run at the proper
frequency and that control limits were met.
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•
Verify that internal standards results were acceptable.
•
Verification that project reporting limits have been achieved.
Data review and verification will be performed for 100 percent of the data.
In addition, the third-party reviewer will re-calculate 40% of the raw data,
which will include the following additional elements:
•
Initial Calibration Review: Review initial calibration
calculations for agreement with summary form results,
linearity, and method-specified minimum requirements;
•
Continuing Calibration Review: Review continuing calibration
calculations for agreement with summary form results,
linearity, and method-specified minimum requirements;
•
Laboratory Control Sample (Method Spike) Review: Review
internal standard responses to ensure that minimum and
maximum method-specified requirements are met and the
correct internal standard has been assigned to target
compounds and surrogates;
•
Target Compound Identification Review: Review target
compounds identified in project and QC samples and ensure
that calculated concentrations and identifications are accurate;
and
If deemed appropriate according to the EPA National Functional
Guidelines, Contract Laboratory Program data qualifiers will be applied
to indicate potential concerns regarding data quality. Data qualifiers that
may be applied to project data based on data validation are listed below:
•
U: The analyte was analyzed, but not detected above the
reported LOD or the LOQ was raised to the concentration found
in the sample due to blank contamination;
•
J: The analyte was positively identified; the associated
numerical value is the approximate concentration of the analyte
in the sample or result/LOQ is estimated due to quality control
issues identified during the verification or validation process;
•
N: The analysis indicates the presence of an analyte for which
there is presumptive evidence to make a “tentative
identification;”
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•
NJ: The analysis indicates the presence of an analyte that has
been “tentatively identified” and the associated numerical value
represents its approximate concentration;
•
UJ: The analyte was not detected above the reported LOQ;
however, the LOQ is approximate and may or may not
represent the actual LOQ necessary to accurately and precisely
measure the analyte in the sample; and
•
R: The sample result or LOQ is rejected due to serious
deficiencies in the ability to analyze the sample and meet QC
criteria. The presence or absence of the analyte cannot be
verified.
Memoranda documenting the results for all data reviews will be prepared
for each analytical data package or sample groups. Completed data
review memoranda will be submitted to the ERM Project Manager and
copies will be retained in the project file.
5.3
POTENTIAL LIMITATIONS ON DATA INTERPRETATION
Field and laboratory data generated for this project will be reviewed to
ensure that all project objectives are met. If any non-conformances are
found in the field procedures, sample collection procedures, field
documentation procedures, laboratory analytical and documentation
procedures, and data evaluation and quality review procedures, the
impact of those non-conformances on the overall project objectives will be
assessed. Appropriate actions, including resampling and reanalysis, may
be recommended to the project team so that the project objectives can be
accomplished.
Evaluation of field and laboratory QC data and/or audits conducted for
field operations and/or laboratory operations may indicate the need for a
corrective action. Problems with analytical QC data will be addressed by
the laboratory QC officer. Problems arising during field operations,
however, will be addressed by the Technical Lead through
communication of the identified problem and a proposed corrective action
to the ERM Project Manager. The ERM Project Manager will discuss the
appropriate actions with the HPD representative and EPA and MDE
Project Coordinators to obtain concurrence, and then relay this
information to the field personnel for implementation. The field
personnel will then report back to the ERM Project Manager upon
successful implementation of the corrective action.
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5.4
RECONCILIATION WITH PROJECT REQUIREMENTS
The project management team, QA Coordinator, and sampling and
analytical team members are responsible for ensuring that all
measurement procedures are followed as specified and that measurement
data meet the prescribed acceptance criteria. Prompt action must be taken
to correct any problem that may arise.
5.4.1
Conduct Preliminary Data Review
A preliminary data review will be performed to uncover potential
limitations to using the data, to reveal outliers, and generally to explore
the basic structure of the data. The first step is to review the quality
assurance reports. The second step is to calculate the BTVs, generate
graphical presentations of the data, and review these summary statistics
and graphs.
5.4.2
Draw Conclusions from the Data
If the sampling design and statistical tests conducted during the final
reporting process show results that meat acceptance criteria, it can be
assumed that the network design and the uncertainty of the data are
acceptable. This conclusion can then be reported to EPA.
5.5
REPORTS TO MANAGEMENT
This subsection describes the types of reports that may be produced for
the project. The types of reports that may be produced include daily data
summary tables, event logs, data quality assessment reports, PE and audit
reports, and the pre-construction summary report.
5.5.1
Daily Data Summary Tables
Daily data summary tables with hourly airborne Total PM concentrations
for each PAM and OAM station, hourly wind speed, wind direction and
daily rainfall will be prepared by the field staff.
5.5.2
Event Logs
When applicable, event logs will be generated to identify nonconforming
situations and corrective actions taken. Corrective actions to remedy a
nonconforming situation in the field can be defined by the ERM field
personnel or the ERM QA/QC Officer or PM. A description of the
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required action will be documented in an event log. Corrective actions
must be approved verbally by the QA/QC Officer prior to
implementation. Upon implementation of the corrective action, the ERM
QA/QC Officer or PM will be provided with the completed event log,
which becomes part of the project file. Copies of completed event log will
also be provided in the data summary reports.
5.5.3
Data Quality Assessment Reports
The field staff will report to the ERM PM, or a qualified designee on the
progress of each phase of field work and any QA/QC issues associated
with field activities. Additionally, the laboratory will maintain detailed
procedures for record-keeping and reporting to support the validity of all
analytical work. The Laboratory QA Manager will provide the ERM
QA/QC Officer certification documentation, including audit reports,
upon request. A data quality assessment will be included in the PreConstruction Report to ensure that the DQOs were met.
5.5.4
Performance Evaluation and Audit Reports
As discussed in Section 3.1, laboratory PEs and audits may be performed
during the course of the project. If performed, the ERM QA/QC Officer
will prepare a report summarizing the results.
5.5.5
Summary Data Reports
The summary data report titled, “Harbor Point Development PreConstruction Air Monitoring Report”, will be produced by ERM and will
include, electronically, the complete laboratory data packages, and all
underlying metadata.
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Figures
Figure 1—Project Organiza on Chart ERM Partner in Charge Harbor Point Development Project Manager, Jonathan Flesher Agency Project Lead EPA III ERM Project Manager Agency Project Lead MDE Darren Quillen Ed Dexter Russell Fish Leonard Rafalko ERM QA Manager Larry Ho enstein ERM Technical Lead Jeff Boggs ERM Project Health and Safety ERM Field Engineer Dan Hoadley Charles McClellen Subcontractors Lines of Authority Lines of Communica on Laboratory Data Consultants Eastern Research Group Data Validator Analy cal Lab Figure 2
Project Area
SITE
3
AREA 1
2
Figure 3
Pre-construction Air Monitoring Locations
Harbor Point
Baltimore, Maryland
OAM-2
OAM-1
MET
PAM-1
MET – Meteorological Station
PAM – Perimeter Air Monitor
OAM – Off-site Air Monitor
1 – Baltimore National Aquarium
2 – MDE’s Old Town Station
Figure 4
Construction Air Monitoring Locations
Harbor Point
Baltimore, Maryland
OAM-2
OAM-1
PAM-4
PAM-3
MET
PAM-3
MET – Meteorological Station
PAM – Perimeter Air Monitor
OAM – Off-site Air Monitor
1 – Baltimore National Aquarium
2 – MDE’s Old Town Station
PAM-1
Figure 5
ERM
Appendix A
Sample & Analysis Plans
Pre-construction Sampling and
Analysis Plan
Area 1, Phase 1 Development
Baltimore Works Site
Baltimore, Maryland
March 2014
By:
Environmental Resources Management Inc.
Harbor Point Development LLC
For:
U.S. Environmental Protection Agency – Region III
Maryland Department of the Environment
Pre-construction Sampling and Analysis Plan for
Area 1, Phase 1 Development
Baltimore Works Site
Harbor Point Development, LLC
1300 Thames Street, Suite 110
Baltimore, Maryland 21231
Date: 27 February 2014
Harbor Point Development, LLC, Project Manager: Jonathan Flesher
Environmental Resources Management, Inc., QA Officer: Larry
Hottenstein
For EPA use:
Approved by EPA Project
Manager:
Expedited Review?
Date:
G
Yes
G
No
Received by QA Office:
Date:
Reviewed by:
Date:
Approved:
Date
Region 3 Quality Assurance
Manager
TABLE OF CONTENTS
1.0
2.0
3.0
4.0
INTRODUCTION
1
1.1
SITE NAME
1
1.2
SITE LOCATION
2
1.3
RESPONSIBLE AGENT
2
1.4
PROJECT ORGANIZATION
2
1.5
STATEMENT OF THE SPECIFIC PROBLEM
5
BACKGROUND
6
2.1
SAMPLING AREA DESCRIPTION
6
2.2
OPERATIONAL HISTORY
6
2.3
PREVIOUS INVESTIGATIONS/REGULATORY INVOLVEMENT
7
2.4
ENVIRONMENTAL AND/OR HUMAN IMPACT
7
PROJECT DATA QUALITY OBJECTIVES
8
3.1
PROJECT TASK AND PROBLEM DEFINITION
8
3.2
DATA QUALITY OBJECTIVES (DQOS)
8
3.3
DATA QUALITY INDICATORS (DQIS)
9
3.4
DATA REVIEW AND VALIDATION
3.4.1
Field Data Review
3.4.2
Laboratory Data Review and Validation
13
13
14
3.5
DATA MANAGEMENT
15
3.6
ASSESSMENT OVERSIGHT
16
SAMPLING RATIONALE
17
4.1
TOTAL PARTICULATE MATTER MONITORING
17
4.2
HEXAVALENT CHROMIUM SAMPLING
17
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5.0
REQUEST FOR ANALYSES
19
5.1
ANALYSES NARRATIVE
19
5.2
ANALYTICAL LABORATORY
19
FIELD METHODS AND PROCEDURES
6.1.1
List of Equipment Needed
6.1.2
Calibration of Field Equipment
20
20
21
6.2
Total Particulate Matter
Hexavalent Chromium Sampling
21
21
22
7.0
SAMPLE CONTAINERS, PRESERVATION AND STORAGE
23
8.0
DISPOSAL OF RESIDUAL MATERIALS
25
9.0
SAMPLE DOCUMENTATION AND SHIPMENT
26
9.1
FIELD NOTES
9.1.1
Field Logbooks
9.1.2
Photographs
26
26
27
9.2
LABELING
27
9.3
SAMPLE CHAIN-OF-CUSTODY FORMS AND CUSTODY SEALS
28
9.4
PACKAGING AND SHIPMENT
28
6.0
10.0
AIR
6.2.1
6.2.2
QUALITY CONTROL
30
10.1
FIELD QUALITY CONTROL SAMPLES
10.1.1 Assessment of Field Contamination (Blanks)
10.1.2 Assessment of Field Variability
30
30
31
10.2
LABORATORY QUALITY CONTROL SAMPLES
31
11.0
FIELD VARIANCES
32
12.0
FIELD HEALTH AND SAFETY PROCEDURES
33
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LIST OF TABLES
1
PROJECT ORGANIZATION
2
SUMMARY OF QUALITY CONTROL PROCEDURES FOR CRVI
ANALYSIS
LIST OF FIGURES
1
SITE VICINITY
2
MONITORING STATION LOCATIONS
APPENDICES
A
STATION SITING INFORMATION
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1.0
INTRODUCTION
The Harbor Point, Area 1, Phase 1 Development will occur at a location
(the site) that was formerly a chromium chemical manufacturing facility.
The historical manufacturing processes at the site resulted in chromium
impacts to soil and groundwater. Hexavalent chromium (CrVI) is
considered by the EPA to be a known human carcinogen by the inhalation
route of exposure (EPA 2013). Inhalation of CrVI dusts is also associated
with non-cancer toxicity.
Phase 1 of the development project consists of the Exelon Tower and
Trading Floor Garage, the Central Plaza Garage, modifications to the
existing Transfer Station, general site development (streets, sidewalks,
etc.) and utilities, foundations, roadways, and other related site
development elements and remedy restorations for development.
Because of the dynamic nature of dust-disturbing activities during
construction, providing real time information on concentration levels of
particulates to project personnel during construction is necessary in order
that dust-generating activities on site can be appropriately controlled.
Real-time instrumentation is available to measure ambient concentrations
of total particulate matter (Total PM), but such instrumentation is not
available for measuring CrVI concentrations in real-time. Therefore, air
samples for measuring CrVI concentrations require laboratory analysis.
The goal of the pre-construction air monitoring and sampling is to collect
data for 15 consecutive calendar days at three (3) monitoring station
locations. In the event that samples cannot be collected (e.g. equipment
malfunction, severe weather conditions, etc.), an extra sampling day(s)
will be added to the schedule to make up for the lost sampling time so
that data has been collected for a total of 15 calendar days. The intended
use of the pre-construction air monitoring data is to obtain empirical data
to establish the Total PM action level and CrVI background concentration
to be utilized during construction.
1.1
SITE NAME
Baltimore Works
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1.2
SITE LOCATION
The site is located on a peninsula on the northeast shore of the Patapsco
River of the Inner Harbor, in the Fells Point section of Baltimore City,
Maryland (Figure 1).
1.3
RESPONSIBLE AGENT
Environmental Resources Management, Inc. (ERM) will be responsible for
the implementation and conduct of the air monitoring program for this
project. ERM is a leading global provider of environmental, health, safety,
risk, social consulting services and sustainability related services with
more than 5,000 people in over 40 countries and territories working out of
more than 150 offices. ERM’s Annapolis, MD office will provide the field
and project management staff and the Irvine, CA office will provide
quality control/assurance personnel for the project.
1.4
PROJECT ORGANIZATION
Table 1. Project Organization
Name
Jonathan
Flesher
Lenny Rafalko
Title/Role
Project
Manager
Partner-inCharge
HARBOR POINT DEVELOPMENT LLC
Organizational
Affiliation
HPD
ERM
2
Responsibilities
•
Oversees all project activities.
•
Directs the scope of work to the ERM PM.
•
Reviews and approves all documents and
coordinate transmittal of documents to
appropriate parties for review.
•
Communicates with stakeholders regarding
project activities.
•
Oversees entire program for ERM.
•
Reviews all final deliverables and invoices.
•
Seeks HPD feedback on performance of
project managers.
•
Addresses program-level issues.
MARCH 2014
Name
Darren
Quillen
Larry
Hottenstein
Title/Role
Project
Manager
QA/QC
Manager
HARBOR POINT DEVELOPMENT LLC
Organizational
Affiliation
ERM
ERM
3
Responsibilities
•
Reports to ERM Partner-in-Charge (Leonard
Rafalko) and HPD (Jonathan Flesher)
•
Directs ERM Field Manager and
subcontractors.
•
Communicates questions or issues to Agency
leads (Ed Dexter, MDE and Russell Fish,
EPA)
•
Ensures that assigned staff has been trained
in SOP implementation.
•
Ensures that all key decisions and project
deliverables are subjected to independent
technical review by qualified personnel
within the time frame of the project schedule.
•
Monitor subcontractor (CrVI analysis) for
compliance with both project and data quality
requirements records, costs, and progress of
the work and re-plan and re-schedule work
tasks as appropriate.
•
Ensure and document that QC checks on field
equipment are performed according to
schedule and meet acceptance criteria, and
the QA/QC
•
Resolves field QA/QC issues.
•
Audit sample preservation, handling,
transport, and custody procedures
throughout the project.
•
Review and approve all data reduction and
reporting procedures for inclusion in
deliverables.
•
Review and respond to audit assessment
findings, determine the root cause for any
nonconformance, confer with the ERM PM
and Partner in Charge on the steps to be
taken for correction, and ensure that
procedures are modified to reflect the
corrective action and are distributed to all
field personnel, including subcontractors.
•
Report QA and any procedural problems to
the ERM PM and Partner in Charge
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Name
Jeff Boggs
Charles
McClellan
Title/Role
Technical
Lead/ Field
Manager
Field
Technician
HARBOR POINT DEVELOPMENT LLC
Organizational
Affiliation
ERM
ERM
4
Responsibilities
•
Provide technical support to ERM’s PM, QA
Manager, and Field Technician as needed.
•
Reports to ERM PM.
•
Prepares and implements this SAP and
deliverables.
•
Ensures data collection activities are
consistent with approved SAP, SOP and
QAPP requirements.
•
Oversees evaluation of data received from the
laboratory in accordance with the project
requirements.
•
Prepares or oversees the preparation of
portions of the reports that summarize data
results and present conclusions.
•
Performs monitoring and collects samples
according to project approved QAPP, SOPs
and this SAP.
•
Reports to ERM Field Manager (if Field
Manager not available, report to ERM PM).
•
Communicates any problems or deviations
from project plans to ERM Field Manager.
•
Ensures that all data collection and handling
activities comply with applicable SOPs,
including audits conducted in the presence of
Agency personnel.
•
Prepares and maintains field forms,
notebooks, and equipment.
•
Implements technical procedures applicable
to tasks.
•
Inspects and accepts supplies and
consumables.
•
Coordinates and schedules sample shipment
to analytical laboratory to meet holding times
and analytical procedure specifications.
MARCH 2014
Name
Julie Swift
1.5
Title/Role
Project
Manager
Organizational
Affiliation
ERG
Responsibilities
•
Reviews and implements analytical
laboratory elements of this SAP with regards
to the CrVI analysis.
•
Manages analytical chemists to complete the
sample analyses selected in this SAP,
according to the approved methods.
