UNI-T | UT3000 series | Operating instructions | UNI-T UT3000 series Operating instructions

Mercury Ultratracer
UT-3000
Operating Manual
English
Version 2.11
Manufacturer: Mercury Instruments GmbH
Liebigstrasse 5
85757 Karlsfeld/Germany
service@mercury-instruments.de
© 2012 by Mercury Instruments GmbH, Karlsfeld (Germany)
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General information for safe operation
Caution:
WARNING: While operating the UT-3000 or the Automatic Calibration
Unit, parts of its interior are under high voltage. UV-beams are produced
inside the instrument. If safety regulations are ignored physical and/or
material damages could occur. Only qualified personnel should be
authorised to operate the UT-3000 and its accessories.
Conditions for correct function of the UT-3000 system are careful
storage and proficient operation and maintenance.
Do not operate instrument if damaged.
When connecting the UT-3000 to a power source please note the related safety
regulations.
The UT-3000 or the Automatic Calibration unit should be operated from the
type of power source indicated on the rating plate.
Make sure that plugs and power cord are not damaged.
Only operate the UT-3000 and its accessories on a stable and dry surface. The
interior of the instrument should never get moist or wet. In case it happens,
consult an expert.
Regulations for prevention of accidents are to be followed.
Before opening the UT-3000 or the calibration device disconnect it from its
mains supply.
Repair and maintenance on the opened and powered instrument must only be
done by qualified personnel.
The UT-3000 is dedicated for the measurement of mercury concentrations in
air and gaseous samples. Do obey the related dangers while working with
toxic or harmful substances. Do not operate the UT-3000 in hazardous areas
or for measurement of flammable or explosive gases. A special version for
mercury measurement in natural gas is available. This must be explicitly
indicated on the instrument and in the according documentation which comes
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with the instrument. The instructions provided in the operation manual have
strictly to be followed.
The calibration device (Automatic Calibration Unit and Manual Calibration
Unit) contains elemental mercury. Damage which may lead to a leakage has
strictly to be avoided. Calibration device must only be opened and/or repaired
by qualified and specially trained persons. Calibration device has to be
protected from shocks and must never be tilt or turned over. Notify also the
Material Safety Data Sheet in the appendix.
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Contents
GENERAL INFORMATION FOR SAFE OPERATION........................................................................................2
1. GENERAL DESCRIPTION ...................................................................................................................................7
1.1 APPLICATIONS.....................................................................................................................................................7
1.2 MEASURING PRINCIPLE ......................................................................................................................................9
2. INSTALLATION ....................................................................................................................................................10
2.1 PREPARATION FOR OPERATION .......................................................................................................................10
2.2 ELECTRICAL POWER SUPPLY............................................................................................................................11
2.3 OPERATION AND DISPLAY COMPONENTS .........................................................................................................11
2.4 CONNECTION OF THE ELECTRICAL OUTPUT ....................................................................................................11
2.4.1 Serial Data output (USB / RS 232)............................................................................................................11
2.4.2 Connection of an Automatic Calibration Unit..........................................................................................14
3. OPERATING INSTRUCTIONS ..........................................................................................................................15
3.1 TURNING ON THE UT-3000 ...............................................................................................................................15
3.2 MAIN MENU .....................................................................................................................................................15
3.3 BASIC SETTINGS ................................................................................................................................................17
3.4 SET SAMPLE PARAMETERS...............................................................................................................................17
3.4.1 Set Sample Volume ....................................................................................................................................17
3.4.2 Set Cycle Duration .....................................................................................................................................18
3.4.3 Auto Range Volume (only for Natural Gas / Tedlar Bag Version) ..........................................................19
3.5 START MEASURING ...........................................................................................................................................19
3.6 DATA LOGGER ..................................................................................................................................................21
3.6.1 Start logging of measurement data ...........................................................................................................21
3.6.2 Sending logged data to a PC by using Hyper terminal .............................................................................22
3.6.3 Delete logged data ......................................................................................................................................24
3.6.4 Import of data into EXCEL .......................................................................................................................24
3.6.5. Using the HG-Transfer Software for Data Transfer to a PC ..................................................................26
4. CALIBRATION......................................................................................................................................................29
4.1 SHOW ACTUAL CALIBRATION ...........................................................................................................................29
4.2 SHOW ALL CALIBRATIONS ................................................................................................................................30
4.3 PERFORM SPAN CHECK ....................................................................................................................................31
4.4 PERFORM NEW CALIBRATION: MANUAL CALIBRATION ................................................................................31
4.4.1 Manual Calibration: Enter pg .............................................................................................................32