•
Monitors, reviews, and documents the quality
of all analytical chemistry work performed by
ERG under this SAP.
•
Oversees management of analytical data.
•
Transmits completed data packages to the
ERM Quality Manager
•
Promptly informs the ERM’s Quality
Manager of any laboratory analytical
problems, data quality issues, or delays in
sample analysis.
•
Promptly responds to any data quality issues
identified through the independent data
validation process.
STATEMENT OF THE SPECIFIC PROBLEM
The problem being addressed is to ensure that representative and accurate
real-time particulate and airborne CrVI data are collected to define the
pre-construction particulate population reflective of routine background
conditions. This data will be used to generate Background Threshold
Values (BTVs) that in turn will be used to ensure that the site perimeter
and work zones are accurately monitored during construction to control
any potential release in a timely manner.
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2.0
BACKGROUND
Area 1 is the principal site of Honeywell’s (formerly AlliedSignal)
Baltimore Works Facility which included chromium processing
production and support buildings on an area that covered approximately
14 acres. The principal contaminant of concern in Area 1 is hexavalent
chromium (CrVI). An Environmental Remediation System (ERS) is
maintained and operated by Honeywell International Inc. (Honeywell) to
contain CrVI-impacted groundwater in Area 1 and control the potential
for human exposure to affected soil.
The site development must not interfere with the efficacy of the corrective
measures or Honeywell’s ability to comply with the performance
standards defined in the Consent Decree between Honeywell, the U.S.
Department of Justice, U.S. Environmental Protection Agency and the
Maryland Department of the Environment.
2.1
SAMPLING AREA DESCRIPTION
The site occupies approximately 14 acres in an urban area. The site is
bordered on the north by the Living Classrooms, on the west by a marina,
on the south by the Northwest Branch of the Patapsco River, and on the
east by the Thames Street Wharf office Building. The specific location of
the site is shown in Figure 1.
The original buildings and infrastructure associated with the Baltimore
Works chromium plant have been removed from the site. The ERS is
operated by Honeywell and consists of a Multimedia cap (MMC),
Hydraulic barrier, Head Maintenance System (HMS), a groundwater
storage and transfer system, and Outboard Embankment. A two-story
building, the Transfer Station, is currently in use in support of the HMS.
2.2
OPERATIONAL HISTORY
There are no operations at the site other than those associated with the
ERS. Those operations were initiated in 2002 following completion of
corrective actions. Approximately 60,000 gallons of chromium
contaminated groundwater are withdrawn annually by the HMS,
temporarily stored the Transfer Station tank room and transported off-site
for treatment at Environmental Quality of Pennsylvania.
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2.3
PREVIOUS INVESTIGATIONS/REGULATORY INVOLVEMENT
The sites has been the subject of numerous Agency-led investigations
dating back to 1989, leading to the approved corrective measures
implementation and are included in the administrative record.
2.4
ENVIRONMENTAL AND/OR HUMAN IMPACT
The primary concern is the potential for particulates containing CrVI to be
distributed on-site and off-site during the period of construction that
involves the disturbance of contaminated materials below the MMC. CrVI
is considered by the EPA to be a known human carcinogen by the
inhalation route of exposure (EPA 2013). Inhalation of CrVI dusts is also
associated with non-cancer toxicity.
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3.0
PROJECT DATA QUALITY OBJECTIVES
This section formulates the problem that the sampling needs to solve and
determines the level of data quality necessary to address the problem.
Specifically, data quality objectives and indicators are developed to ensure
that the collected data will be of sufficient quality to be able to adequately
address the problem.
3.1
PROJECT TASK AND PROBLEM DEFINITION
The purpose of the pre-construction air monitoring study is to collect
representative and accurate real-time airborne total PM and CrVI
laboratory analytical data to define the pre-construction particulate
population reflective of background urban conditions.
3.2
DATA QUALITY OBJECTIVES (DQOS)
Data quality objectives (DQOs) are quantitative and qualitative statements
that define study objectives, the appropriate type of data, specify tolerable
levels of potential decision errors, and define the performance criteria
limiting the decision errors.
This following describes decisions to be made based on the data and
provides criteria on which these decisions will be made.
•
Concisely describe the problem to be studied.
The problem being addressed is to ensure that representative and
accurate real-time particulate and airborne CrVI data are collected
to define the pre-construction particulate population reflective of
routine background conditions.
•
Identify what questions the study will attempt to resolve, and what
actions (decisions) may result.
What are the pre-construction real time airborne Total PM and
CrVI concentrations representative of routine city traffic conditions,
including transportation, industrial, construction, and other sources
of airborne Total PM and CrVI?
This data will be used to generate a Total PM Background
Threshold Value (BTV) that in turn will be used as the site-specific
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dust action level to ensure that the site perimeter and work zones
are accurately monitored during construction to control any
potential dust release in a timely manner.
•
Identify the information that needs to be obtained and the
measurements that need to be taken to resolve the decision
statement.
Real-time total PM (direct reading instrumentation) and particulate
CrVI data (laboratory analysis) using accurate, field and laboratory
methods, including data quality review from multiple sampling
locations (on site and off site) that are representative of urban
conditions in the vicinity of the site.
•
Define study boundaries and when and where data should be
collected.
The study boundaries are the atmosphere at the site and adjacent
urban area. Air monitoring stations will be located at the site
perimeter and at off-site locations representative of urban
conditions. The study will be conducted for a minimum of 15
consecutive calendar days and be completed prior to initiation of
development construction activities.
3.3
DATA QUALITY INDICATORS (DQIS)
Data quality indicators (accuracy, precision, completeness,
representativeness, comparability, and method detection limits) refer to
quality control criteria established for various aspects of data gathering,
sampling, or analysis activity. In defining DQIs specifically for the project,
the level of uncertainty associated with each measurement is defined.
ERM has reviewed, understands and agrees with the DQI’s defined by the
contract laboratory Eastern Research Group, Inc.’s (ERG) Standard
Operating Procedures (SOP), dated 14 February 2014, for hexavalent
chromium analysis per ASTM D7614. Based upon our review and
understandings of the DQIs provided in ERG’s SOP, ERM has determined
that the laboratory can meet the project needs.
•
Accuracy is the degree of agreement of a measurement with a
known or true value. To determine accuracy, a laboratory value is
compared to a known or true concentration determined by such
QC indicators as: matrix spikes, surrogate spikes, laboratory
control samples (blind spikes) and performance samples. For the
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Cr(VI) analyses covered under this SAP, accuracy will be
determined according to the ASTM method – a filter method spike
with acceptance criteria of 80% – 120%.
Accuracy shall be calculated as percent recovery of spiked analytes
as follows:
% Ri = (Yi ÷ X i ) × 100%
where:
•
%Ri
=
percent recovery for compound i
Yi
=
measured spike concentration in sample i
(sample concentration with the spike - original
sample concentration)
Xi
=
actual spike amount in sample i
Precision is the degree of mutual agreement between or among
independent measurement of a similar site setting. Precision is
expressed in terms of analytical variability. For this project,
analytical variability will be measured as the relative percent
difference (RPD) between results of duplicate monitors and
between results of co-located samplers.
Precision will be calculated as the RPD as follows:
where:
%RPDi
= Relative percent difference for compound i
Oi
= Value of compound i in original sample
Di
= Value of compound i in duplicate sample
Duplicate Total PM concentration data and co-located CrVI sample
concentration results (“primary” and “duplicate”) will be
compared to determine the RPD. The acceptable RPD for real-time
Total PM is <40% and for CrVI is <20%.
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•
Completeness is expressed as percent of valid usable data actually
obtained compared to the amount that was expected. According to
EPA guidance, completeness goals in the range of 75% - 95% are
typical. The target goal for completeness for this project is 100%
percent for all data, given the critical importance of the data in
establishing valid background concentrations. Completeness will
be calculated as follows:
%C =
A
x100%
I
where:
%C
=
Percent completeness (analytical)
A
=
Number of usable sample results reported (all
results not rejected)
I
=
Total number of results reported
Non-valid data (i.e., data qualified as “R” rejected) will be
identified during the data review and the reasons for rejection
explained in the data review report.
•
Representativeness is the expression of the degree to which data
accurately and precisely represent a characteristic of an
environmental condition or a population. It relates both to the area
of interest and to the method of taking the individual sample.
Representativeness of the environmental conditions at the time of
sampling will be achieved by selecting sampling locations,
methods, and times so that the data describe the urban air
conditions that the project seeks to evaluate. Representative
samples will also be ensured through following proper protocols
for sample handling (storage, preservation, packaging, custody,
and transportation), sample documentation, and laboratory sample
handling and documentation procedures.
•
Comparability expresses the confidence with which one data set
can be compared to another. The comparability goal will be
achieved by maintaining consistency in sampling conditions,
selection of sampling procedures, sample preservation methods,
and analytical methods as provided in ASTM D7614.
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The method detection limit for CrVI as provided by the contract
laboratory, ERG, is 0.0078 nanograms per milliliter (ng/mL) (0.0036
ng per cubic meter (M3) based on 21.6 M3 sample volume, i.e., 15
liters per minute for 24 hours).
Table 2 provides the summary of laboratory quality control procedures
and corrective actions for evaluating laboratory QC samples.
Table 2. Summary of Quality Control Procedures for CrVI Analysis
Parameter
Frequency
Acceptance Criteria Corrective Action
Initial 5point
calibration
standards
Before every
sequence
Initial
Calibration
Before
every
sequence,
following
the initial
calibration
Recovery 85-115%
One per
Batch,
following
the ICV
Below MDL
Verification
(ICV)
Initial
Calibration
Blank
(ICB)
Correlation
coefficient≥ 0.995
1) Repeat analysis of
calibration standards.
2) Prepare calibration
standards and reanalyze.
1) Repeat analysis of initial
calibration verification
standard.
2) Repeat analysis of
calibration standards.
3) Prepare calibration
standards and reanalyze.
1) Reanalyze.
2) Prepare blank and
reanalyze.
3) Correct contamination and
reanalyze blank.
4) Flag data of all samples in
the batch.
Continuing
Calibration
Verification
(CCV)
Laboratory
Control
Every 10
samples and at
the end of the
analytical
sequence
Recovery 85-115%
One per 10
samples
Recovery 80-120%
Duplicate
and/or
Replicate
samples only
RPD < 20% for
concentrations
greater than 5 x the
MDL.
2) Prepare CCV.
3) Flag data bracketed by
unacceptable CCV.
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1) Reanalyze.
2) Prepare spike and
reanalyze.
Sample
Replicate
Analysis
1) Repeat analysis of CCV.
12
1) Check integration
2) Check instrument function
3) Flag samples
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Parameter
Continuing
Calibration
Blank (CCB)
Frequency
After every
CCV and at
the end of the
sequence
Acceptance Criteria Corrective Action
Below MDL
1) Reanalyze.
2) Prepare blank and
reanalyze.
3) Correct contamination and
reanalyze blank.
4) Flag data of all samples in
the batch.
3.4
DATA REVIEW AND VALIDATION
This section describes data review, including what organizations or
individuals will be responsible for what aspects of data review and what
the review will include. Since the data need to be legally defensible, data
packages and data validation will be required. EPA defines validation as a
3rd party review of all laboratory data based on strict protocols. Data
reviewed include raw data such as standards log books, extractions logs,
instrument print outs, chromatograms (ifapplicable), mass spectra (if
applicable), etc. Calibration data, sample analysis data, and quality
control data are all evaluated.
3.4.1
Field Data Review
The process of reviewing field data will involve evaluating field records
for consistency and completeness (i.e., ensuring that each sample result is
fully supported by accurate metadata), reviewing QC and calibration
information, evaluating whether the SOPs were followed by conducting
and documenting a field audit, summarizing deviations and determining
their impact on data quality, summarizing the samples collected, and
providing a summary of the review in the project report.
Per ASTM Standard D7614-12, Section 13.6, the following conditions will
render a sample invalid:
1) Filters that are dropped or become contaminated with any foreign
matter (dirt, finger marks, ink); or
2) Filters with tears or pin holes; or
3) Start and stop flow rates differ by more than 10%: or
4) Filter samples collected by the samplers which operated less than
23 hours or more than 25 hours; or
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5) A power failure occurs during a sample run which causes the stop
time or sample duration requirements to be violated; or
6) Field blank fails if the concentration is higher than 3 times the
method detection limit.
Field and laboratory analytical data will be summarized in tables as
appropriate. ERM will perform a 100% check of all data presented on data
summary tables, including review of all CrVI sampler total air volumes.
3.4.2
Laboratory Data Review and Validation
The laboratory will review the data internally in accordance with its SOP
and established internal procedures prior to submitting the data to the
ERM PM. Specifically, the laboratory will review the data package to
ensure the following:
•
Sample preparation information is correct and complete;
•
Holding times have been met;
• Analytical information is complete and was generated within
acceptable criteria;
• Any discrepancies/corrective actions identified during sample
login, preparation or analysis have been addressed and
documented;
• The appropriate SOPs have been followed;
• QC samples were within established control limits;
• Analytical requirements have been met (e.g., the correct analytical
procedures were used as defined by the COC); and
• Documentation is complete and any QC issues are fully explained
in a detailed case narrative.
Following receipt of the laboratory report, ERM will send the report
(including raw data and all QA/QC information) to the designated thirdparty, independent validator. The third party will perform Level II
validation, as described in EPA’s Guidance on Environmental Data
Verification and Data Validation (2002).
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3.5
DATA MANAGEMENT
All data will be reviewed and verified by the ERM QA/QC Officer/PM or
qualified designee (interchangeable herein throughout this document with
“ERM PM”). The ERM PM will ensure that the field and technical data
obtained for the project will provide the end user with acceptable data. All
field and technical data shall be reviewed, by the ERM PM or a qualified
designee, such as the ERM QA/QC Officer, to ensure that the data is
accurate prior to the inclusion in the project report.
Data processing is summarized as follows:
1. The field data sheets (real-time Total PM and CrVI sampler), realtime instrument data logs, log books, and COC forms are submitted
(faxed, electronic, or hard copy) by field personnel to the ERM PM
weekly. The ERM PM, or their designee checks all forms for
accuracy and ensures that each unique sample ID is correctly
transposed across forms and logs accompanied by the correct
metadata, then stores the information electronically into ERM’s
project files.
2. Samples are sent to the laboratory under COC.
3. The laboratory enters the sample information into their tracking
system and performs the analysis.
4. The laboratory electronically submits raw data, sample results, and
their QA information to ERM and to an independent third party
validator, who in turn performs Level II validation, as described in
EPA’s Guidance on Environmental Data Verification and Data
Validation (2002).
5. ERM submits the field data sheets, real-time instrument data logs,
and COC forms to the third party validator.
6. The third party validator electronically submits their validation
report to ERM.
Real-time Total PM concentration data will be provided as hourly
averages based on one (1) minute frequency data collection. The daily
average real-time Total PM concentration data will be used to calculate the
dust action level, i.e., the background threshold value (BTV).
ERM reviews the data validation report, and, if acceptable, stores all data
into the project files. If the result(s) of a CrVI analysis is found
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unacceptable, ERM may request re-analysis of the data by the laboratory.
Under this condition, the ERM PM will bring this result to the attention of
EPA and MDE and request their concurrence of ERM’s recommendation
of whether or not to perform the re-analysis
3.6
ASSESSMENT OVERSIGHT
The QA program is described in the QAPP and is overseen by the QA/QC
Manager for the project, Larry Hottenstein. All audit and assessment
reports will be part of the project record and included in the final
sampling report. The QA/QC Manager, or their designee will ensure that
audits of data quality are being performed as follows:
•
One field audit is planned for the 15-day sampling period. The
audit will be conducted by the ERM QA/QC Manager and an
audit report and corrective action(s), if any, will be submitted to
the ERM PM. The field audit will include monitoring station
siting, instrument maintenance and calibration and the
initiation and recovery of a minimum of one CrVI sample.
•
The laboratory’s results of their latest laboratory audit and
performance evaluation (PE) sample are appended to the QAPP
to demonstrate laboratory compliance with QAQC
requirements.
•
The QA/QC Manager will review the field and lab quality
assessments conducted as described in Sections 3.4.1 and 3.4.2,
to ensure appropriate corrective actions are being taken, if
warranted, and direct additional corrective measures if deemed
necessary.
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4.0
SAMPLING RATIONALE
Air quality data for establishing pre-construction concentrations for Total
PM and particulate CrVI will be collected during a 15-day sampling
period at three, fixed locations; one location will include a duplicate Total
PM monitor and a duplicate CrVI sampler (60 CrVI samples collected in
total). The pre-construction air monitoring station locations (Figure 2)
were selected as representative of the site urban neighborhood
background ambient air conditions as follows:
4.1
•
Perimeter Air Monitor #1 (PAM-1) will be located approximately
400 feet east of Area 1, immediately adjacent to S. Caroline Street,
representative of the urban residential neighborhood background
air conditions;
•
Off-Site Air Monitor #1 (OAM-1) will be located approximately 0.5
miles west of the site at the Baltimore National Aquarium,
representative of Baltimore Inner Harbor waterfront background
air conditions; and
•
OAM – 2 will be located approximately 1.0 miles north of the site at
the Old Town monitoring station established by MDE,
representative of the urban background air conditions.
TOTAL PARTICULATE MATTER MONITORING
Real-time instrumentation is available to measure ambient concentrations
of total particulate matter (Total PM). DustTrak Model 8533 real-time dust
monitors have been selected for this study and are reported to monitor
Total PM concentrations for particle sizes ranging from approximately 0.1
microns to 15 microns in diameter and is reported measure Total PM
concentrations ranging from 1.0 µg/M3 to 150 mg/M3.
4.2
HEXAVALENT CHROMIUM SAMPLING
Concurrently with real-time monitoring for Total PM using the DustTrak
Model 8533, at each monitoring station location described above, airborne
CrVI concentrations will be determined from 24-hour air samples
collected using BGI Model PQ-100 samplers. CrVI air samples will be
analyzed in accordance with the Standard Operating Procedure for the
Preparation and Analysis of Hexavalent Chromium by Ion Chromatography as
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prepared by ERG, dated 14 February 2014. A copy of the ERG SOP is
provided in the QAPP, Appendix C.
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5.0
REQUEST FOR ANALYSES
This section describe the analytical support for the project depending on
several factors including the analyses requested, analytes of concern,
turnaround times, available resources, available laboratories, etc.
5.1
ANALYSES NARRATIVE
Air samples will be collected at three (3) locations, one of which will
include duplicate monitoring and co-located and sampling equipment.
Expedited turn-around time of three (3) business days will be requested
for the laboratory results for CrVI air samples to complete the study as
soon as practicable after 15 days of sampling. Duplicate CrVI air samples
will be collected at the PAM-1 co-located station location.
Air samples (including QC samples) will be analyzed for CrVI per ERG’s
SOP as provided in the project QAPP, Appendix C.
5.2
ANALYTICAL LABORATORY
ERG is an EPA contract laboratory and has provided their Standard
Operating Procedure for the Preparation and Analysis of Hexavalent Chromium
by Ion Chromatography, dated 14 February 2014, and provided in the
QAPP, Appendix C
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6.0
FIELD METHODS AND PROCEDURES
Descriptions of the equipment, methods and procedures that will be used
to accomplish the air sampling goals are provided in this section. It
should be noted that personnel involved in sampling must wear clean,
disposable, powder-free, nitrile gloves. Descriptions of sample tracking
and shipping are provided in Section 7.
6.1.1
List of Equipment Needed
The equipment and materials that will be used in the field to collect
samples are listed below:
•
DustTrak Model 8533 monitors will be operated in the field to
collect real-time Total PM concentration data. . One (1) back-up
DustTrak Model 8533 monitor will be available throughout the
study;
•
BGI PQ-100 samplers will be used to collect air samples for CrVI
laboratory analysis. One (1) back-up DustTrak Model 8533 and one
(1) back-up BGI PQ-100 sampler will be available throughout the
study;
•
Bios Defender 510-H primary flow calibrator;
•
Laboratory prepared filters mounted in holders;
•
Teflon tubing and connectors;
•
Shipping coolers and packing/sealing supplies;
•
Electric extension cords and ground fault interrupter/surge
protectors;
•
Weather proof equipment cases and tripods;
•
Disposable, powder-free, nitrile gloves and Teflon tweezers;
•
Maintenance tool kit; and
•
First Aid kit.
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6.1.2
Calibration of Field Equipment
The DustTrak Model 8533 monitors will be calibrated daily at the
beginning and end of each 24-hour sampling period utilizing a BIO
Defender 510-H primary air flow calibration meter. The BGI-PQ100
samplers monitors will be calibrated daily at the beginning and end of
each 24-hour sampling period utilizing a BGI TetraCal primary air flow
calibration meter. The DustTrak Model 8533 monitor beginning flow rate
will be calibrated to two (2) Lpm and the BGI-PQ100 sampler will be
calibrated to 15 Lpm, with the air sampling media attached to the sampler.
Equipment maintenance and calibration records for the project will be
maintained at the site office and in project files stored on ERM’s server.
Details of calibration methods are included in the SOPs for each
instrument being utilized for the project in the QAPP, Appendix B. All
calibration information will be recorded daily on the field data sheets also
provided in the project QAPP, Appendix B. Field data sheets will be
transmitted daily to the ERM office, checked as described above, and
stored on ERM’s secure server.
6.2
AIR
6.2.1
Total Particulate Matter
Fixed, Total PM air monitoring locations will be established in the field as
shown on Figure 2. DustTrak Model 8533 real-time dust will be operated
continuously 24 hours per day, seven (7) days per week at the three (3)
monitoring station locations during the 15 consecutive days of preconstruction air monitoring program for measurement of Total PM
concentrations. DustTrak Model 8533 monitors will be operated at two (2)
Lpm and will be calibrated daily at the time of the CrVI sample recovery.
Air sampling inlets will be set at a height of no less than two (2) meters
above ground surface. The siting requirements described in 40 CFR Part
58, Appendix E will be used as guidance. The duplicate DustTrak Model
8533 monitors at PAM-1 will be connected to a “T” to ensure the same air
stream is being monitored by both instruments.
Specific monitoring station siting information including exact locations,
labeled aerial and ground level photographs, and electric power and
security provisions is provided in Appendix A.
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6.2.2
Hexavalent Chromium Sampling
Fixed CrVI air sampling locations will be established in the field as shown
on Figure 2. BGI-PQ100 air samplers will be operated continuously 24
hours per day, seven (7) days per week at the three (3) monitoring station
locations during the 15 consecutive days of pre-construction air
monitoring program for laboratory analysis of CrVI concentrations. BGIPQ100 air samplers will be operated at 15 Lpm and will be calibrated daily
at the time of the CrVI sample recovery.
Air sampling inlets will be set at a height of no less than two (2) meters
above ground surface. The siting requirements described in 40 CFR Part
58, Appendix E will be used as guidance. The co-located BGI-PQ100 air
samplers at PAM-1 will be sited two (2) to four (4) meters apart.
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7.0
SAMPLE CONTAINERS, PRESERVATION AND STORAGE
Air samples will be collected using laboratory provided nitric acid and
sodium bicarbonate pre-treated filters mounted into filter holders.
Laboratory prepared filters/holders will be shipped from the laboratory,
maintained in the field, and returned to the laboratory frozen at 0°C.
The following procedure will be used for installation and recovery of the
filter holder containing the sample filter and sample inlet apparatus.
1) Ensure that the sample media are delivered to the sample site
within a cooler with ice packs to keep the filters cold and protected
from the elements.
2) Prior to installation of the filter holder and glass funnel apparatus
onto the PQ100 sampler, ensure that the sampler is free of dust and
debris buildup. Wipe the sampler down with a damp cloth as
appropriate.
3) Wearing powder-free nitrile gloves, remove the filter holder from
its packaging. Note the filter ID (if so identified by the lab). If the
filter is not marked with an identifying number, mark the filter
holder packaging with an appropriate sample ID indicating sample
location, day, and time. Record all sample media identification on
the field data sheet. The field data sheet is included as an
attachment to this SOP and is also used as the COC (Chain-ofCustody).
4) Mark the corresponding glass funnel inlet assembly packaging with
the same identification parameters as the filter holder.
5) Loosen the nut on the filter holder outlet fitting and remove the
Teflon plug. Store the Teflon plug in the filter holder packaging to
protect it from contamination. Install the filter holder onto the end
of the stainless steel U-tube by inserting the tubing into the filter
holder outlet fitting and tightening the nut.
6) Leave the Teflon plug in the inlet side of the filer holder until ready
to perform the initial flow rate verification.
7) After ensuring all sample run data has been collected from the
PQ100 unit, including the total sample volume, replace the Teflon
plug in the filter holder inlet and tighten the nut.
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8) Remove the filter holder from the sampler by loosening the nut on
the outlet fitting and removing form the stainless steel U-tube.
9) Replace the Teflon plug at the filter holder outlet and tighten the
nut.
10) Place the sample holder into a labeled, zip-lock plastic bag and
place in the cooler with ice packs as soon as possible to maintain
sample integrity during storage and shipping.
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8.0
DISPOSAL OF RESIDUAL MATERIALS
In the process of collecting environmental samples during the air
monitoring study, the ERM sampling team will generate different types of
potentially contaminated IDW that include the following:
•
Used personal protective equipment (PPE) in the form of used
nitrile gloves.
•
Disposable sampling equipment in the form of Teflon tweezers.
The EPA's National Contingency Plan (NCP) requires that management of
IDW generated during sampling comply with all applicable or relevant
and appropriate requirements (ARARs) to the extent practicable. The
sampling plan will follow the Office of Emergency and Remedial
Response (OERR) Directive 9345.3-02 (May 1991), which provides the
guidance for the management of IDW. In addition, other legal and
practical considerations that may affect the handling of IDW will be
considered.
•
Used PPE and disposable equipment will be double bagged and
placed in a municipal refuse dumpster. These wastes are not
considered hazardous and can be sent to a municipal landfill.
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9.0
SAMPLE DOCUMENTATION AND SHIPMENT
9.1
FIELD NOTES
Field records (sample collection sheets and field logs of daily activities)
will be maintained in the field office and on ERM’s server and will include
logbooks, preprinted sampling data forms, photographs, sample shipment
tracking logs and copies of sample Chain of Custody.
9.1.1
Field Logbooks
Field logs will be used to document daily field activities and will be
prepared and maintained by the Field Technician responsible for air
monitoring. Preprinted sampling data forms will also be utilized to
document specific sampling information. At a minimum, the following
information will be recorded during the collection of each sample:
•
Sample location and description
•
Sampler's name(s)
•
Date and time of sample collection
•
Designation of sample as composite or grab
•
Type of sample (air)
•
Type of sampling equipment used
•
Field instrument readings and calibration
•
Field observations and details related to analysis or integrity of
samples (e.g., weather conditions, damaged filter media, etc.)
•
Sample preservation
•
Lot numbers of the sample containers, sample identification
numbers and any explanatory codes, and chain-of-custody form
numbers
•
Shipping arrangements (overnight air bill number)
•
Name(s) of recipient laboratory(ies)
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In addition to the sampling information, the following specific
information will also be recorded in the field logbook for each day of
sampling:
9.1.2
•
Team members and their responsibilities
•
Time of arrival/entry on site and time of site departure
•
Other personnel on site
•
Summary of any meetings or discussions with tribal, contractor, or
federal agency personnel
•
Deviations from sampling plans, site safety plans, and QAPP
procedures
•
Changes in personnel and responsibilities with reasons for the
changes
•
Levels of safety protection
•
Calibration readings for any equipment used and equipment model
and serial number
Photographs
Photographs will be taken at the sampling locations. They will serve to
verify information entered in the field logbook. For each photograph
taken, the following information will be written in the logbook or
recorded in a separate field photography log:
9.2
•
Time, date, location, and weather conditions
•
Description of the subject photographed
•
Name of person taking the photograph
LABELING
All samples collected will be labeled in a clear and precise way for proper
identification in the field and for tracking in the laboratory. The samples
will have preassigned, identifiable, and unique numbers. At a minimum,
the sample labels will contain the following information: station location,
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date of collection, analytical parameter(s), and method of preservation.
Every sample will be assigned a unique sample number.
9.3
SAMPLE CHAIN-OF-CUSTODY FORMS AND CUSTODY SEALS
All sample shipments for analyses will be accompanied by a chain-ofcustody (COC) record. COC’s will be completed and sent with the
samples to the laboratory and each shipment (i.e., each day).
The chain-of-custody form will identify the contents of each shipment and
maintain the custodial integrity of the samples. Generally, a sample is
considered to be in someone's custody if it is either in someone's physical
possession, in someone's view, locked up, or kept in a secured area that is
restricted to authorized personnel.
Samples will be maintained prior to and following sampling in a
dedicated, secured freezer inside the Honeywell Transfer Station at the
project site. Until the samples are shipped, the custody of the samples will
be the responsibility of ERM. The sampling Field Technician will sign the
chain-of-custody form in the "relinquished by" box and note date, time,
and air bill number.
The sample numbers for all filter media blanks, field handling blanks and
duplicates will be documented on this form (see Section 10.0). A
photocopy will be made for the EPA’s and MDE’s project files.
A self-adhesive custody seal will be placed across the top of each sample
filter holder. The shipping containers in which samples are stored will be
sealed with self-adhesive custody seals any time they are not in someone's
possession or view before shipping. All custody seals will be signed and
dated.
9.4
PACKAGING AND SHIPMENT
All sample containers will be placed in a strong-outside shipping
container. The following outlines the packaging procedures that will be
followed for low concentration samples.
1.
Ice packs will be used to eliminate melting ice from damaging the
sample holders..
2.
The bottom of the cooler should be lined with bubble wrap to
prevent breakage during shipment.
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3.
Check filter holder inlet and outlet caps for tightness.
4.
Secure container tops with clear tape and custody seal all
container tops.
5.
Affix sample labels onto the containers with clear tape.
6.
Seal all sample containers in heavy duty plastic zip-lock bags.
Write the sample numbers on the outside of the plastic bags with
indelible ink.
7.
Place samples in a sturdy cooler lined with Styrofoam and plastic.
Enclose the appropriate COC(s) in a zip-lock plastic bag affixed to
the underside of the cooler lid.
8.
Fill empty space in the cooler with bubble wrap or Styrofoam
peanuts to prevent movement and breakage during shipment.
9.
Ice packs will be used to maintain the 0oC temperature
requirement during shipping.
10. Each cooler will be securely taped shut with fiberglass strapping
tape, and custody seals will be affixed to the front, right and back
of each cooler.
Records will be maintained by ERM’s PM of the following information:
•
Sampling contractor's name (if not the organization itself).
•
Name and location of the site.
•
Total number of samples shipped to the laboratory.
•
Carrier, air bill number(s), method of shipment (priority next day).
•
Shipment date and when it should be received by lab.
•
Irregularities or anticipated problems associated with the samples.
•
Whether additional samples will be shipped or if this is the last
shipment.
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10.0
QUALITY CONTROL
This section describes the quality control samples that are being collected
to support the sampling activity, including field and trip blank samples.
All quality control samples will be sent to the laboratory blind.
10.1
FIELD QUALITY CONTROL SAMPLES
Field quality control samples are intended to help evaluate conditions
resulting from field activities and are intended to accomplish two primary
goals: assessment of field contamination; and assessment of sampling
variability. The former assesses for substances introduced in the field due
to environmental or sampling equipment and is assessed using blanks of
different types. The latter assesses variability due to sampling technique
and instrument performance as well as variability possibly caused by the
heterogeneity of the matrix being sampled and are assessed using
replicate sample collection. The following sections cover field QC samples.
10.1.1
Assessment of Field Contamination (Blanks)
Field contamination is usually assessed through the collection of different
types of blanks. Field blanks are sample containers handled in the field.
Trip blanks are prepared by the laboratory and shipped to and from the
field.
10.1.1.1
Field Blanks
Field blanks are collected during air sampling. One (1) field blank is
prepared each day sampling occurs in the field. These blanks are
submitted "blind" to the laboratory, packaged like other samples and each
with its own unique identification number.
The field blanks will be preserved, packaged, and sealed in the manner
described for the CrVI air samples. A separate sample number and station
number will be assigned to each sample, and it will be submitted blind to
the laboratory.
10.1.1.2
Trip Blanks
Trip blanks will be prepared to evaluate if the shipping and handling
procedures are introducing contaminants into the samples. A minimum of
one trip blank will be submitted to the laboratory for analysis with every
shipment of samples for CrVI analysis. Trip blanks are filter media that
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have been shipped to the site prior to sampling. The sealed trip blanks are
not opened in the field and are shipped to the laboratory in the same
cooler with the samples collected for CrVI analyses. The trip blanks will
be preserved, packaged, and sealed in the manner described for the CrVI
samples. A separate sample number and station number will be assigned
to each trip sample and it will be submitted blind to the laboratory.
10.1.2
Assessment of Field Variability
Duplicate samples are collected simultaneously with a standard sample
from the same source under identical conditions into separate sample
containers. Field duplicates will be collected using a co-located sampler.
Each duplicate portion should be assigned its own sample number so that
it will be blind to the laboratory. A duplicate sample is treated
independently of its counterpart in order to assess laboratory performance
through comparison of the results. At least 10% of samples collected per
event will be field duplicates.
Duplicate real-time Total PM concentration data and CrVI samples will be
collected daily at sample location PAM-1.
Duplicate samples will be collected from this monitoring station because
the location is closest to the project site and is representative of urban
neighborhood ambient air conditions.
Duplicate samples will be preserved, packaged, and sealed in the same
manner as other samples of the same matrix. A separate sample number
and station number will be assigned to each duplicate, and it will be
submitted blind to the laboratory.
10.2
LABORATORY QUALITY CONTROL SAMPLES
Laboratory quality control (QC) samples are analyzed as part of standard
laboratory practice. The laboratory monitors the precision and accuracy of
the results of its analytical procedures through analysis of QC samples. In
part, laboratory QC samples consist of matrix spike and duplicate samples
for CrVI analyses. The term "matrix" refers to use of the actual media
collected in the field.
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11.0
FIELD VARIANCES
As conditions in the field may vary, it may become necessary to
implement minor modifications to sampling as presented in this plan.
When appropriate, the QA Officer, EPA and MDE representatives will be
notified and a verbal approval will be obtained before implementing the
changes. Modifications to the approved plan will be documented in the
sampling project report.
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12.0
FIELD HEALTH AND SAFETY PROCEDURES
Project-specific health and safety procedures that must be followed in the
field include the use of clean, disposable, powder-free, nitrile gloves
whenever handling the sampling tubing, connectors or sample filter
media. Potential hazards that may be encountered are electric shock
caused by contact with operating electronic monitoring or sampling
equipment during wet sampling periods. Caution must be taken at all
times to maintain dryness inside the water proof cases protecting the
electronic equipment, thereby protecting field personnel from possible
electric shock.