4.4.2 Manual Calibration: Enter µl ...............................................................................................................36
4.4.3 Examples for calibration functions ..................................................................................................40
4.5 PERFORM NEW CALIBRATION: AUTOMATIC CALIBRATION (OPTION) ..........................................................43
4.5.1 Connecting the Automatic Calibration Unit with the UT-3000 ...................................................43
4.5.2 Activating the Automatic Calibration Function .............................................................................44
4.5.3 Cal. Concentration ................................................................................................................................45
4.5.4 Cal. Interval .............................................................................................................................................45
4.5.5 Manual Start of the Automatic Calibration .....................................................................................46
4.5.6 Automatic Start of the Calibration ....................................................................................................47
4.5.7 Empty Syringe .......................................................................................................................................48
4.5.8 Cal. Mode.................................................................................................................................................48
4.5.9 Activation of Automatic Span Calibration ......................................................................................48
5. SERVICE-MENU ..................................................................................................................................................49
5.1 SET DATE AND TIME .........................................................................................................................................50
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5.2 DEVICE DATA ....................................................................................................................................................50
5.3 SHOW FLOW ......................................................................................................................................................50
5.4 PURGE REPETITIONS (FOR AUTOMATIC CALIBRATION OPTION ONLY) ........................................................50
5.5 CHANGE SYRINGE (FOR AUTOMATIC CALIBRATION OPTION ONLY) .............................................................51
5.6 SET CALIBRATION DATA ..................................................................................................................................51
5.6.1 Set Flow Calibration .............................................................................................................................51
5.6.2 Set Measuring Calibration ..................................................................................................................52
5.6.3 Set T-Cal. Cell Calibration ...................................................................................................................52
5.7 TRAP COUNTER .................................................................................................................................................52
5.8 SET RS232 MODE .............................................................................................................................................52
5.9 SET ZERO DURATION ........................................................................................................................................52
5.10 SET STATUS .....................................................................................................................................................53
5.11 SPECIAL SERVICE CODES ...............................................................................................................................54
6. MAINTENANCE....................................................................................................................................................55
6.1 SPARES AND ACCESSORIES ...............................................................................................................................55
6.2 TECHNICAL DRAWINGS .....................................................................................................................................57
6.3 ERROR MESSAGES .............................................................................................................................................64
6.3.1 Lamp ! ......................................................................................................................................................64
6.3.2 Sampling Flow out of Range!.............................................................................................................64
6.3.3 Heating Flow out of Range! ................................................................................................................64
6.3.4 Temp. out of range ! See instruction manual! ...............................................................................64
6.3.5 Check heating coil ! ..............................................................................................................................64
6.3.6 T-Sensor not connected ! Connect T-Sensor of Calibration Cell! ............................................64
6.3.7 Temp out of Range ! See instruction manual! ...............................................................................65
6.3.8 Pump ! (flashing) ...................................................................................................................................65
6.3.9 Lamp Stability! .......................................................................................................................................65
6.3.10 Logger full (flashing)..........................................................................................................................65
6.3.11 No Sample!!!.........................................................................................................................................65
6.3.12 EEP INIT; Warning No. 20: Check Parameters! See Instruction Manual! ............................65
6.3.13 Warning No. 50: Check Calibration! See Instruction Manual! .................................................65
6.3.14 Warning No. 60: Check Flow-Calibration ! See Instruction Manual! ......................................65
6.3.15 Warning No. 70; Check Calibration Data! .....................................................................................66
6.3.16 Warning No. 80; RS232 Communication Error; Connect Syringe! .........................................66
6.3.17 Warning No. 91; Check Calibration! ...............................................................................................66
6.3.18 Repeat Zero ..........................................................................................................................................66
6.3.19 Low Sampling Flow ............................................................................................................................66
6.4 TROUBLESHOOTING ..........................................................................................................................................67
6.4.1 Unusual Measuring Peaks ..................................................................................................................67