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Figures
Figure 1
Site Location Map
SITE
3
AREA 1
2
Figure 2
Pre-construction Air Monitoring Locations
Harbor Point
Baltimore, Maryland
OAM-2
OAM-1
MET
PAM-1
MET – Meteorological Station
PAM – Perimeter Air Monitor
OAM – Off-site Air Monitor
1 – Baltimore National Aquarium
2 – MDE’s Old Town Station
APPENDIX A
SITING INFORMATION
Baltimore City/Inner Harbor Vicinity – Air Monitoring Station Locations
OAM-1
OAM-1
PAM-1
Perimeter Air Monitor (PAM-1)
900 Block S. Caroline Street
Baltimore, MD 21231
Lat./ Long. provided
Electric power from and secure to
parking lot light pole
(Same location as AM-3 during Apr. –
Jun. 2013 study.)
PAM-1
Off-Site Air Monitor (OAM-1)
Baltimore National Aquarium
501 E. Pratt Street
Baltimore, MD 21202
Lat./ Long. provided
Electric power from light pole. Site
behind and secure to concrete bench.
(Same location as OAM-2 during Jun. –
Jul. 2013 study.)
Off-Site Air Monitor (OAM-2)
Thomas J. Burke Fire Station
1100 Hillen Street
Baltimore, MD 21202
Lat./ Long. provided
Electric power from MDE shelter. Site
inside fenced area and secure to chain
link fence.
(MDE Monitoring Location)
OAM-2
Appendix B
Field Sampling Method SOPs
Field Sampling Protocol and Standard Operating Procedure
REAL-TIME AIR SAMPLING FOR TOTAL PARTICULATE MATTER
IN AMBIENT AIR
February 2014
FIELD SAMPLING PROTOCOL AND STANDARD OPERATING PROCEDURE
REAL-TIME AIR SAMPLING FOR TOTAL
PARTICULATE MATTER IN AMBIENT AIR
February 2014
By:
Environmental Resources Management Inc.
Harbor Point Development LLC
For:
U.S. Environmental Protection Agency – Region III
Maryland Department of the Environment
TABLE OF CONTENTS
APPENDICES ................................................................................................................................ I
1.0
INTRODUCTION ............................................................................................................ 1
2.0
EQUIPMENT LIST .......................................................................................................... 1
3.0
HEALTH AND SAFETY .................................................................................................. 2
4.0
MONITOR SET-UP AND OPERATION ..................................................................... 2
4.1
DRX AEROSOL MONITOR MODEL 8533................................................................. 2
4.2
INSTALLATION .............................................................................................................. 3
5.0
INITIAL MONITOR SETUP AND PROGRAMMING ............................................. 3
5.1
INSTRUMENT SETUP.................................................................................................... 3
5.2
SETUP MENU .................................................................................................................. 4
5.3
ZERO CALIBRATION .................................................................................................... 5
5.4
SAMPLE FLOW RATE SETTING ................................................................................. 6
5.5
MONITOR DATE AND SETTINGS.............................................................................. 7
6.0
MONITOR OPERATION .............................................................................................. 8
7.0
TAKING MASS CONCENTRATION MEASUREMENTS......................................... 9
8.0
ALARM ............................................................................................................................ 11
9.0
MONITOR MAINTENANCE....................................................................................... 14
10.0
CONTACTS..................................................................................................................... 18
APPENDICES
A
ERM
FIELD DATA SHEET
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1.0
INTRODUCTION
This protocol and standard operating procedure (SOP) is intended to provide a general
overview and step-by-step instructions for personnel in the field responsible for carrying
out real-time ambient air sampling for total particulate matter (Total PM). The
instructions cover assembly of the instrument, instrument programming and operation,
deployment and field data recording. This SOP has been prepared in accordance with
the guidance documents Guidance for Preparing SOPs (USEPA 2007) and Quality
Assurance Handbook for Air Pollution Measurement Systems (USEPA 1994, USEPA 2008).
This document assumes that instrument location siting has already been successfully
completed ensuring each location meets the acceptable criteria with regards to the
proximity of obstructions (i.e. buildings, trees, etc.), technician safety, and any potential
contamination contributions from surrounding operations.
2.0
EQUIPMENT LIST
The following equipment will be required for the air monitoring program:
•
DustTrak® DRX Aerosol Monitor Model 8533, including:
•
•
•
•
•
o TrakPro™ Software
o Zero Filter
o Power Supply
o 6600 mAH Lithium Ion Rechargeable Battery
o USB Cable
o Analog alarm/output cables
o Calibration Certificate
o Spare Internal Filter Elements
o Flexible Teflon tubing and connectors
BIOS Defender 510-H Air Flow Calibrator unit;
Laptop PC with TrakPro™ Software;
Waterproof case for each instrument;
Rigid stand with legs to support Waterproof case 2 meters above ground; and
Field data sheets – provided in Appendix A, clipboards, pens.
Additional Field Supplies:
•
•
•
ERM
Miscellaneous tools (wrenches, screwdrivers, pliers, etc.);
Electric extension cords;
Ground Fault Interrupter power strips
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•
•
3.0
Personal protective equipment (PPE), see the site specific Health and Safety Plan
(HASP);
Field notebook.
HEALTH AND SAFETY
All monitoring activities undertaken at the Site must be completed under the approved,
site-specific HASP. The HASP identifies the hazards, personal protective equipment,
monitoring, and emergency procedures for conducting work at the Site. Monitoring and
support personnel must acknowledge their review of the HASP prior to performing
work at the Site.
4.0
MONITOR SET-UP AND OPERATION
4.1
DRX AEROSOL MONITOR MODEL 8533
The monitor used within this SOP is the DustTrak® DRX Aerosol Monitor Model 8533
(the “monitor”) manufactured by TSI Incorporated. The monitor employed during this
program uses TrakPro™ Software. The DRX 8533 monitors Total PM concentration and
stores 1-minute averages on an internal data logger. The instrument measures real-time
aerosol mass readings using light-scattering laser photometers for particles
approximately 15 µm or less in diameter. The DRX 8533 monitors can be operated at
flow rates up to three (3) liters per minute (Lpm). Figure 1 presents the typical DRX
8533 monitor.
Figure 1. DRX8533
For purposes of this monitoring program, the DRX 8533 monitor will be operated in the
“Total” mass concentration channel, i.e., Total PM data collection without the particle
size impactor.
ERM
The DRX 8533 contains an internal 6600 mAH Lithium Ion rechargeable battery. For
purposes of this monitoring program, AC power will be available for providing the
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monitor with constant power therefore the internal battery will only be used to maintain
instrument operation in the event monitoring could be interrupted by AC power loss.
4.2
INSTALLATION
This document assumes that sample locations have already been sited and adhere to the
proper sample location criteria. The monitor should be placed on a reasonably level
surface with the sample inlet at a height of no less than two (2) meters with
unobstructed air flow for at least 270 degrees around the monitor.
For duplicate
monitoring, each monitor will be connected to the same monitor inlet.
The monitors should be secured from the effects of wind loading to prevent tipping over
in elevated wind conditions. The tripod stand with weatherproof case housing the
monitor can be secured with cinder blocks on each leg and will be attached by chain
with lock to an unmovable object to protect from theft.
5.0
INITIAL MONITOR SETUP AND PROGRAMMING
5.1
INSTRUMENT SETUP
The DustTrak DRX monitor can be connected to a computer to download data and
upload sampling programs.
Connecting to the Computer
Connect the USB host port of a Microsoft® Windows®-based computer to the
USB device port on the side of the DustTrak monitor.
Installing TrakPro™ Data Analysis Software
TrakPro software can preprogram the DustTrak monitor, download data, view
and create raw data and statistical reports, create graphs, and combine graphs
with data from other TSI instruments that use TrakPro software. The following
sections describe how to install the software and set up the computer.
ERM
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Note
To use TrakPro software with the DustTrak Aerosol Monitor, the PC must
be running Microsoft Windows® and the computer must have an
available Universal Serial Bus (USB) port.
®Microsoft and Windows are registered trademarks of Microsoft Corporation
1. Insert the TrakPro Data Analysis Software CD into the CD-ROM drive.
The install screen starts automatically.
Note
If the software does not start automatically after a few minutes, manually
run the program listed on the label of the CD using the Run command on
the Windows Start Menu.
2. Follow the directions to install TrakPro software.
TrakPro software contains a comprehensive installation guide. TSI recommends
printing out this guide prior to starting the TrakPro software installation on your
computer, so it may be consulted during the installation. The TrakPro Software
manual is located in the Help file in TrakPro software. There is no separately printed
TrakPro Data Analysis software manual.
5.2
SETUP MENU
Pressing Setup activates the Setup Menu touchscreen buttons along the left edge of the
screen. Setup is not accessible when the instrument is sampling.
The main screen of the Setup screen displays the following information:
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Serial Number
Model Number
Firmware
Calibration Date
Pump Run Time
Cum Mass Conc.
Cum Filter Conc.
Filter Time
5.3
The instruments serial number.
The instruments model number.
Instruments current version of firmware.
Date of the last factory calibration.
Pump running time in hours.
Amount of mass run through instrument over life.
Amount of mass run through instrument since last filter
h of last filter change.
Date
ZERO CALIBRATION
TSI recommends performing a zero check prior to each use for the DustTrak monitor,
before running any extended tests, and after the instrument experiences a significant
environmental change. Examples of significant environmental changes would be
ambient temperature changes that exceed 15°F (8°C) or moving from locations with high
aerosol concentrations to low concentrations.
Zeroing Instrument
Run Zero Cal prior to every 24-hour sampling event. Zero Cal requires that the zero
filter be attached prior to running. Zero Cal must also be performed if the unit is reading
negative concentrations. It is not possible for the DustTrak monitor to read negative
concentrations. Negative concentrations are a symptom of zero drift.
ERM
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Zero Cal
Never perform a zero cal. without attaching a zero filter.
1. Press Zero Cal Button
2. Attach Zero Filter
3. Press the Start button to start Zeroing process.
4. A count-down clock will appear indicating the time remaining. The screen
with indicate Zero Cal Complete when done.
Remove filter after zeroing has been completed. The instrument is now zero calibrated
and ready for use.
5.4
SAMPLE FLOW RATE SETTING
For purposes of this monitoring program, the flow rate setting shall be 2.0 Lpm. For
DustTrak DRX Model 8533, the flow cannot be changed. Run Flow Cal to calibrate the
flow set point. The flow set point is factory set to 3 Lpm total flow; two (2) Lpm of the
total flow is measured aerosol flow, and one (1) Lpm of total flow is split off, filtered,
and used for sheath flow. There is an internal flow meter in the DustTrak DRX
instrument that controls flow rate to ±5% if factory set point. TSI recommends checking
the flows with an external flow reference meter, especially when collecting data. The
pump will automatically start when entering the Flow Cal screen.
ERM
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Flow Cal
1. Attach a flow calibrator (BIOS Defender 510-H) to inlet port.
2. Move the arrows up or down to achieve desired flow on the reference flow
meter. Each up or down arrow will change the flow about 1%. Allow time
between button presses to let pump change to the new flow rate.
3. Select Save once the desired flow rate is achieved. Select Undo to return to the
factory set point.
4. Record the calibration data in the field logbook.
5.5
MONITOR DATE AND SETTINGS
Set the DRX 8533 to the correct date and time prior to use. Follow the procedure below
for setting the monitor date and time.
Settings
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Settings screen sets basic unit parameters:
Set current date, current time and date/time format. Time can be set in 12 or 24 hour
format. Date can be set in yyyy/dd/mm, yyyy/mm/dd or mm/dd/yyyy. The date
format for the project will be yyyy/mm/dd to ensure consistency with the format
adopted all other sampling documentation.
6.0
MONITOR OPERATION
Follow the procedure below for operating the DRX 8533 aerosol monitor:
The RunMode tab brings up sampling mode options.
Run Mode
Sampling mode options include Survey Mode, Manual Log, and Log Mode 1-5.
ERM
Survey
Survey Mode runs a real time, continuous active sample, but does
not log data.
Manual
Manual Log sets the instrument to log data for a specified run
time
Log Modes
Log Mode starts and stops the instrument at specified times, run for a
specified test length, and perform multiple tests of the same length
with a specified time period between tests.
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FEBRUARY 2014
The Manual sampling mode is to be set for this project.
Manual Mode
Log Interval
The log interval can be set from 1 second to 60 minutes. It is the amount
of time between logged data points.
Test Length
Test length can be set from 1 minute to the limit of the data storage.
Time Constant Time Constant can be set from 1 to 60 seconds. This will control the
update rate of the main screen. It is the rolling average of data
displayed on the main screen and is not linked to logged data in either
Manual or Program Log modes.
The Log Interval will be set to one (1) minute, the Test Length will be set to allow 24hours storage (“storage limit”) and the Time Constant will be set to one (1) second for
this project. In Manual mode, data will be stored to a file named ―Manual_XYZ where
XYZ is an incrementing integer.
7.0
TAKING MASS CONCENTRATION MEASUREMENTS
Measurements are started and controlled from the main screen. The Total mass
concentration will be selected for measurement and display. Prior to starting a
measurement the instrument should be zeroed from the Setup screen and the run mode
should be configured and selected from the RunMode screen.
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FEBRUARY 2014
When the instrument is on, but not taking any mass measurements the start button will
be green and instruments pump will not be running. To start taking a measurement,
press the green Start button.
While taking a measurement the screen will display the current measured mass
concentration. The various regions of the screen are shown below:
Screen Regions
Display Mode
Run Mode
File Name
Test Progress
Mass Fractions
Error Indicators
Mass Fractions
Shows the size segregated mass measurements. The
Region (live keys) highlighted channel displayed in larger font on the left can
be changed by touching on the screen the measurement of
most interest on the right- hand side of the screen. Set the
Total channel as the highlighted display during monitoring.
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FEBRUARY 2014
Display Mode
Region
(live key)
The size segregated mass fractions displayed in this area can be
selected by touching in the ―Display mode region. The modes
that can be selected with this live key are:
All: PM1, PM2.5, Resp. PM10 and Total
IAQ-ENV: PM1, PM2.5 PM10 and Total
IH: Resp., PM10 and Total
Run Mode Region Shows the run mode selected from the
RunMode screen.
File Name Region Displays the file name to which the data is currently being
saved.
8.0
Test Progress
Region
Shows the time-based progress of the test.
Error
Indicator
Shows the current stats of the instrument
ALARM
Alarm allows you to set alarm levels on any of the 5 mass channels PM1, PM2.5, RESP,
PM10 and Total. However, the alarm functioning is determined by the logging interval.
The alarm will turn ON only if the average concentration over the logging interval
exceeds the set point. If the logging interval is too long and the concentration exceeds
the set point and stays at that level, the alarm will not turn ON until after the logging
interval has passed. Likewise, the alarm will not stop until after the concentration has
dropped below 5% of the threshold and after the logging interval has passed.
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FEBRUARY 2014
The Alarm is dependent on the logging interval. For the DustTrak to alarm as soon as
the Alarm Setpoint is exceeded, the logging interval must be set as low as possible (i.e., 1
second or 2 seconds). If long test durations do not permit setting such a short logging
interval, use the STEL alarm instead. The STEL is always based on 1 second
concentrations and is independent of the logging interval. For more details on the STEL
alarm, see section below on STEL.
In Survey mode, the alarm is dependent on the time constant.
Alarm1
Setpoint [mg/m3]
Relay1 [On, Off]
When the relay alarm is turned on, unit will close
relay switch when Alarm1 level is surpassed.
Relay alarm can only be linked to one mass channel at
a time.
Relay selection is available on the 8533 desktop
model only.
STEL 1 [On, Off]
When the STEL alarm is turned on, STEL data will
be collected when Alarm1 level is surpassed.
STEL alarm can only be linked to one mass channel at
a time.
STEL selection is available on the 8533 desktop
model only.
S
ll i setpoint
STEL N
The falarm2
is the mass concentration level
Alarm2 Setpoint
[mg/m3]
Alarm2 Enable [On,
Off]
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The alarm1 setpoint is the mass concentration level
upon which the alarm1 is triggered.
Alarm will trigger if the mass concentration, taken at
the logging interval, rises above the setpoint.
Note: Alarm 2 must be lower than Alarm 1 when both
alarms are enabled.
upon which the alarm2 triggers.
Alarm triggers if the mass concentration, taken at the
logging interval, rises above the setpoint.
Note: Alarm 2 must be lower than Alarm 1 when both
alarms are enabled.
Enables Alarm2 to be logged and will activate the
Audible or Visible alarms if they are enabled.
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FEBRUARY 2014
Audible [On, Off]
Visible [On, Off]
When the audible alarm is turned on, the instrument
will activate internal beeper when Alarm1 or Alarm2
level is surpassed.
Audible alarm can only be linked to one mass channel
When the visible alarm is turned on, unit will show the
alarm icon (Alarm1
, Alarm 2
) in title bar when
Alarm1 or Alarm2 level is surpassed.
The STEL Alarm will be used for this project and will be set to 80% of the projectspecific dust action limit.
STEL Alarm
STEL stands for Short Term Exposure Limit. When a STEL alarm is selected, the
instrument will inspect the data on a second by second basis, independent from the
selected logging interval. If the mass exceeds the STEL limit, a STEL alarm triggers and
the following actions will be taken.
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STEL indicator
The STEL indicator will show Red on the main screen.
Data
Data will be taken off the STEL alarm channel at a 1
minute logging interval for 15 minutes.
This data will be stored in a separate file named
STEL_XXX, where XXX will be matched to the logged
data file.
The instrument will also continue to log the mass
concentration data at the logging interval selected.
STEL Alarm repeat
If the instrument remains over the STEL limit after the
15 minute interval, or if the instrument exceeds the
STEL limit later during the sample period, additional
STEL files will be generated.
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FEBRUARY 2014
9.0
MONITOR MAINTENANCE
The DustTrak DRX Aerosol Monitor requires maintenance on a regular basis. The table
below lists the factory recommended maintenance schedule.
Some maintenance items are required each time the DustTrak monitor is used or on
an annual basis. Other items are scheduled according to how much aerosol is drawn
through the instrument. For example, TSI recommends cleaning the inlet sample
3
tube after 350 hours of sampling a 1 mg/M concentration of aerosol. This
recommendation should be pro-rated according to how the instrument is used. 350
3
hours at 1 mg/M3 is the same amount of aerosol as 700 hours at 0.5 mg/M or 175
3
hours at 2 mg/M , etc.
Recommended Maintenance Schedule
Item
Perform zero check
Clean inlet
Clean 2.5 µm calibration impactor
Replace internal filters
Return to factory for cleaning and calibration
(For 8533EP, TSI recommends that both the
DustTrak monitor and the External Pump
Module be returned to TSI)
Replace the internal HEPA filters in the
External Pump module
Frequency
Before each use.
3
350 hr. at 1 mg/m *
Before every use.
3
350 hr. at 1 mg/m * or
when indicated by the main screen filter error
indicator.
Annually
Annually
*Pro-rated, see discussion above.
The DustTrak monitor keeps track of the accumulated amount of aerosol drawn through
it since its last cleaning. When the internal filter replacement is due, the filter error
indicator will turn from green to red.
Cleaning the Inlet
The inlet should be cleaned based on the schedule in Table 4–1.
1. Turn the DustTrak monitor off.
2. Unscrew the inlet nozzle from the instrument.
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FEBRUARY 2014
Unscrew Inlet Nozzle
3. Clean the inlet port. Use a cotton swab to clean the outside of the inlet port. The
swabs can be dampened with water or a light solvent (e.g., isopropanol). Clean
the inside of the sample tube by using a small brush, along with a light solvent.
Dry the tube by blowing it out with compressed air, or let it air-dry thoroughly.
Do NOT Blow into Instrument
a. Screw (hand-tighten) inlet back into instrument.
Replacing the Internal Filters
Replace the internal filters based on the schedule in Table 4–1 or when the filter
indicator on the main screen changes to red.
1. Turn the instrument off.
2. Remove old filters from the instrument.
Desktop Model
a. Open filter access door on the back of the instrument.
b. Use the enclosed filter removal tool (PN 801668) to unscrew the filter cap.
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FEBRUARY 2014
c. Pull out single cylindrical filter from filter well. If filter well is visibly dirty,
blow out with compressed air.
Pull out Single Cylindrical Filter from Filter Well
d. Put a new filer (P/N 801673) back into filter well and screw filter cap back
into place.
e. Open blue retention clip by pinching ends inward and pushing down.
Open Blue Retention Clip
f.
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Remove 37-mm filter cassette by pulling downward and outward.
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FEBRUARY 2014
Remove 37-mm Filter Cassette
g. Open filter cassette using enclosed tool PN 7001303.
Open Filter using Enclosed Tool
h. Remove screen mesh from filter cassette and blow out using compressed air. Blow in
reverse direction to remove captured particulate.
i. Replace mesh in filter cassette and press halves together. Ensure filter has been fully
closed. The filter tool PN 7001303 can be used to ensure the filter is fully closed.
Replace Mesh in Filter Holder
j.
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Place filter cassette back into position and close blue retaining clip. Make sure
retaining clip snaps back into place.
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FEBRUARY 2014
3. It is important to reset the instruments filter counter after replacing filters. Resetting
the counter will clear the filter error condition shown on the main screen. Reset the
counters by the following:
a. Turn on the instrument.
b. Press the Setup button to go into the setup screen.
c. Touch the Cum Filter Conc.: (live key) to reset the aerosol mass.
d. Replace user serviceable filters? Dialog will appear. Press OK.
e. Reset filter concentration? Dialog will appear. Press Yes to reset the cumulative
filter concentration to zero.
e. The Setup screen will not show zero for the Cum Filter.
f. Concentration and the current date for the Filter Time.
10.0
CONTACTS
In the event you must reach ERM for any reason please use the following contact
information:
Jeff Boggs – Field Project Manager
Mobile:
(443) 803-8495
Email:
[email protected]
Larry Hottenstein – QA Manager
Office:
(949) 623-4700
Mobile:
(949) 294-9775
Email:
[email protected]
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FEBRUARY 2014
APPENDIX A
Field Data Sheet
Field Form Real Time Particulate Matter for ERM
DustTrak DRX Aerosol Monitor Model 8533
Pre-construction Air Monitoring Area 1, Phase 1 Development, Baltimore Works Site, Baltimore, MD
ERM WO
199768
Date
Field Technician (Print and Sign Name)
Others Present During Equipment Calibration, Operation or Maintenance? Provide Name(s)
Weather Observations (rain, dry, windy, etc.)
Photographs and any observed ambient conditions that may have potential to affect equipment operation or results?
Jeff Boggs – Field Project Manager
Mobile:
(443) 803-8495
Email:
[email protected]
Larry Hottenstein – QA Manager
Office:
(949) 623-4700
Mobile:
(949) 294-9775
Email:
[email protected]
Darren Quillen – Project Manager
Office:
(410) 972-0234
Mobile:
(410) 991-9568
Email:
[email protected]
Chuck McClellan – Field Technician
Office:
(410) 972-4127
Mobile:
(410) 937-7640
Email:
[email protected]
Comments Regarding Site Security (appears secure, evidence of tampering, etc.)
Recommendations for Corrective Actions
Are PAM-1 and PAM-1 Duplicate connected to the same inlet?
Any evidence of power loss?
Indicate if Recommended Maintenance Performed
Perform Zero Check before each use
Clean Inlet at 350 hours at 1 milligram per cubic meter
Clean 2 um calibration impactor before every use
Location ID
PAM-1
PAM-1 Duplicate
OAM-1
OAM-2
Serial ID
Start Time (24
hour clock)
Yes
No
Calibration Using BIOS Defender 510-H
End Time (24
hour clock)
Start Flow (Lpm)
End Flow (Lpm)
Photos of Start and End and Other Comments
Field Sampling Protocol and Standard Operating Procedure
Sampling of Hexavalent Chromium in Ambient Air
February 2014
The world’s leading sustainability consultancy
FIELD SAMPLING PROTOCOL AND STANDARD OPERATING PROCEDURE
Sampling of Hexavalent Chromium in Ambient Air
February 2014
Prepared by:
Environmental Resources Management
Air Measurements Group
3281 E. Guasti Rd. Suite 300
Ontario, CA 91761
The world’s leading sustainability consultancy
TABLE OF CONTENTS
1.0
INTRODUCTION ............................................................................................................ 1
2.0
EQUIPMENT LIST .......................................................................................................... 1
3.0
HEALTH AND SAFETY .................................................................................................. 2
4.0
SAMPLE MEDIA AND RECEIPT FROM LABORATORY....................................... 2
5.0
SAMPLER APPARATUS, ASSEMBLY, AND INSTALLATION .............................. 2
6.0
5.1
BGI PQ100 APPARATUS................................................................................... 2
5.2
BGI PQ100 ASSEMBLY AND RETROFIT ....................................................... 4
5.3
BGI PQ100 INSTALLATION AT THE SAMPLE SITE .................................. 7
INITIAL SAMPLER SETUP AND PROGRAMMING............................................... 7
6.1
SAMPLE FLOW RATE SETTING ..................................................................... 7
6.2
SAMPLER DATE, TIME, TEMPERATURE, AND BAROMETRIC
PRESSURE SETTINGS ....................................................................................... 9
7.0
SAMPLE MEDIA INSTALLATION ............................................................................ 11
8.0
SAMPLER PRE-TEST FLOW VERIFICATION AND INITIATING A SAMPLE
RUN ................................................................................................................................. 12
8.1
9.0
10.0
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PRE-TEST FLOW VERIFICATION ................................................................ 12
SAMPLE RECOVERY ................................................................................................... 14
9.1
SAMPLE RUN ENDING AND FINAL FLOW VERIFICATION
PROCEDURES ................................................................................................... 14
9.2
SAMPLE REDEPLOYMENT............................................................................ 15
SAMPLE STORAGE, PACKAGING, AND SHIPPING........................................... 16
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
11.0
QUALITY ASSURANCE/QUALITY CONTROL ...................................................... 17
11.1
FIELD BLANKS.................................................................................................. 17
11.2
TRIP BLANKS .................................................................................................... 18
11.3
FLOW RATE CALIBRATION ......................................................................... 18
11.4
DAILY FLOW RATE VERIFICATIONS ......................................................... 18
12.0
SAMPLER MAINTENANCE........................................................................................ 18
13.0
CONTACTS..................................................................................................................... 18
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
1.0
INTRODUCTION
This protocol and standard operating procedure (SOP) is intended to provide a general overview and stepby-step instructions for personnel in the field responsible for carrying out ambient air sampling for
hexavalent chromium (CrVI). The instructions cover assembly of the sampler apparatus, sampler
programming and operation, sample media preparation, deployment, sampling, monitoring/checking, field
data recording, sample recovery, labeling, chain-of-custody procedures, and final shipping to the
analytical laboratory.
This document assumes that sample location siting has already been successfully completed ensuring
each location meets the acceptable criteria with regards to the proximity of obstructions (i.e. buildings,
trees, etc.), technician safety, and any potential contamination contributions from surrounding operations.
2.0
EQUIPMENT LIST
The following equipment will be required for the sampling program:
• BGI Model PQ100 Sampler Kits Including:
PQ100 Sampler with firmware version 6.0 or 1.0M or higher
Tripod base assembly with legs
Downtube assembly
Retrofit kit from Eastern Research Group (ERG)
 BGI flow adapter fitted with a stainless steel Swagelock union
 ¼” Stainless steel U-tube
 Pre-cleaned Teflon filter holder pre-charged with a pre-cleaned sodium
bicarbonate impregnated cellulose fiber filter
 Glass funnel inlet assembly
o PQ101 battery charger/AC power supply
o CQ2 PC Communication Adapter Cable
o Flexible tubing for pump connection
BGI tetraCal (formerly triCal) Calibrator unit (Note: Dry calibrators and rotometers are not
recommended);
Laptop PC with BGI software installed – software available for download at
http://www.bgiusa.com/aam/portable.htm;
Field data sheets/ chain-of-custody (COC) – provided in Attachment-A, clipboards, pens;
Rigid coolers with ice packs - filters are to be kept at 0 °C or below at all times except during the
actual sample periods;
Secure, on-site freezer for temporary sample storage.
o
o
o
o
•
•
•
•
•
Additional Field Supplies:
•
•
•
•
•
•
•
•
•
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Miscellaneous tools (wrenches, screwdrivers, pliers, etc.);
Hand-held GPS with extra batteries;
Camera;
Personal protective equipment (PPE), see the site specific Health and Safety Plan (HASP);
Shipping supplies;
Field notebook;
Powder-free Nitrile gloves;
Ziploc bags;
Laser print label maker – hand printed labels are also acceptable.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
3.0
HEALTH AND SAFETY
All sampling activities undertaken at the Site must be completed under an approved, site-specific HASP.
The HASP identifies the hazards, personal protective equipment, monitoring, and emergency procedures
for conducting work at the Site. Samplers and support personnel must acknowledge their review of the
HASP prior to performing work at the Site.
4.0
SAMPLE MEDIA AND RECEIPT FROM LABORATORY
The sodium bicarbonate impregnated cellulose fiber filters will arrive pre-loaded into pre-cleaned Teflon
filter holders from ERG eliminating the need for technicians to directly handle the filters both during presampling setup and post-sampling recovery procedures. The filter holders will also arrive with a precleaned glass funnel sample inlet assembly. The filter holders will arrive in a cooler with frozen ice packs
and must be kept in the freezer until ready for deployment into the field.
The Teflon filter holders have inlet and outlet connections that accept ¼” OD tubing using Swagelok style
compression fittings. Each filter holder will arrive with a Teflon plug inserted into both the inlet and
outlet to seal against contamination until ready for deployment.
The glass funnel inlet apparatus will also arrive pre-cleaned from the laboratory and should remain sealed
in its packaging until deployment into the field for sampling.
5.0
SAMPLER APPARATUS, ASSEMBLY, AND INSTALLATION
5.1
BGI PQ100 APPARATUS
The sampler used within this SOP is the Model PQ100 Air Sampler manufactured by BGI Incorporated.
The unit employed during this program uses firmware version 6.0 or 1.0M or higher. The PQ100 uses a
programmable pump and associated control logic that allows the unit to monitor its own air flow rate and
adjust the pump speed to compensate for changes in load pressure and/or other forces that may affect the
air flow rate. This allows the user to maintain a steady flow rate through the sample media throughout the
sample duration. Figure 5-1 presents the typical PQ100 sampler and an example of installation on the
tripod assembly. Figure 5-2 presents a simplified schematic of the PQ100 and associated process flow.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
Figure 5-1.
BGI PQ100 Sampler and Installation on Tripod Assembly
Figure 5-2.
BGI PQ100 Sample System
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
For purposes of this monitoring program, the PQ100 sampler will be operated without the particle size
selector and filter holder shown in Figures 5-1 and 5-2. The sampler will be retrofitted with a custom
apparatus supplied by ERG. The retrofit replaces the typical BGI F20 filter holder and particle sizing
inlet with a section of stainless steel tubing used to attach a Teflon filter holder assembly and glass funnel
inlet apparatus.
Air is drawn by the pump through the glass funnel sample inlet and through the sample media, into the
stainless steel U-tube, through the downtube into the flow sensor. The signal generated by the sensor is
then routed to a microprocessor which determines if the flow is at the set point value and adjusts the
pump speed as necessary to maintain the correct flow rate. A pulsation damping volume has been
incorporated into the unit to compensate for pulsation effects from the pump.
The PQ100 contains an internal 12-volt battery but can also be operated using an external 12-volt deep
cycle battery. For purposes of this test program, AC power will be available for providing the sampler
with constant power therefore the internal 12-volt battery will only be used to maintain sampler operation
in the event sampling is interrupted by AC power loss.
5.2
BGI PQ100 ASSEMBLY AND RETROFIT
Refer to Figures 5-4 and 5-5 as well as the BGI PQ100 Instruction Manual and Quick Start Guide during
assembly of the PQ100 sampler apparatus. The sampler will be assembled without the use of the particle
size inlet (01), water jar (03), filter holder adapter (161), F20 filter holder, and brace (163) as shown in
Figure 5-4 and will instead be fitted with the ERG retrofit apparatus as shown in Figure 5-5. The item
numbers listed below in the following steps will refer to the Figure 5-4 schematic.
1. Unpack the instrument and legs checking the packing list against received items. Attach the legs
(160) to the rigid base (11A) using attached knurled snap lock fittings.
2. Attach the downtube (162) onto the cylindrical base fitting in the rigid stand. The filter holder
adapter (161) and F20 filter holder that typically go between the base and the downtube are
omitted (See Figure 5-5).
3. Attach the flow adapter piece fitted with the stainless steel Swagelok fitting onto the top of the
downtube. This piece is supplied by ERG specifically for this retrofit (See Figure 5-5).
4. Attach the stainless steel U-tube supplied by ERG to the Swagelok fitting on top of the flow
adapter and tighten the nut. Make sure that the inlet to the stainless steel tubing is capped off
until ready to attach the sample media to avoid potential contamination.
5. Set the PQ100 pump into the stand, screw in the hose adapter, and attach the flexible hose from
the pump to the downtube base.
6. Attach the PQ101 battery charger/AC power supply to the PQ100 unit and place up inside the
charger box and hook along the edge of box.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
7. Plug the other end into standard 115-120 VAC, 15-amp power. If using an extension cord, ensure
that the cord has been inspected and is in good operating condition with no cracks or frays of the
insulation and uses a proper three-prong grounded plug. Protect the power connection (AC plug)
from moisture and possible shorting by sealing the connection using nylon electrical tape. If
possible, also place the connection in an area protected from weather such as beneath the sample
platform (if so equipped). A plastic Ziploc bag sealed around the connection has also been used
successfully.
8. It is recommended that the unit be plugged in for at least 24 hours prior to sample initiation to
allow the internal battery to charge.
Figure 5-4.
Standard PQ100 Assembly
Note: The BGI particle size selector (01), water jar (03), filter holder adapter (161), F20 filter holder, and
brace (163) will be omitted and replaced by the retrofit apparatus shown in Figure 5-5.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
Figure 5-5.
ERM
PQ100 Assembly with ERG Retrofit
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
5.3
BGI PQ100 INSTALLATION AT THE SAMPLE SITE
This document assumes that sample locations have already been sited and adhere to the proper sample
location criteria. The sampler should be placed on a reasonably level surface with the sample inlet at a
height of 2-15 meters (EPA-specified breathing zone). The height of the sample inlet should be
appropriate as assembled but should be double-checked to ensure sampling no less than 2 meters above
ground and with unobstructed air flow for at least 270 degrees around the sampler. For collocated
sampling, each sampler should be placed at a distance of no less than 2 meters and no more than 4 meters
from each other and have sample inlet heights that differ by no more than 1 meter (in most situations
using collocated samplers the sample inlets will be at the same approximate height).