6.5 ROUTINE MAINTENANCE ..................................................................................................................................68
6.5.1 Replacement of Membrane Filter .............................................................................................................68
6.5.2 Replacement of the filter cartridges ..........................................................................................................68
6.6 FUSES .................................................................................................................................................................70
6.7 CLEANING THE GOLDTRAP ..............................................................................................................................71
6.8 REPLACEMENT OF THE GOLDTRAP .................................................................................................................73
6.9 FLOW ADJUSTMENT (FOR QUALIFIED PERSONNEL ONLY) ..............................................................................75
6.9.1 Heating Flow Adjustment....................................................................................................................75
6.9.2 Sampling Flow Adjustment ................................................................................................................75
6.10 GOLD TRAP ASSEMBLY ..................................................................................................................................76
7. TECHNICAL INFORMATION .............................................................................................................................78
7.1 TECHNICAL SPECIFICATIONS............................................................................................................................78
7.2 INFLUENCING EFFECTS .....................................................................................................................................78
7.3 STORAGE AND TRANSPORT ...............................................................................................................................79
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8. VERSION FOR HG DETERMINATION IN NATURAL GAS AND OTHER HYDROCARBON GASES
(TEDLAR® BAG VERSION) ...................................................................................................................................80
8.1 SAMPLING SYSTEM FOR MERCURY DETERMINATION IN NATURAL GAS ..........................................................80
8.2 SETUP FOR CONTINUOUS MEASUREMENT OF HG IN NATURAL GAS.................................................................83
8.3 UT-3000 VERSION FOR ANALYSIS USING A SAMPLE BAG (TEDLAR® BAG).....................................................84
8.3.1 Setup of the UT-3000 analyzer ...........................................................................................................85
8.3.2 Sampling of natural gas with the sample bag (Tedlar® bag) .....................................................86
8.3.3 Measuring the sample from the bag .................................................................................................86
8.4 SELECT PUMP TYPE ..........................................................................................................................................90
9. COMMUNICATION WITH EXTERNAL DATA ACQUISITION SYSTEM (OPTION) .................................91
9.1 PARAMETER SETTINGS FOR REMOTELY TRIGGERED ZERO AND SPAN CHECK ...............................................91
9.2 UT- 3000 EXTERNAL DATA ACCESS (VERSION 04.05.2004) ...............................................................................91
APPENDIX .................................................................................................................................................................97
EC-DECLARATION OF CONFORMITY .............................................................................................................97
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1. General Description
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1. General Description
1.1 Applications
The UT-3000 is dedicated for automatic measurement of mercury concentrations in air and other
gaseous samples.
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The mercury Ultratracer provides a compact and reliable tool for automatic measuring of
Total Gaseous Mercury (TGM) in air at ultratrace levels. Utilising the high performance
GoldTrap amalgamation module and the optimised state-of-the-art Atomic Absorption
detector detection limits at sub-ng/m³ levels are achieved.
The instrument operates automatically, all functions are controlled by an embedded
microprocessor. Once the analysis has been started, measurements are performed
automatically and data are collected by the built-in data logger. The capacity of the data
logger is up to 100 days.
The UT-3000 is used in following applications:
Air quality studies
Monitoring of indoor air pollution
Environmental pollution source tracking
plume profiling
Studies of mercury dispersion in the atmosphere
Studies of interaction between atmosphere and surfaces
Pollution prevention
Natural gas and derivatives (observe special hazardous zone requirements)
Hydrogen and other gases (observe special hazardous zone requirements)
Soil and ground degassing studies
FIGURES: THE UT-3000 ULTRATRACER IN THE FIELD - A VERSATILE INSTRUMENT FOR MONITORING MERCURY IN AIR
AND GASES AT ULTRA TRACE LEVELS
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1. General Description
FIGURE: FORMATION OF SMOG IN A CITY (KUALA LUMPUR)
FIGURE: PIPELINE FOR NATURAL GAS (RUSSIA)
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FIGURE: THE UT-3000 IN OPERATION: MONITORING
OF URBAN AIR QUALITY (MUNICH).
FIGURE: ANALYSIS OF MERCURY IN
NATURAL GAS USING THE UT-3000 WITH THE
TEDLAR BAG TECHNIQUE
FIGURE: MEASUREMENT OF MERCURY IN NATURAL GAS (EGYPT)
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1.2 Measuring principle
The UT-3000 uses the Mercury Instruments GoldTrap to capture total gaseous mercury (TGM)
directly from the sample. GoldTraps work because mercury sticks to gold at room temperature.
The sample gas is pulled through a 0.45 micron PTFE filter and then passes the trap. The gas
continues to flow through the trap but the mercury stays behind--trapped on the gold. After the
mercury is captured, the GoldTrap is heated very quickly; this releases the mercury as a gas
(thermal desorption). The gaseous mercury is then swept by the flow of purified mercury free air
into the optical cell of the detector. Here the mercury is measured by atomic absorption
spectrometry (AAS).
Basis for determination of the mercury concentration by AAS is the resonance absorption of the
Hg-atoms at a wavelength of 253.7 nm. The sample gas is carried into the optical cell by a builtin pump. The optical cell is entirely made of synthetic quartz glass. Radiation of a mercury lamp
passes through the cell and is measured by a solid state detector. The attenuation of the UV light
reaching the detector depends on the number of mercury atoms in the optical cell. The
microprocessor performs the quantitative evaluation of the mercury concentration in the sample.
In order to get an extremely stable baseline, the UV-light source is controlled by a reference
beam and reference detector device. In addition to this, the UV detectors of the UT-3000 are
thermostatically controlled. Heating the optical cell and the GoldTrap makes the UT-3000
insensitive to volatiles like water vapor and hydrocarbons.
UT-3000 Mercury Ultratracer
Optical Cell
10 l/h
40 l/h
GoldTrap
V2
V1
Pump
Mass flow
meter
Zero air
filter
0.45 µm
PTFE filter
Sample IN
Calibration
port
FIGURE: UT-3000: SCHEMATIC GAS FLOW
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2. Installation
2.1 Preparation for Operation
The UT-3000 is unpacked and placed on a flat surface (e.g. table). The handle can be adjusted
in several steps in order to be used for carrying the instrument or as a base to position it on a
bench (only if applicable; there is also a version for 19” rack mount available).
FIGURE: ADJUSTMENT OF CARRYING HANDLE
The sample inlet filter (0.45 µm PTFE) is unpacked. Insert the filter into the filter holder on the
front panel of the instrument and push it carefully over the white nozzle in the center of the filter
holder. Turn the filter slightly to get a tight connection.
The printed side of the filter shows towards the operator.
Never operate the instrument without a sample inlet filter installed !
Sample Filter
always in place!
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2. Installation
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2.2 Electrical power supply
The voltage of the power source has to be the same as the operation voltage indicated on the
rating plate of the UT-3000. One end of the included power cord has to be connected to the
power cord receptable on the back of the UT-3000. The opposite end has to be plugged into an
appropriate power outlet. For operation turn on the UT-3000 by pushing the power
switch on the back plate to position I.
FIGURE: REAR PANEL OF UT-3000
2.3 Operation and display components
The UT-3000 features a waterproof IP66 keypad and a graphic LCD with background
illumination for comfortable operation.
2.4 Connection of the electrical output
2.4.1 Serial Data output (USB / RS 232)
To read out data from the built-in data logger or measurement results in realtime connect the UT3000 with a PC. The serial input of the PC (COM1 or COM2) has to be connected to the USBport on the rear panel of the instrument using an appropriate cable (part no. 202-07a). Below the
USB-port there is also available a 9-pin DSUB-socket labelled “RS232”. This socket is normally
used for the controlling of the automatic calibration device option. But by manually switching an
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internal dipswitch on the backplane (see picture below) you can use this RS232-socket instead of
the USB with an appropriate 1:1 cable (part-no. 202-07) for the output of measuring values.
FIGURE: BACKPLANE WITH DIPSWITCH BETWEEN USB (FACTORY SETTING) AND RS232
RS 232
5
9
1
Pin Nr.
5
3
2
GND
RxD
TxD
6
FIGURE: SERIAL RS232 OUTPUT SOCKET ON INSTRUMENTS REAR SIDE
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Data are transferred as ASCII-characters every time a measurement cycle has been completed.
They can be received and filed on the PC using a terminal program, for example Windows Hyper
Terminal.
The parameters for data transfer are:
9600 Baud / 8 Data bits/ 1 Stop bit/ no Parity and Xon/ Xoff.
The data set has following format:
Date Time Status Volume Reading [CR][LF]
One data set has 34 bytes, end is carriage return and line feed.
Following Status Codes are possible:
Code
MS
LA
SF
HF
HC
PU
CD
CP
LS
NS
WC
Meaning
Measuring
Lamp Error
Sampling Flow out of range
Heating Flow out of range
Check Heating Coil
Pump failure
Check Calibration Data
Check Calibration
Lamp Stability
No Sample
Wrong Calibration
Example for data sets:
09.03.07 10:22 MS 001.0 000006.0
09.03.07 10:26 MS 001.0 000006.0
09.03.07 10:30 MS 001.0 000006.0
09.03.07 10:34 MS 001.0 000006.0
09.03.07 10:38 MS 001.0 000006.2
09.03.07 10:42 MS 001.0 000006.1
09.03.07 10:46 MS 001.0 000005.9
A description of the status messages is given in chapter 7.2.
For readout of measuring data stored in the data logger see chapter 3.6.
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2.4.2 Connection of an Automatic Calibration Unit
If an Automatic Calibration Unit is installed together with the UT-3000, both
instruments have to be connected before starting operation.
a) Use the connecting cable which has two 4-pin round plugs and plug it into the sockets on
the rear side of the instruments marked “Temperature” and “PT100”.
b) Take the cable with the 9-pin DSUB plugs. Identify the plug labelled “UT-3000” and
connect it to the RS232 socket on the rear side of the UT-3000. Identify the plug labelled
“Calibration unit” and connect it to the RS232 socket on the rear side of the Automatic
Calibration Unit.
FIGURE: BACK SIDE OF UT-3000 (UPPER) AND AUTOMATIC CALIBRATION UNIT (LOWER) WITH CONNECTION
TUBING, PT100-CABLE AND RS232-CABLE
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3. Operating instructions
3.1 Turning on the UT-3000
Do not operate the UT-3000 without the sample inlet filter installed in place. If this
precaution is ignored, the system, especially the GoldTrap, may be damaged by dust
particulate.