The samplers should be secured from the effects of wind loading to prevent tipping over in elevated wind
conditions. Weighted wooden platforms have been used during prior test programs for adjusting the
height of the sampler and securing the sampler firmly to the ground. Attaching 1’ lengths of 2”x4”
boards to the feet of the stand using lag bolts and securing with sandbags has also been used successfully.
6.0
INITIAL SAMPLER SETUP AND PROGRAMMING
6.1
SAMPLE FLOW RATE SETTING
The PQ100 may be delivered from the supplier with a default setting of 16.67 lpm based on the EPA
standard. For purposes of this test program, the flow rate setting shall be 15.0 lpm. To set the flow rate
to 15.0 lpm, choose the “Set Flow Rate” option in the main menu of the PQ100 and set the value to 15.0
lpm. After setting the flow rate, perform a calibration of the PQ100 following the calibration procedure
outlined below using the tetraCal unit in direct or manual modes. Use a spare ERG filter assembly
marked “calibration” for performing the flow setting and calibration. You will not use the glass funnel
sample inlet for the initial flow calibration.
First ensure the PQ100 unit is set to “Volume Flow” under the “Select F Unit” menu title. See procedure
below.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
Attach the tetraCal unit to the inlet of the calibration filter holder assembly using an appropriate length of
¼” OD Teflon or polyethylene tubing. The tubing should fit directly into the filter holder inlet and be
secured and sealed by tightening the nut. Attach the other end of the tubing to the tetraCal unit. You may
need to use a piece of flexible rubber tubing to attach the ¼” Teflon tubing to the tetraCal inlet. Follow
the instructions below as presented in the BGI PQ100 Instruction Manual to calibrate the PQ100 flow rate
setting to 15.0 lpm. Record the calibration data in the field logbook.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
If the tetraCal unit is not available, then use of an equivalent flow rate standard is acceptable for
calibrating the PQ100 in manual mode as outlined above. Note that piston-type dry calibrators and
rotameters are not recommended as calibration standards for the PQ100.
6.2
SAMPLER DATE, TIME, TEMPERATURE, AND BAROMETRIC PRESSURE
SETTINGS
Set the PQ100 to the correct date and time prior to use. Follow the procedure below for setting the
sampler date and time.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
The tetraCal unit can be used to calibrate the temperature and barometric pressure of the PQ100 as well.
These parameters should already be in calibration when received from the equipment supplier however if
it is observed that the temperature and barometric pressure parameters are potentially out of calibration,
follow the procedures below to calibrate these parameters using the tetraCal unit. Record any calibrations
performed in the field logbook.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
7.0
SAMPLE MEDIA INSTALLATION
Follow the procedure below for installation of the filter holder containing the sample filter and sample
inlet apparatus. Refer to Figure 5-5 for an example of the completed sampler unit.
1) Ensure that the sample media are delivered to the sample site within a cooler with ice packs to
keep the filters cold and protected from the elements.
2) Prior to installation of the filter holder and glass funnel apparatus onto the PQ100 sampler, ensure
that the sampler is free of dust and debris buildup. Wipe the sampler down with a damp cloth as
appropriate.
3) Wearing powder-free nitrile gloves, remove the filter holder from its packaging. Note the filter
ID (if so identified by the lab). If the filter is not marked with an identifying number, mark the
filter holder packaging with an appropriate sample ID indicating sample location, day, and time.
Record all sample media identification on the field data sheet. The field data sheet is included as
an attachment to this SOP and is also used as the COC (Chain-of-Custody).
4) Mark the corresponding glass funnel inlet assembly packaging with the same identification
parameters as the filter holder.
5) Loosen the nut on the filter holder outlet fitting and remove the Teflon plug. Store the Teflon
plug in the filter holder packaging to protect it from contamination. Install the filter holder onto
the end of the stainless steel U-tube by inserting the tubing into the filter holder outlet fitting and
tightening the nut.
6) Leave the Teflon plug in the inlet side of the filer holder until ready to perform the initial flow
rate verification.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
8.0
SAMPLER PRE-TEST FLOW VERIFICATION AND INITIATING
A SAMPLE RUN
The sample runs conducted during this test program will be initiated and terminated manually by the field
technician. This eliminates the need for programming the PQ100 for pre-determined start/stop times and
run durations. As such, procedures for programming pre-set start/stop times have been omitted from this
SOP.
8.1
PRE-TEST FLOW VERIFICATION
A pre-test flow rate verification will be conducted following the installation of the filter holder assembly
and prior to initiation of the sample run in order to ensure proper operation and flow rate of the PQ100.
Following installation of the filter holder assembly onto the stainless steel U-tube, connect the tetraCal
unit (or other primary flow standard) to the inlet of the filter holder as was done during the initial flow
rate setting calibration. Follow the instructions below for performing the initial flow rate verification:
1) Manually start the PQ100 from the menu presented below by selecting the “Run Now” option.
2) Allow the unit to warm up for 5 minutes. The display should read the actual flow, standard flow,
barometric pressure, and elapsed time as shown below.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
3) After warm up, record the flow rate reading indicated by the tetraCal and the PQ100. The unit is
acceptable if the flow rate indicated by the PQ100 is within ±4.0% of the flow indicated by the
tetraCal unit.
4) Stop the pump by depressing the “Enter” button. See the example screenshot below.
5) Detach the tetraCal unit at the filer holder inlet and replace the Teflon plug.
6) Wearing powder-free nitrile gloves, remove the glass funnel sample inlet assembly from its
packaging (ensuring once again that the packaging has been appropriately labeled to correspond
to the filter holder).
7) Loosen the nut on the filter holder inlet fitting and remove the Teflon plug. Store the Teflon plug
in the filter holder packaging to protect from contamination. Install the glass funnel sample inlet
assembly onto the filter holder by inserting into the inlet fitting of the filter holder and tightening
the nut.
8) After installation of the filter holder and glass funnel inlet assemblies, the sampling run is ready
to begin. Start the sampling run by depressing the “Enter” button to start the sample pump. The
run data recorded by the PQ100 during the initial flow rate verification should reset once the new
sampling run is started. Record all of the following parameters on the field data sheet:
•
•
•
•
•
•
•
•
•
•
Operator Name
Sample ID
Sample Location
Sampler Serial No.
Sample Start Date
Sample Start Time
Initial Elapsed Time reading (should be 00:00)
Ambient Temperature and Pressure (current instantaneous values)
Sample flow (aLpm and sLpm)
Note any unusual or notable activities in the area in the comments section
9) The sample event is now running. Operate the sampler for a period of 24 hours ± 30 minutes.
Repeat this procedure for each additional sample location making sure to stagger the start times
of each sample location to allow enough time for the completion of recovery and re-deployment
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
procedures (presented below) at each location prior to the anticipated end time of the previous
sample.
9.0
SAMPLE RECOVERY
9.1
SAMPLE RUN ENDING AND FINAL FLOW VERIFICATION PROCEDURES
Samples will be operated for a period of 24 hours ± 30 minutes. Make sure to plan ahead in order to
arrive at the sample locations in time to end the sample event while also allowing enough time for
preparation of recovery and re-deployment procedures. Follow the instructions below for sample
recovery and re-deployment:
1) After arriving at the sample location, ensure the sampler continued to operate normally
throughout the sample period and that nothing has been disturbed. Note any issues encountered
or potential disturbances on the field data sheet. Note also any unusual activities in the
surrounding area.
2) Record the final sample flow rate (aLpm and sLpm) on the field data sheet. Stop the sample
pump by depressing the “Enter” button as described above in item No. 4 of Section 8.1. The
PQ100 screen will display the run parameters as indicated below.
3) Record the data on the filed data sheet including:
a.
b.
c.
d.
e.
f.
g.
h.
i.
j.
Sample End Date
Sample End Time
Total Elapsed Sample Time
Ambient temperature and barometric pressure (current instantaneous values)
Average barometric pressure (on PQ100)
Average temperature (on PQ100)
Total sample volume (on PQ100)
Average flow rate
Total calculated standard volume
Note any unusual or notable activities in the area in the comments section
4) Wearing powder-free nitrile gloves, remove the glass funnel inlet assembly from the filter holder
and place into the original packaging that has been properly labeled. Store in the sample media
cooler with ice packs.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
5) Attach the tetraCal (or other flow standard) to the inlet of the Teflon filter holder with the Teflon
tubing used during the calibration and initial flow verification.
6) After ensuring all sample run data has been collected from the PQ100 unit, re-start the pump. As
the unit had previously been running and was manually shut down after then end of the sample
period, it should already be at or near operating temperature and therefore the warmup period will
be minimal. Obtain the flow rate readout from the tetraCal unit after two minutes of warmup
time. Record this data on the field data sheet under the final flow rate verification.
7) Disconnect the tetraCal unit from the inlet of the filter holder.
8) Replace the Teflon plug in the filter holder inlet and tighten the nut.
9) Remove the filter holder from the sampler by loosening the nut on the outlet fitting and removing
form the stainless steel U-tube.
10) Replace the Teflon plug at the filter holder outlet and tighten the nut.
11) Per ASTM Standard D7614-12, Section 13.6, the following conditions will render the sample
invalid:
a. Filters that are dropped or become contaminated with any foreign matter (dirt, finger
marks, ink; or
b. Filters with tears or pin holes; or
c. Start and stop flow rates differ by more than 10%: or
d.
Filter samples collected by the samplers which operated less than 23 hours or more than
25 hours; or
e. A power failure occurs during a sample run which causes the stop time or sample
duration requirements to be violated; or
f.
Filed blank fails if the concentration is higher than 3 times the method detection limit.
12) Ensure there is no excess dust or debris on the outside of the filter holder and return the sample
into its packaging from the laboratory that was previously labeled. As soon as possible place the
sample into the cooler with ice packs to maintain sample integrity during storage and shipping.
13) If sample run data is to be downloaded from the PQ100 unit, do so at this time using a laptop
computer with the appropriate BGI software.
9.2
SAMPLE RE-DEPLOYMENT
If excessive dust or debris is observed on the sampler, use a damp cloth to wipe down the unit before
proceeding to installation of sample media and initiation of the next sample run.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
Following recovery of the sample at a particular location and any maintenance activities, prepare the next
sample for deployment following the procedures outlined in the sections above. Install the filter holder,
perform the initial flow rate verification, install the glass funnel sample inlet assembly, and initiate the
sample run, recording all data as outlined in the previous sections. It is suggested that each location be
recovered and re-deployed before moving on to the next sample location. Make sure to stagger the start
times at each location during the program initiation to allow sufficient time to conduct recovery and
redeployment procedures at each location while maintaining the ability to end sampling at each location
at approximately the 24-hour mark ± 30 minutes.
10.0
SAMPLE STORAGE, PACKAGING, AND SHIPPING
Once the samples from all locations have been recovered and new samples have been deployed, take the
cooler containing the recovered samples to a clean location protected from the wind; a lab or office
location is recommended. Follow the instructions below for storage and preparation for shipping.
1) Ensure that enough ice packs is available for keeping all of the samples cold during transport
from the site and during shipping. Samples can be stored sealed in their packaging in the freezer
until ready for shipping. The hold time for these samples is a maximum of 10 days.
2) The field data sheets filled out for each sample location are also to be used as the laboratory COC
forms for each sample. Fill out the appropriate “Field Recovery” section with the relinquishing
individual and date/time. Normally these data sheets will be provided by the laboratory in
triplicate forms in which the original will remain with the samples during return shipping and the
collector will keep the back copy. If however the forms are not provided as triplicate, make
copies of all data sheets/COCs prior to sending with the samples. Original copies are retained
and the copy will accompany the samples.
3) Line the bottom of the cooler with brown paper packing material then add a layer of ice packs.
Do not use bubble wrap or foam packing peanuts as this tends to deplete the ice packs much
faster than the paper material. Cover the ice packs with another layer of paper packing material.
4) Ensure each sample is sealed in its packaging from the laboratory. It is recommended that each
sample be double bagged using plastic Ziploc bags. Ensure that each sample is properly labeled.
5) Place the samples into the cooler and fill in the gaps between samples with paper packing
material. Place a layer of paper packing material over the samples. If desired, place more ice
packs along the sides of the samples but remember to cover the ice packs with paper packing
material to slow sublimation. Place enough packing material into the cooler so that the samples
will not shift around during shipping.
6) Place the COC forms into a Ziploc bag and place these on top of the packing material inside the
cooler. Seal the cooler with packing tape. It is not required, however, the use of a custody seal
on the cooler is recommended to ensure sample integrity during shipping.
7) It is anticipated that samples will be shipped to the analytical laboratory in two batch shipments
per week following the schedule outlined below.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
Anticipated Sample Shipping Schedule:
Shipping Day:
Samples Recovered on:
Monday
Friday, Saturday, Sunday, Monday
Thursday
Tuesday, Wednesday, Thursday
8) Ship the samples to the analytical laboratory at the following address via priority overnight
shipping (next day AM delivery):
Eastern Research Group
Sample Receiving
PM: Julie Swift
601 Keystone Park Drive
Morrisville, NC 27560
919-468-7924
11.0
QUALITY ASSURANCE/QUALITY CONTROL
11.1
FIELD BLANKS
Daily field blanks will be collected and submitted for analysis. Collect a field blank each day of sampling
at one selected sample location following the procedures below:
1) The field blank must be collected prior to the installation of the actual sample media.
2) Using powder-free nitrile gloves remove a new pre-charged filter holder from its packaging and
record the filter ID on the field data sheet as well as on the media packaging. Make sure to note
in the sample log that this sample is a field blank.
3) Remove the Teflon plugs and install the filter holder onto the stainless steel U-tube as instructed
in Section 7.0.
4) Do not perform flow verification on the field blank sample. Proceed directly to attaching the
glass funnel sample inlet assembly to the filter holder.
5) After installation of the glass funnel inlet assembly, wait for 10 seconds to allow exposure then
remove the glass funnel sample inlet assembly and filter holder.
6) Replace the Teflon plugs and place the filter holder and the sample inlet assembly into their
respective packages and seal.
7) Place each component in the cooler with ice packs for transport from the site. Store the samples
in the freezer until ready for shipping to the laboratory.
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
11.2
TRIP BLANKS
One trip blank will accompany each shipment of samples to the laboratory. Follow the instructions below
to collect the trip blank:
1) Obtain a new pre-charged filter holder and glass funnel sample inlet assembly and identify them
with an appropriate sample ID on both the sample packaging and the field data sheet/COC.
Identify the units as trip blanks in the sample log.
2) Do not open the packaging and in no way expose the sample filter holder or glass funnel
assembly.
3) After properly identifying each, place the filter and glass funnel assembly into the shipment for
return to the laboratory. Two trip blanks will be sent each week corresponding to the two sample
batches shipped each week.
11.3
FLOW RATE CALIBRATION
The sampler flow rate will be calibrated at 15.0 lpm prior to test program initiation using the
manufacturers recommended flow rate standard (tetraCal) or other equivalent calibration standard
(DeltaCal). Dry piston-type and rotameter flow standards are not recommended for the PQ100. The
calibration will be checked monthly or sooner if it is suspected that the flow rate calibration has drifted.
11.4
DAILY FLOW RATE VERIFICATIONS
Sample flow rate will be checked prior to the initiation of sampling and at the end of each sample period.
The average flow rate calculated will be coupled with the total elapsed sample time to determine the total
sample volume. This value can also be compared to the total sample volume reported by the PQ100 for
validation purposes.
12.0
SAMPLER MAINTENANCE
The samplers should require little to no maintenance with the exception of routine cleaning of excess dust
and dirt buildup between sampling events. Pay attention to sampler operation looking for any abnormal
noises and or behaviors. The sample pumps have a rebuild period of 5000 hours and since the units
employed during this test program will be supplied from an equipment vendor, it is anticipated that each
unit will be delivered in good operating condition with no overdue maintenance requirements. It is
recommended that the operator check with the equipment vendor to ensure all sampler maintenance has
been conducted and is up to date.
13.0
CONTACTS
In the event you must reach ERM for any reason please use the following contact information:
Jeff Boggs – Field Project Manager
Mobile:
(443) 803-8495
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
Email:
[email protected]
Larry Hottenstein – QA Manager
Office:
(949) 623-4700
Mobile:
(949) 294-9775
Email:
[email protected]
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Sampling of Hexavalent Chromium in Ambient Air – Feb. 2014
ATTACHMENT – A
Field Data Sheet and COC
ATTACHMENT 1 FIELD FORMS
6
7
Appendix C
Laboratory Analytical Method SOPs
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modified to the procedure listed below. The modified method was submitted and
accepted as an ASTM Standard Test Method D7614 for the Determination of Total
Suspended Particulate (TSP) Hexavalent Chromium in Ambient Air Analyzed by Ion
Chromatography and Spectrophotometric Measurements. Sodium bicarbonate
impregnated cellulose filters are exposed to ambient air using hexavalent chromium
samplers designed, fabricated, and supplied by ERG (see SOP ERG-MOR-013 for
sampling procedure).
3.0
METHOD DETECTION LIMIT
The method detection limit (MDL) is determined every year according to the procedure
in 40 CFR, Part 136, Appendix B. A standard is spiked onto at least seven prepared
filters at a concentration one to five times the estimated detection limit. These filters are
extracted and analyzed according to the method outlined below. The Federal Register
MDL equation is listed in Section 15.1. The method detection limit is 0.0078 ng/mL,
which is 0.0036 ng/m3 (based on 21.6 m3 sample volume).
4.0
SCOPE AND APPLICATION
This procedure provides step-by-step instructions for analyzing hexavalent chromium
collected on sodium bicarbonate-impregnated ashless cellulose filters exposed to ambient
air.
5.0
METHOD SUMMARY
This SOP covers the determination of Cr6+ from sodium bicarbonate-impregnated ashless
cellulose filters exposed to ambient air and submitted to the laboratory. The filters are
extracted in a 20 mM sodium bicarbonate in deionized (DI) water solution via shaking for
45 minutes. The extract is analyzed by ion chromatography using a system comprised of
a guard column, an analytical column, a post-column derivatization module, and a
UV-VIS absorbance detector. In the analysis procedure, Cr6+ exists as chromate due to
the near neutral pH of the eluent. After separation through the column, the Cr6+ forms a
complex with the 1,5-Diphenylcarbazide (DPC) which can be detected at 530 nm. The
analysis is completed using the Chromeleon7 Client software version 6.50 SP4 Build
1000.
6.0
DEFINITIONS
AGP
CCB
CCV
CD
cm
Advanced Gradient Pump
Continuing Calibration Blank
Continuing Calibration Verification
Compact Disc
centimeter(s)
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Cr6+
DC
DI
DIUF
DPC
DVD
g
HPLC
IC
ICV
ICB
LPM
L
LCS
mL
M
MB
MDL
mM
MQO
ng/mL
nm
PE
PC
PCR
RE
RSD
SOP
SP
µL
µm
UV/VIS
7.0
Hexavalent Chromium
Detector/Chromatography
Deionized
Deionized Ultra Filtered
1,5-Diphenylcarbazide
Digital Versatile Disc
gram
High Performance Liquid Chromatograph
Ion Chromatograph
Initial Calibration Verification
Initial Calibration Blank
liter(s) per minute
liter(s)
Laboratory Control Samples
milliliter(s)
molar
Method Blank
Method Detection Limit
millimolar
Method Quality Objectives
nanogram(s) per milliliter
nanometer(s)
Performance Evaluation
Post Column
Post-Column Derivatizing Reagent
Relative Error
Relative Standard Deviation
Standard Operating Procedure
Single Pump
microliter(s)
micron(s)
Ultraviolet-Visible
INTERFERENCES
Sodium carbonate, used as the stabilizing medium in the Cr6+ filters, was observed to
cause interferences with the analysis. Higher concentrations of the sodium bicarbonate
impregnating solution may cause flow restrictions during the ambient air sampling. The
use of an impregnated filter of smaller pore size has been shown to cause definite flow
restrictions during sampling.
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8.0
9.0
SAFETY
8.1
The IC does not require venting, and elaborate safety precautions are unnecessary.
Safety glasses must always be worn in the laboratory. Gloves and lab coats are
required during the handling of all hazardous solutions.
8.2
The compressed gas cylinders must be stored and handled according to relevant
safety codes outlined in the corporate health and safety manual. The cylinders
must be secured to an immovable structure. They must be moved using a gas
cylinder cart.
8.3
Calibration standards are purchased in dilute solutions from certified vendors.
Standard laboratory practices for hazardous material handling should be
employed for handling acids, derivatizing reagents, and neat Cr6+ salts when these
are used for analysis.
EQUIPMENT
This SOP assumes familiarity with the operation of Dionex ion chromatographic systems.
For more detailed instructions in the operation of the Dionex IC, please refer to SOP
(ERG-MOR-042) and the Dionex operations manual.
10.0
9.1
The Dionex ICS-5000 ion chromatography system consists of an AS-DV
autosampler, an SP isocratic pump with seal wash, a DC chromatography
compartment housing the injection valve, 1000 uL sample loop and IC columns, a
PC-10 post-column reagent delivery device, and a VWD UV/VIS absorbance
detector.
9.2
The Dionex-600 IC consists of an AS40 autosampler with chromatography
compartment, a 1.0 mL sample loop for the AS40, a GP50 advanced gradient
pump (AGP) with vacuum degas option, an eluent container set with rack, an
eluent degas module, a LC20 chromatography enclosure, a Rheodyne injection
valve (Model 9126-038), an AD25 UV/VIS absorbance detector, and a PC10
post-column pneumatic delivery package.
9.3
The instrument is controlled and data is collected and processed using the
Chromeleon7 Client chromatography software version 6.80 running on a
computer using a Microsoft Windows operating system.
MATERIALS
10.1
47mm ashless cellulose filters, Whatman 41 or equivalent
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10.2
Materials required for analysis include: waste containers and a helium regulator
that regulates the pressure source for the post-column derivatizing solution and
degassing of the eluents. Also, the specific guard and analytical columns are
listed below in Section 14.2.
10.3
DIUF water for preparing eluent, post-column derivatizing reagent, sodium
bicarbonate solutions, and standards.
10.4
Class A volumetric flasks: 10 mL, 100 mL, 200 mL, 500 mL, 1 L, and 2 L.
10.5
Wide-mouth high density polyethylene storage bottles: 125 mL.
10.6
Analytical balance, capable of 100 µg sensitivity.
10.7
Polystyrene tubes with caps and tube rack: 14 mL.
10.8
Ultrasonicator, to be used for standard preparation.
10.9
Glove boxes supplied with a screen rack and ultra-pure nitrogen to purge while
handling and drying filters. One glove box should be designated as a filter
preparation only glove box.
10.10 Graduated cylinders: 50 mL, 100 mL, and 500 mL.
10.11 4 Large plastic containers for rinsing filters and filter baths.
10.12 Freezers.
10.13 Teflon® coated or plastic tweezers for handling filters. Tweezers are cleaned with
DI Water before use.
10.14 Pipettes: 100 μL, 5000 μL, and 10 mL.
10.15 Disposable nitrile gloves.
10.16 Autosampler vials and caps.
10.17 Wrist action shaker, to be used for sample preparation.
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11.0
CHEMICALS, REAGENTS, AND STANDARDS
11.1
Eluent Solution
A standard eluent solution of the following reagents is prepared in deionized
water:


250 mM ammonium sulfate, 99.99% purity trace metals basis
50.9 mM ammonium hydroxide, ACS reagent grade
In a 2 L volumetric flask, dissolve 66 g of ammonium sulfate in ~1 L DI water.
Sonicate ammonium sulfate and water. When mixed, add 7 mL of ammonium
hydroxide. Dilute to 2 L with DI water and sonicate briefly. The solution can be
used for up to 5 days, but loses strength over the course of several days.
11.2
Post-column Derivatizing Reagent (PCR)
In a 50 mL volumetric flask, dissolve 0.25 g of 1,5-diphenylcarbazide (DPC),
97% purity, in HPLC-grade methanol. Sonicate until DPC goes into solution. In a
500 mL volumetric flask add DI water, leaving room for 14 mL of 98% sulfuric
acid and 50 mL of DPC solution. Add 14 mL of 98% sulfuric acid and allow the
solution to cool. Add the DPC solution to the 500 mL flask. Fill to the mark with
DI water. Sonicate the solution briefly. This reagent is stable for three days. To
minimize waste it should be prepared in 0.5 L or 1 L quantities as needed.
11.3
Sodium Bicarbonate Impregnating Solution
In a 500 mL volumetric flask, add 5.0 g of sodium bicarbonate. Dilute to 500 mL
with DI water. Sonicate to mix.
11.4
20 mM Sodium Bicarbonate Solution
In a 2 L volumetric flask, add 3.36 g of sodium bicarbonate. Dilute to 2 L with
DI water. Sonicate to mix.
11.5
Primary and Secondary Stock Solutions
Two stock solutions should be prepared and/or obtained from separate sources.
The primary is to be used exclusively for the calibration standards and the
secondary for laboratory control samples (LCS) and calibration verification.
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11.6
Working Stock Solutions
The working stock solutions are 1000 ng/mL Cr6+. Working stock solutions
should be prepared for both calibration standards and laboratory control
samples/calibration verification. It is important not to use the same primary stock
solution for both working stock solutions.
11.7
11.6.1
Calibration Working Stock Solution: Dilute the appropriate volume of
the calibration primary stock solution to 100 mL using the 20 mM
sodium bicarbonate in DI water solution.
11.6.2
LCS Spike Solution (Working Stock): Dilute the appropriate volume of
the laboratory control primary stock solution to 100 mL using the 20
mM sodium bicarbonate in DI water solution. The LCS Spike solution
is used to spike laboratory control samples and to make the calibration
verification solution.
Calibration Standards
The six calibration standards are prepared by diluting the calibration working
stock solution to the concentrations specified below.
11.8
11.7.1
0.05 ng/mL Cr6+ - Dilute 10 μL of the working stock solution to 200 mL
using the 20 mM sodium bicarbonate solution.
11.7.2
0.1 ng/mL Cr6+ - Dilute 10 μL of the working stock solution to 100 mL
using the 20 mM sodium bicarbonate solution.
11.7.3
0.2 ng/mL Cr6+ - Dilute 20 μL of the working stock solution to 100 mL
using the 20 mM sodium bicarbonate solution.
11.7.4
0.5 ng/mL Cr6+ - Dilute 50 μL of the working stock solution to 100 mL
using the 20 mM sodium bicarbonate solution.
11.7.5
1.0 ng/mL Cr6+ - Dilute 100 μL of the working stock solution to 100 mL
using the 20 mM sodium bicarbonate solution.
11.7.6
2.0 ng/mL Cr6+ - Dilute 200 μL of the working stock solution to 100
mL using the 20 mM sodium bicarbonate solution.
Calibration Verification Solution
As part of the quality assurance program in the evaluation of the data, a
calibration verification from a secondary source at an intermediate concentration
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(0.5 ng/mL) is run as a check of the precision of the instrument and calibration.
An Initial Calibration Verification (ICV) is run immediately following the
calibration standards and Continuing Calibration Verifications (CCV) are run
after every 10 injections.
11.8.1
12.0
Calibration Verification Solution Preparation - Dilute 50 μL of the LCS
Spike Solution to 100 mL using the 20 mM sodium bicarbonate solution.
COLLECTION, PRESERVATION, SHIPMENT, AND STORAGE
12.1
Handling of Filters
Whenever the filter is handled, clean Teflon® coated or plastic tweezers are used
with disposable nitrile gloves. All filter drying and spiking is completed in the
laboratory nitrogen-purged glove box.
Note: For normal ambient air samples, gloves do not need to be replaced
while handling filters during extraction. For high particulate loaded
filters, the analyst needs to be aware of potential contamination and gloves
should be replaced if needed.
12.2
Preparation of Filters
12.2.1
Soak filters in a 10% nitric acid (50 mL of 70% nitric acid in 450 mL DI
water) bath for a minimum of 16 hours and a maximum of 24 hours.
New nitric acid solution is prepared before cleaning each filter batch.
About 50 filters can be soaked per half liter of solution.
12.2.2
Rinse filters thoroughly with DI water until the pH of filter matches the
pH of the DI water (about 30 minutes).
12.2.3
Dry the filters completely on a screen rack in a nitrogen-purged glove
box (minimum of 5 hours). The filters will become stiff after they have
dried.
12.2.4
Soak the filters in the impregnating solution (0.12 M sodium bicarbonate
in DI water) overnight. If the filters are not completely dry before
placing them in the impregnating solution, the solution will become
dilute and will not collect samples as efficiently.
12.2.5
Dry the filters completely on a screen rack in a nitrogen-purged glove
box until filters start to curl (minimum of 5 hours).
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12.3
12.2.6
Place dried filters into petri dishes. Place the petri dishes into small
plastic freezer bags labeled with the batch number and store in a freezer
until needed.
12.2.7
Analyze 10 percent of the cleaned filters. If there are any detects above
the MDL, the whole batch is discarded and a new batch is prepared.
Preservation and Storage of Filters
The filters are kept in the freezer until needed in the field for sampling or used in
the laboratory to prepare spikes or blanks during analysis. The filters are frozen
to prevent the sodium bicarbonate from reacting with possible interfering
substances present in the air.
12.4
Cleaning Filter Holders
Clean the filter holders between sample collection by placing used holder parts
into a container. Fill the container with DI water and agitate the filter holders.
Discard DI water and repeat two times. Fill the container with DI water and
sonicate the filter holders for one hour. Air dry filter holders completely before
reuse.
12.5
Shipment of the Filters
Place filters in filter holder cartridges and tighten. Place in plastic freezer bags
and place this into a labeled plastic can with funnel. The filter batch number is
recorded on the chain of custody, and the chain of custody is put with the plastic
can into a cooler packed with silver ice packs to keep the filters frozen. The
coolers are shipped to the field approximately 1-2 weeks in advance. The filters
are kept in freezers in the field until the sampling event.
12.6
Sample Hold Time
Stability of samples after sampling has been tested to 21 days. Samples should be
extracted and analyzed within 21 days of sampling.
13.0
CALIBRATION AND STANDARDIZATION
13.1
Prepare calibration standards at a minimum of five levels as described in
Section 11.7. The initial calibration ranges from 0.05 to 2.0 ng/mL Cr6+.
13.2
Analyze each calibration standard and tabulate the area response against the
concentration injected. Follow the analytical procedures described in
Sections 14.2. Use the results to prepare a calibration curve.
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13.3
Use a Least Squares Linear Regression Calculation (Chromeleon7 Client
chromatographic software) to calculate the correlation coefficient, slope, and
intercept of the regression. A correlation coefficient of at least 0.995 is required.
A relative error (RE) between the concentration calculated using the regression
line and the theoretical concentration of each calibration standard of < 20% is
acceptable. See equation in Section 15.4. The regression is expressed as follows:
y = mx + b
where:
y = dependent variable (response)
m= slope of regression line
b = intercept
x = independent variable (concentration)
13.4
14.0
The Calibration Verification solution is used to verify the calibration at the
beginning and throughout the sequence. Analyze an ICV after the initial
calibration and analyze a CCV after every 10 injections, and at the end of the
analysis batch. The primary stock solution for the ICV and CCV must be from a
different source than what is used for the calibration standards. The recovery
criteria are 85-115%. If the ICV or CCV is not within 15% of the target
concentration, prepare a new Calibration Verification solution and/or recalibrate
the instrument.
PROCEDURE
14.1
Filter Extraction
Due to the oxidation/reduction and conversion problems of Cr3+ and Cr6+, the
extraction should be performed immediately prior to analysis. It is important that
the ion chromatograph be equilibrated, calibrated and ready for analysis. Prepare
one cleaned, unused filter for every 20 filter samples in an extraction batch.
Unused, clean filters will also be used to prepare duplicate blank spikes for every
20 filter samples in an extraction batch. See section 16.5.
14.1.1
Remove the exposed filter from the petri dish, using tweezers and
disposable nitrile gloves. Fold the filter, place it in a 14 mL polystyrene
test tube and add 10 mL of the 20 mM sodium bicarbonate in DI water
solution. Cap the tube tightly. New tweezers should be used for each
filter.
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14.2
14.1.2
Place the tubes in a test tube rack. Place the tubes into the shaker for 45
minutes.
14.1.3
After 45 minutes of shaking, remove the tubes and put 5 mL of the
sample extract into a to a 5 mL Dionex autosampler vial. Store the
remaining extract in a refrigerator until analysis of all samples are
complete. Store sample extracts in the refrigerator for up to one week,
then transfer extracts to a labeled plastic bag and place in the fume hood
in the laboratory for disposal.
Sample analysis
The analysis time is approximately 10 minutes. The following conditions are used
for analysis.
15.0
14.2.1
Guard Column - IonPac NG1.
14.2.2
Analytical Column - IonPac AS7, 4 x 250 mm.
14.2.3
Eluent flow rate - 1.0 mL/min (250 mM ammonium sulfate and
50.9 mM Ammonium hydroxide).
14.2.4
Post column Reagent flow rate - 0.3 mL/min (2 mM DPC in 10%
methanol and 1 N sulfuric acid).
14.2.5
Detection Wavelength - 530 nm.
14.2.6
Sample Volume - 1000 µL.
CALCULATIONS
The Chromeleon® Client chromatography software calculates sample concentrations
based on the calibration values entered into the program. These values are verified by a
peer reviewer after analysis, and corrections can be made before reporting.
15.1
Method Detection Limit (MDL)
The MDL is determined every year according to the procedure in 40 CFR,
Part 136, Appendix B. A standard is spiked onto at least seven prepared filters at
a concentration one to five times the estimated detection limit. These filters are
extracted and analyzed according to the method outlined. The method detection
limit is 0.0078 ng/mL, which is 0.0036 ng/m3 (based on 21.6 m3 sample volume).
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The MDL is calculated as follows:
MDL = (t) × (SD)
Where:
t = Student’s t value for a 99% confidence level and a standard deviation
estimate with n - 1 degrees of freedom [t = 3.14 for seven replicates]
SD= standard deviation of the replicate analysis
15.2
Calculation of Stock Standard Concentration
The concentration in ng/mL is calculated below:
Stock Concentration =
15.3
(Volume Stock Added ( L) x Working Standard (ng / mL)) 1(mL)

Total Volume (mL)
1000( µL )
Calculation of Calibration and Check Standard Concentration
The concentration in the calibration, check standard and method spike standards is
calculated below:
Cal Std Conc . =
15.4
(Volume Stock Added ( L) x Stock Concentration (ng / mL)) 1(mL)

Total Volume (mL)
1000( µL)
Calculation of Least Squares Linear Regression Calibration Curve
Use a Least Squares Linear Regression routine (using Chromeleon® Client
chromatography software) to calculate a correlation coefficient, slope, and
intercept. Use concentration as the X-term (independent variable) and response as
the Y-term (dependent variable).