The UT-3000 version for use with an Automatic Calibration Unit must not be operated
without the connecting tubing of the Automatic Calibration Unit connected to the UT3000 (see chapter 4.2.1).
After turning on the UT-3000 the mercury lamp ignites and heats to operation temperature.
Following indications will appear on the display first:
In case of using an automatic calibration device (which has to be connected and switched on
before, see chapter 4.3.2), there will be an initiation step of the syringe after lamp stabilizing
phase (INIT SYRINGE).
3.2 Main Menu
After the instrument has stabilized, which typically takes 5-15 minutes (depending on the
ambient temperature), following steps will be performed automatically:
Zeroing - Trap Cleaning - Trap Cooling - Zeroing - Trap Cleaning - Trap Cooling Zeroing - System Evaluation - Trap Cooling - Sampling ...
The Main Menu can be entered by pressing the ESC-key during Sampling.
By simply pressing the numbered keys shown on the Main Menu the desired function can be
chosen.
For the Tedlar bag version a different main menu is displayed. In this case some of
the other menus may also differ, see chapter 6.4.
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FIGURE: MAIN MENU
Following functions can be selected from the main menu:
F1: Start Measuring = measurement cycle starts with automatic sampling, followed by gold
trap heating and atomic absorption measurement.
F2: Set Sample Parameters = set sample volume or measurement cycle duration.
F3: Data Logger = data logger management: switch on/off data logger, display logged data,
transfer logged data to PC, clear logged data.
F4: Calibration = show actual or all calibrations or perform new calibration or span check.
Page2▼= show next page
F1: Print last data: all data (up to 200 measurements) since the last sample volume setting are
printed. For this function a printer must be connected to the parallel printer output.
F2: Continuous print on/off: results are printed automatically if a measurement is completed.
For this function a printer must be connected to the parallel printer output.
F3: Set 4-20 mA: F1- allows setting of measuring unit µg/m³ - ng/m³; F2- setting of the
measuring range relevant for the 4-20 mA signal. F3- the 4-20 mA output can be tested, the
output signal will be according to the set mA value..
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3. Operating instructions
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3.3 Basic Settings
For the first measurement settings in the Service Menu have to be made.
Press ESC-Service in the main menu to go to the service menu.
Now you have to enter a service code. Follow the instructions given in chapter 5 in order to
perform the required settings.
3.4 Set Sample Parameters
3.4.1 Set Sample Volume
Press F2-Set Sample Parameters in the main menu and activate “Set sample volume” by
moving the arrow to the corresponding line. Then press F1 and enter the desired sample volume.
Characters can be deleted with the -key. The according sampling time is automatically
calculated and displayed.
a) For fast screening measurements (accuracy >1 ng/m³) a sample volume of 1 l is
recommended.
b) To achieve better sensitivity and optimum analysis speed (accuracy ~0.2 ng/m³) a sample
volume of 10 l is recommended.
c) For a maximum sensitivity (accuracy ~0.1 ng/m³) a sample volume of
20 l or more can be set.
Note: The sample volume determines the sampling duration. As a constant flow rate of
0.67 l/min is applied during sampling, a 1 l sample volume gives a sampling duration of ca.
90 seconds (a 10 l sample gives a sampling duration of ca. 15 minutes respectively).
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3. Operating instructions
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3.4.2 Set Cycle Duration
Press F2-Set Sample Parameters in the main menu and activate “Set Cycle Duration” by
moving the arrow to the corresponding line. Then press F2 and enter the desired cycle duration.
Characters can be deleted with the - key. The according sample volume is automatically
calculated and displayed.
The Cycle Duration is the total time needed for a complete measuring cycle, that means:
Sampling Duration, Zeroing, Heating, Trap Cooling, Trap Cleaning, …
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3. Operating instructions
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3.4.3 Auto Range Volume (only for Natural Gas / Tedlar Bag Version)
If Auto Range is activated the sample volume will be automatically adjusted according to the
mercury concentration of the sample. After Start Measuring the smallest possible sample volume
is selected automatically. If the absorbance signal is low, the sample volume will be increased
after each measurement until the absorbance is within the optimum range.
3.5 Start Measuring
Press in the Main Menu F1-Start Measuring. Now the analyzer automatically performs a
cleaning procedure and then starts sampling. After sampling is completed following steps will be
performed:
zeroing - trap heating - trap cooling – trap cleaning – trap cooling - sampling.
If the first measurement cycle has been completed, the system performs automatically the next
measurement cycle unless ESC is pressed or the instrument is switched off.