15.5
Calculation of the Coefficient of Correlation
The correlation coefficient, R, is the square root of R2 where:
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
 ( X ) (Y ) 
  ( XY ) 
n


2
( X )  
( Y ) 2 
2
2
(X ) 
   (Y ) 

n
n 
 
2
R2 
15.6



Calculation of the Concentration of Cr6+ in Sample
The concentration in the sample is calculated below:
Conc. Cr6+ In Sample (ng/mL) = (Sample Response – Intercept)
Slope
15.7
Calculation of ICV and CCV Percent Recovery
The ICV and CCV percent recovery is calculated below:
[Conc. Cr6+ in Std.] × 100
Expected Conc.
15.8
To calculate the concentration of Cr6+ in the air sampled, the volume of air
sampled must be known.
Cr 6 Concentration (ng/m 3 ) 
RA (ng/mL)  V2 (mL)
V1 (m 3 )
where:
RA
V1
V2
15.9
=
=
=
Concentration of Cr6+ in analyzed sample
Volume of air sampled
Total volume of sample extract
Calculation of Laboratory Control Sample Recovery
Percent recoveries of the LCS and LCS duplicates are calculated as follows.
First, the concentration of Cr6+ in the LCS is calculated as described in
Section 15.5. The corrected weight of Cr6+ is divided by the amount of Cr6+
spiked and multiplied by 100 as shown below:
% Recovery = (Actual Concentration of Cr6+ in LCS) × 100
Theoretical Conc. of Cr6+ in LCS
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15.10 Calculation of Relative Error (RE)
% RE = (Theoretical Conc.- Actual Conc.) x 100
Theoretical Conc.
16.0
QUALITY CONTROL
The analyst must perform the quality control checks listed in Table 24-1 and meet the
requirements in this section. Method Quality Objectives (MQO) and data assessment
criteria are determined from the results of the quality control samples. The MQO criteria
are presented in Table 24-1. A data QC review check sheet is presented in Table 24-2.
16.1
Sample Collection Quality Control
The sample acceptance criteria for the filters are given below. All samples being
logged in from the field are checked for these criteria. If a sample does not meet
these criteria, the sample is invalid.
16.2
16.1.1
Filters dropped or contaminated with any foreign matter (i.e., dirt, finger
marks, ink, liquids, etc.) are invalid.
16.1.2
Filters with tears or pinholes which occurred before or during sampling
are invalid.
16.1.3
Sample flow rate:

If the average flow rate is less than 9.0 LPM or exceeds 16 LPM the
filter is invalid.

If the start and stop flow rates differ more than ± 10% the filter is
invalid.
16.1.4
Filter samples collected by samplers which operate less than 23 hours or
more than 25 hours are invalid.
16.1.5
If a power failure occurs during a sample run which causes the stop time
or sample duration requirements to be violated, the sample is invalid.
Initial Calibration
Run a calibration curve with a minimum of five points as described in
Section 13.0 at the beginning of each sequence and whenever the Calibration
Verification standard does not fall within 15% of the target concentration. The
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initial calibration range is from 0.05 to 2.0 ng/mL of Cr6+. Calculate a correlation
coefficient. If the correlation coefficient is less than 0.995 or RE is greater than
20%, identify the cause and correct it. Repeat the calibration if necessary, or
prepare and reanalyze any outlying points on the calibration curve.
16.3
Initial Calibration Verification/Continuing Calibration Verification
Analyze Initial Calibration Verification (ICV) after the calibration. Analyze a
Continuing Calibration Verification (CCV) after every 10 injections and at the
end of the sequence to verify instrument calibration. If the calibration check
response is not within 15% of expected concentration, determine the cause. The
instrument may be malfunctioning, the calibration verification standard may not
be valid, or the instrument may need to be recalibrated.
16.4
Initial Calibration Blank/Continuing Calibration Blank
Analyze an initial calibration blank (ICB) prepared from the 20mM sodium
bicarbonate solution after the initial calibration and ICV. Analyze a continuing
calibration blank (CCB) after every CCV and at the end of the sequence to verify
that no contamination is occurring during the analysis. The acceptance criterion
is less than or equal to the MDL.
16.5
Laboratory Control Sample (LCS)
To ensure there are no matrix effects from the filters, prepare duplicate
Laboratory Control Samples for every extraction batch, up to a maximum of 20
samples per batch. Spike 10 µL of the LCS spike solution onto an unused,
cleaned filter, dry the filter in the nitrogen-purged glove box, and prepare and
analyze the filter with the rest of the samples. The acceptance criterion is 80120% recovery. If the spikes are outside of these limits, check the calibration and
extraction procedures. These can also be referred to as Method Spikes.
16.6
Method Blank Sample (MB)
Prepare a method blank sample with every extraction batch by extracting a blank
filter with 20 mM sodium bicarbonate solution. The acceptance criterion is less
than or equal to the MDL.
16.7
Replicate Analysis
Replicate analyses should be performed on all duplicate or collocated samples
received by the laboratory. The replicate results should be within 20% of each
other for samples greater than 5 times the MDL. If the replicate results are
outside of these limits, verify that the peaks are integrated properly, that there is
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no interference from other components in the sample and that the instrument is
working properly, and then flag the data.
16.8
Method Detection Limit
The method detection limit (MDL) is described in Section 15.1
16.9
Retention Time
The retention time must be within 5% of the expected retention time in order for a
peak to be identified as Cr6+. The expected retention time is the average retention
time of the calibration standards. If retention times vary by more than 10% from
calibration verification sample to calibration verification sample, stop the analysis
and check for an instrument problem. If the retention time changes from the
beginning of the day to the end of the day, the system may be changing over the
course of the day.
16.10 Performance Evaluation (PE) Samples
Performance evaluation samples should be obtained as available from
independent sources and analyzed as a routine samples.
16.11 Initial Demonstration of Capability
Each analyst must demonstrate proficiency for sample preparation and analysis by
generating data of acceptable accuracy and precision for four blank spikes (or
MDLs). For demonstration of capability, acceptable accuracy and precision is
defined as having both a %RSD equal to or lower than 20% and a percent
recovery within the range of 70-130%. This demonstration is repeated whenever
new staff receives training or significant changes in instrumentation are made.
16.12 Control Charts
16.12.1 Retention Time
Chart the Cr6+ retention time for each calibration verification standard,
laboratory control sample, and sample that contains Cr6+. The retention
time should not vary by more than 5% of the expected retention time.
The expected retention time is the average retention time of the six
calibration standards. If the retention time is out of this range check the
column, check the mobile phase delivery system for leaks or plugs, and
make sure the sample valve is properly aligned. Retention time control
charts should be created for each sequence and kept in a notebook.
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16.12.2 Laboratory Control Samples
Chart the LCS concentrations. The analyzed LCS concentration should
not vary by more than 20% of the expected concentration. If the LCS
concentrations are outside of these limits, check the calibration and
extraction procedures. LCS control charts should be created for each
column used and kept in a notebook.
16.13 Field Blanks
Prepare and ship Field Blank samples at least 10 percent sample collection
frequency. Extract the Field Blank sample to verify cleanliness of the filters and
filter holders. The acceptance criterion is less than or equal to the MDL. If
results are greater than the MDL, another Field Blank sample is submitted to the
field. All data associated with that blank (samples recovered between clean
blanks) are flagged.
17.0
PREVENTION
When possible, minimize the amount of chemicals used in the preparation and analysis of
the Cr6+ filters to reduce waste.
18.0
DATA REVIEW AND CORRECTIVE ACTION
18.1
Data Review Documentation
Project files including at a minimum the information required in Section 22 are
assembled by the performing analyst. Documentation for sample custody,
preparation and analysis will be reviewed for completeness and acceptability by
the Task Lead or secondary reviewer associated with the project or program
requiring the analysis as described in this section.
The second review of the data is performed by the Task Lead or designated
secondary reviewer using the QC review checklist (checklist) shown in Table 242 to confirm that quality requirements have been met. Corrections and flags are
added to the data consistent with the corrective action required for each review
finding. Second level reviewers must complete, initial, and date the checklist.
The completed check list is included as part of the data package. Data not
meeting SOP requirements are flagged and brought to the attention of the Project
Manager for resolution.
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18.2
Quality Staff Review
A minimum of 10% of the data is reviewed by ERG Quality Staff. Quality staff
review includes but is not limited to checks that all SOP-specified quality
parameters have been met and that data reviewers have completed their review
checklists. Reviews should be documented on the review form initiated in 18.1
by the primary data reviewer. Comments or issues with data identified by the
Quality Staff reviewer are brought to the attention of the Project Manager for
resolution. Quality Staff will use the review process as an indication of episodic
or systematic quality program issues that may require improvements to the ERG
laboratory quality system and or additional training for ERG staff. As an option,
Quality Staff may request review of 1% of the data from this method for a project.
One percent (1%) review will follow the guidance in this section.
Corrective action for Hexavalent chromium analysis data quality issues are
presented in Table 24-1.
19.0
WASTE MANAGEMENT
Hazardous waste disposal is discussed in detail in SOP ERG-MOR-033.
20.0
19.1
The PCR waste should be placed in an appropriately labeled waste container in
the fume hood in the laboratory.
19.2
In the laboratory there should be a satellite hazardous waste container for the
hexavalent chromium working standards and instrument waste.
19.3
The analyst is responsible for contacting the hazardous waste contact to dispose of
the waste.
MAINTENANCE
20.1
Periodic Maintenance
For regular periodic maintenance, see Dionex-600 manual, Section 4. Any
maintenance performed should be recorded in the maintenance logbook in the lab.
20.1.1
Inspect for leaks. Wipe up any liquid spills and rinse dried reagents off
with deionized water.
20.1.2
Replace the eluent filter when changing eluents (see Dionex-600
manual, Section 4). The pump must then be primed to remove air in the
eluent line.
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20.1.3
21.0
22.0
Rinse the PCR line and container with methanol when the instrument is
not in use for more than 3 days.
SHORTHAND PROCEDURE
21.1
Prepare filters.
21.2
Send filters to site.
21.3
Receive filter samples.
21.4
Inspect filter samples.
21.5
Place filters in an extraction tube.
21.6
Add 10 mL of 20 mM Sodium Bicarbonate in DI water solution to the extraction
tube.
21.7
Shake for 45 minutes.
21.8
Calibrate the IC.
21.9
Analyze the extracts by IC.
DOCUMENTATION AND DOCUMENT CONTROL
22.1
All information concerning sample preparation, standard preparation, instrument
conditions, etc., must be written in the analyst’s notebook or recorded in the
LIMS.
22.2
A list of the injections must be recorded in addition to the following information:
type of eluent used, system number, date of analysis, and retention time.
22.3
All calculations and the type of method for determining concentration must be
recorded in the analyst’s notebook. Any unusual problems or conditions must
also be noted.
22.4
Record all maintenance performed on the instrument in the maintenance logbook
for this particular instrument.
22.5
Record all sample injections, including quality control samples, performed by the
instrument in the injection logbook for this particular instrument.
22.6
It is imperative the project documentation be updated following each sample.
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22.7
Analysts will copy raw instrument and QC files to a designated corporate network
shared drive at the completion of each analysis sequence or batch. Primary data
reviewers will use the data on the shared network drive for their data review
process. The completed data packages ready for upload into the ERG LIMS
system will be retained on the network drive as the backup for this data.
All processed data are archived in the LIMS on the shared network drive. Data is
periodically archived to shared server and compact disc (CD) or digital versatile
disc (DVD), verified on the system where the data originated and stored for at
least five years in the laboratory. An archive copy of a data package is retained
for at least five years in the laboratory data storage.
23.0
REFERENCES
DX-600 Series Chromatography System, and DX-600 Chromatography System
Operator’s Manual, Dionex Corporation, 117171.
Advanced Gradient Pump Operators Manual, Dionex Corporation,
Document No. 034463, 117171.
CARB 039, Extraction and Analysis of Hexavalent Chromium by Ion Chromatography,
1993. A summary is found at http://www.arb.ca.gov/aaqm/sop/summary/summary.htm.
ASTM Standard Test Method D7614 for the Determination of Total Suspended
Particulate (TSP) Hexavalent Chromium in Ambient Air Analyzed by Ion
Chromatography and Spectrophotometric Measurements
24.0
TABLES, DIAGRAMS, FLOWCHARTS, VALIDATION DATA
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Table 24-1. Summary of Quality Control Procedures for Hexavalent Chromium Analysis
Parameter
Frequency
Acceptance Criteria
Corrective Action
Every Data Package
Complete documentation in the
Sample
In Data Packet
appropriate data package or
preparation,
and/or notebook.
notebook
standard
Meets SOP
preparation,
ERG-MOR-063
instrument
criteria.
conditions
Every Data Package
All sample
In Data Packet and/or Complete documentation in the
or injection sequence injection log.
appropriate data package or
injections,
injection log.
including quality
Meets SOP
control samples
ERG-MOR-063
criteria.
Every Data Package
Type of eluent
In Data Packet and/or Complete documentation in the
used, system
notebook. Meets SOP appropriate data package or
notebook
number, date of
ERG-MOR-063
analysis, and
criteria.
retention time.
Every Data Package
Complete documentation in the
Calculations and
In Data Packet
or
Sequence
appropriate data package or
method for
and/or notebook.
notebook
determining
Meets SOP
standards
ERG-MOR-063
concentration
criteria.
COCs
In Data Packet
In Data Packet
Initial 5-point
calibration
Before every
sequence
Correlation coefficient
≥ 0.995; RE < 20%
Initial Calibration
Verification (ICV)
Before every
sequence, following
the initial calibration
Recovery 85-115%
Complete documentation in the
appropriate data
1) Repeat analysis of calibration
standards
2) Reprepare calibration standards
and reanalyze
1) Repeat analysis of initial
calibration verification standard
2) Repeat analysis of calibration
standards
3) Reprepare calibration standards
and reanalyze
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Table 24-1. Summary of Quality Control Procedures for Hexavalent Chromium Analysis
(Continued)
Parameter
Frequency
Acceptance Criteria
Corrective Action
Initial Calibration
Blank (ICB)
One per Batch,
following the ICV
Analyte must be ≤
MDL
1) Reanalyze
2) Reprepare blank and reanalyze
3) Correct contamination and
reanalyze blank
4) Flag data of all samples in the
batch
1) Repeat analysis of CCV
2) Reprepare CCV
3) Flag data bracketed by
unacceptable CCV
1) Reanalyze
2) Reprepare standard and
reanalyze
3) Flag data of all samples since
the last acceptable LCS
1) Reanalyze
2) Flag data for all samples in the
batch
Continuing
Calibration
Verification (CCV)
Every 10 injections
and at the end of the
sequence
Recovery 85-115%
Laboratory Control
Sample (LCS)
Two per sample
batch, up to 20
samples.
Recovery 80-120%
Method Blank (MB)
One per batch
Analyte must be ≤
MDL
Replicate Analysis
Duplicate/Collocate
and/or replicate
samples only
RPD ≤ 20% for
concentrations greater
than 5 x the MDL.
1) Check integration
2) Check instrument function
3) Flag samples
Continuing
Calibration Blank
(CCB)
After every CCV and
at the end of the
sequence
Analyte must be ≤
MDL
1) Reanalyze
2) Reprepare blank and reanalyze.
3) Correct contamination and
reanalyze blank
4) Flag data of all samples in the
batch
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Figure 24-1. Flowchart for Hexavalent Chromium Samples
Prepare Filters
Send filters to site
Receive filter samples
Inspect Filter Samples
Place filters in extraction tube and add
10 mL 20 mM Sodium Bicarbonate to
sample filter
Shake for 45 minutes
Calibrate IC
Analyze Sample Extracts by IC
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Table 24-2. Hexavalent Chromium Quality Control Review Checklist
Sequence ID:___________________________ Instrument: ______________________________________ Batch:____________________________
Cal Curve (Method): _____________________________________________ Analyst: ________________________ Date: ___________________
10% Review Sample IDs: __________________________________________ Reviewer: _______________________ Date: ___________________
Optional 1% Review Sample IDs: ___________________________________ Reviewer: _______________________ Date: ___________________
Parameter
All sample injections, including
quality control samples
Acceptance Criteria
In Data Packet and/or injection log meets SOP
ERG-MOR-063 criteria
COCs included and sample
volume correct
Lab receipt acknowledged. LIMS number
added to COC. Sample volume correct.
Initial 5-point calibration
Correlation coefficient ≥ 0.995 and RE <20%
Initial Calibration Verification
(ICV) following int. calibration
Recovery 85-115%
Blanks (ICB/CCB) following
ICV/CCV
Analyte must be ≤ MDL
Continuing Calibration
Verification (CCV) every 10
injections and at the end of the
sequence
Recovery 85-115%
Analyst
Check
(Initials
and Date)
Task
Lead/Data
(Initials
and Date)
10 % QA
Review
(Initials
and Date)
1%
Optional
QA
Review
(Initials
and Date)
Comments
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Parameter
Laboratory Control Sample one
per 10 samples
Acceptance Criteria
Recovery 80-120%
Method Blank
one per batch
Analyte must be ≤ MDL
Replicate Analysis
RPD ≤ 20% for concentrations > 5 x the MDL.
Manual Integration
Per SOP ERG-MOR-097
Manual Check of Calculations
Manual check must agree with computer
generated result
Check Qualifiers
Check to make sure LIMS data flags are correct
Analyst
Check
(Initials
and Date)
Task
Lead/Data
(Initials
and Date)
Review checklist from SOP or equivalent must be completed by primary data reviewer/TL/QA.
10 % QA
Review
(Initials
and Date)
1%
Optional
QA
Review
(Initials
and Date)
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