The result of the last measurement is displayed numerically at the centre of the bottom line, up to
5000 measurement results are displayed as bar graph. The time axis of the screen can be scrolled
with the F3 and F4 keys.
FIGURE: SCREEN DURING SAMPLING. THE HISTORY OF
READINGS IS DISPLAYED AS A BAR GRAPH. THE RESULT OF THE
LAST MEASUREMENT IS DISPLAYED IN A BOX ON THE BOTTOM
LINE.
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3. Operating instructions
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FIGURE: SIGNAL PEAK DURING THERMAL DESORPTION OF THE
GOLDTRAP.
Zeroing
Heating
Sampling
Trap Cooling
Purge Cell
Trap
Cleaning Trap Cooling
Trap Cooling
Purge Cell
Trap
Cleaning Cooling
UT-3000
Zeroing
Heating
Sampling
Cleaning Cooling
UT-3000 ng (Tedlar Version only)
FIGURE: UT-3000: MEASUREMENT CYCLE
Sampling
5 s to 15 min; depending on
sample volume
Zeroing Heating / Cleaning
11 s
20 s
Cooling
45 s for sample vol. 1 L and
up
>45 s for sample vol < 1 l
TABLE: DURATIONS OF THE ANALYSIS STEPS
Repeat Zero: Zeroing is repeated up to 10 times if the heating flow is out of range
(7 l/h < heating flow <13 l/h)
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3.6 Data Logger
The internal data logger of the UT-3000 can store data of up to 5000 measurements. The
maximum logging duration depends on the set sample volume, for a sample volume of 10 l the
logging capacity will be approximately 60 days.
If F3- Data Logger is selected in the main menu, the Logger Menu is displayed.
F1- Logger Mode: the logger function can be switched on or off.
F2- Show Logdata: the logged readings are displayed as a bar graph. The graph can be scrolled
with the F3 and F4 keys.
F3- Send Logdata to PC: If a PC is connected to the RS232 output of the Ultratracer and a data
transfer program (e.g. Hyper Terminal) has been started, data are sent to the PC after pressing the
F3 key (see chapter 3.6.2).
F4- Clear Logdata: the logged and stored data are erased.
3.6.1 Start logging of measurement data
After the data logger has been activated the measurement data are automatically logged whenever
the measurement mode is active. The status of the logger is indicated on the display (F1- Logger
Mode ON/OFF).
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3. Operating instructions
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For transferring the stored data to a PC the USB output of the UT-3000 has to be connected to an
USB interface of the PC. If you want to use the RS232 output, you have to change the factory
setting (USB) first (see 2.4.1), then connect the RS232 output of the UT-3000 with a serial
interface (COM1 or COM 2) of the PC, using a 1:1 connection cable.
Two sockets are available on the instrument back panel (see also chapter 3.5.2): a 9-pin D-Sub
socket for connecting the UT-3000 to a COM-port of the PC and a USB socket for connecting
the UT-3000 to a USB port of the PC.
If USB connection is used you have to install a USB driver (CDM Driver which comes with the
Hg-Transfer software) on your PC first. The USB-driver is on the CD-ROM with the HgTransfer software.
3.6.2 Sending logged data to a PC by using Hyper terminal
Select the Logger Mode menu as described under chapter 3.5.
Then following steps have to be performed on the PC (in WINDOWS):
Select Start All Programs Accessories Communications Hyper Terminal.
Start the program Hyper Terminal.
Enter a name for the connection (for example UT3000), select a symbol and press OK.
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Select Direct Connection COM1 (or COM2 if used)
and press OK.
Select Port Settings: 9600 bits per second / 8 data
bits / parity: none / stop bit: 1 / Flow Control:
hardware.Press the OK-bar.
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Select the Transfer pull down menu. Select Capture Text. Enter file name and press Start.
Press F3-Send logdata to PC on the UT-3000.
The logged data are now transferred from the UT-3000 to the PC. Starting date, starting time,
sample volume and measurement data are transferred in this order. Data sets are separated by
a carriage return.
3.6.3 Delete logged data
Select the Logger Mode as described above under 3.5.
Press F4- clear Logdata.
The Clear Logdata command will delete all measurement data stored in the RAM.
3.6.4 Import of data into EXCEL
The data once stored as text file with Hyper Terminal can easily be imported into an EXCEL
data sheet by selecting the data import function in EXCEL.
Measurement data are sent using a point (“.”) for decimals. Depending on the setting of
your EXCEL it may be necessary to convert the point into a comma (“,”). Use the search
and replace function of EXCEL to do this quickly.
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FIGURE: LOGGED DATA IMPORTED INTO EXCEL: DATE, TIME,
SAMPLE VOLUME, MERCURY CONCENTRATION [NG/M³]
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3.6.5. Using the HG-Transfer Software for Data Transfer to a PC
Calibration and analysis data are sent via serial output of the UT-3000 to a connected computer
using the Hg-Transfer software (comes with the instrument). The Hg-Transfer software has to
be installed on the connected computer before data are transferred. Data can be displayed, stored
(as .txt file or EXCEL® file) and printed.
Figure:
Hg-Transfer software main screen.
With choosing „Port Settings“
you can select the port of your computer
used for connection with the VM-3000
and the communication parameters.
By choosing „Configuration“ you can
choose the type of analyzer:
UT = UT-3000.
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Transferring of the data from the UT-3000 to the PC is started by clicking onto the
start icon.
During measuring there is a continuous transfer of readings.
The following data are shown:
Date Time Status Sample Volume Measured Value
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When there are already logged data stored in the UT-3000, the whole log-file can be sent to the
PC using the Hg-Transfer-Software.
The values displayed in the Hg-Transfer window can be stored with the Save Logfile
command (EXCEL® format).
With the Save Continuously command results of a running measurement are
continuously stored (EXCEL® format).
With pressing About (i) you can check which version of hg-Transfer-Software you are
using.
With choosing Exit you are leaving the Hg-Transfer software.
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4. Calibration
A calibration is recommended to be performed regularly according to applied quality standards.
Go to the main menu and press F4: Calibration.
In the Calibration Mode menu you can select:
F1- to show the last performed calibration
F2- to show the history of all calibration data (can be deleted with F4)
F3- to perform a span check
F4- to perform a new calibration.
4.1 Show actual calibration
Press F1 in the Calibration Mode menu. The actual calibration parameters are displayed on the
screen.
By pressing the arrow-key one can have a look on the calibration data and on the calibration
curve.
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4.2 Show all calibrations
Press F2 in the Calibration Mode menu. A list indicating all previously stored calibrations is
displayed.
The three-letter-code in the right column means:
man
manual calibration
aut
automatic calibration
err
calibration data of an automatic calibration were out of range; in this
case the data of the previous calibration are used.
Allowed range of calibration equation: Y= aX+b; where
0.00002<a<0.00015 and –0.001<b<0.001
NOTE: the calibration data table can completely be cleared by pressing F4 !
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4.3 Perform Span Check
If F3- Perform Span Check is selected in the Calibration Mode menu a manual span check can
be performed. A calibration unit (see 4.4.2) has to be connected by cable (Pt100), this tells the
analyzer the mercury concentration of the calibration gas.
After pressing the F3-button the analyzer will be prepared for the span check by the standard
cleaning routine of GoldTrap : Zeroing / Trap cleaning / Trap cooling / Zeroing / Trap
cleaning / Trap cooling / Zeroing / System Evaluation / Trap cooling.
Then a volume of calibration gas has to be injected into the calibration port on the front side of
the analyzer. The volume (1-999 µl) has to be typed in and confirmed by pressing ENT.
4.4 Perform New Calibration: Manual Calibration
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F1 is pressed in the Calibration Mode menu in order to perform a manual calibration.
Now you can select if a known mass of mercury or a known volume of mercury calibration gas
is injected into the calibration gas port: F1- Enter pg or F2- Enter µl.
Note: the F2- Enter µl command can only be used with the Static Calibration Set
(available as an accessory to the UT-3000) connected to the UT-3000.
Manual Calibration
F1
Enter pg
F2
Enter µl
F2
Cal. Mode Y=aX with F2 Y=aX + b
Toggle
ESC <<< Back
By pressing F2 the type of calibration function can be selected: with zero offset (Y= aX+b) or
without zero offset (Y= aX).
For manual calibration the calibration function Y=aX is recommended.
4.4.1 Manual Calibration: Enter pg
Go to 4.4.1.2 if the Calibration Set A (supplied as an accessory for the UT-3000) is used
as a calibration gas source.
This mode is used if a known mercury mass is injected into the Calibration Port of the UT-3000
using a calibrated syringe. It is possible to use any mercury calibration gas source, for example as
described in method VDI 2267/Part 8 [Measurement of the mass concentration of mercury.
Sampling by sorption as amalgam and determination by atomic absorption spectrometry (AAS)
with cold vapor technique].
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The calibration is carried out by following steps:
a) Make sure a new septum has been inserted in the instrument calibration port.
b) Press F1- Enter pg.
c) Type the mass of mercury [in pico-gram Hg] which is contained in the injected volume
and press ENT.
d) Fill the syringe to be used with calibration gas from the calibration device.
e) Push the capillary of the syringe through the septum of the calibration port on the front
panel of the UT-3000 and inject the calibration gas.
f) Press ENT. After a pause of 10 seconds the GoldTrap is automatically heated and the
measuring signal is recorded.
g) Repeat step a-d for additional calibration points.
h) Press F1 if no further calibration points should be measured.
Enter the mass of mercury to be injected into the calibration port. Recommended range for
calibration: 10 … 5000 pg for full range measurements or 10 ... 500 pg for low range
measurements.
Inject calibration gas and press ENT.
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Waiting time 10 sec.
End of Calibration
If the last calibration standard has been injected, press F1- End. Now the calibration function is
calculated automatically. An outlier is marked as a square. It can be accepted to be included in
the calibration function (F1- Yes) or it can be excluded from the calibration function
(F2- No).
If the outlier is not accepted (F2- No), the user is asked to repeat the calibration point.
On a second page calibration data are
displayed.
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On a third page the parameters of the
calibration function are displayed.
The main menu is displayed again after the calibration mode is left.
Practical recommendations for performing a calibration:
Mercury masses should be within the same range like the measuring range. Static calibration
sources (= mercury filled bottles with headspace) deliver calibration gas with comparatively high
mercury concentrations (ca. 12 - 14 pg/µl at room temperature). For a low measuring range of 0.1
to 10 ng/m³ the mercury masses injected should be ideally from 1 pg to 100 pg. However,
1 pg will be difficult to apply as this would require at room temperature a very small volume (0.1
µl) which is not practical. In practice, volumes from 1 µl to 100 µl will be used.
Use the syringe delivered with the Static Calibration Set or alternatively a syringe with
a capillary length of 50-52 mm ! Do not use a syringe with a different capillary length !
How to calculate the mercury mass ?
Read the temperature of the mercury calibration bottle as exactly as possible.
Determine the mercury concentration from either the table which usually comes together with the
calibration device or from below calculation formula.
Calculation of mercury saturation concentration in headspace after equilibration:
where: A= 3216522.61
B= 8.134459741
C= 3240.871534
T= absolute temperature (= Temperature in °C + 273.2)
From the mercury concentration calculate the mass of mercury which is in the volume which
shall be injected. For example, if the mercury concentration of the calibration gas is
16.700 µl/l, one µl contains 16.7 pg Hg and 10 µl will contain 167 pg Hg.
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4.4.2 Manual Calibration: Enter µl
A Mercury Instruments Static Calibration Set is connected to the UT-3000. The user has only
to enter the volume of the injected calibration gas and the instrument automatically calculates the
mercury mass from volume injected and calibration cell temperature. For calibrations in the
lowest measuring range it is recommended to use volumes from 1 µl to 10 µl.
FIGURE: CALIBRATION SET FOR MANUAL CALBRATION (LEFT: CLOSED; RIGHT: OPENED)
connect to UT-3000
Syringe
Insulation
Insulation
Glass frit
HG
HG
Activated sulfurized carbon
Peltier
cooler
Ventilator
FIGURE: SCHEMATIC DRAWING OF THE MERCURY CELL OF THE
STATIC CALIBRATION SOURCE.
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The Mercury Instruments Calibration System consists of a specially designed mercury vessel
surrounded by an aluminium jacket that is cooled by a thermoelectric cooler. The temperature of
the mercury vessel is exactly measured with a high precision temperature sensor. The mercury
chamber contains elemental mercury of high purity. The electronic temperature sensor has to be
connected to the UT-3000 ULTRATRACER using the cable delivered with the system. The
temperature of the calibration gas and the concentration of mercury are displayed on the UT-3000
screen if a calibration is performed.
Using the Static Calibration Unit:
CAUTION: never tilt the Static Calibration Unit nor turn it over during use!
Prevent from shocks !
For transportation remove the septum cap from the mercury vessel and close it with a
screw cap. Do not apply force to the mercury containing glass bottle !
Used septum may have small mercury droplets on its surface: be careful when
removing it. Use a small piece of wire (paper clip) to remove the septum from the red
plastic cap. Place septum and wire into a plastic bag for disposal.
a) Place the calibration unit on a clean, stable and flat surface.
Make sure that the room is well ventilated or use a fume hood whenever you open
the mercury cell !
Take the red septum cap and make sure that a new septum has been inserted.
Open the cover of the calibration unit by twisting the latch. Remove the red cap which
closes the mercury cell for transportation and store it in a safe place. Note that there may
be small droplets of mercury clinging onto the surface of the septum, therefore handle
the cap and the septum with care ! Do not touch the septum with fingers. Screw the
red septum cap (with a new septum !) onto the glass thread of the calibration cell.
b) Connect the power supply (round plug) to the calibration unit. The green LED will light
and the internal Peltier cooler will start to operate.
c) Allow the system to stabilize for at least one hour.
d) Take the syringe which is included in the system and hold it vertically. Push the capillary
of the syringe carefully through the septum of the calibration unit as far as possible,
always holding it vertically.
Do not apply too much force to the septum and the screw cap, as these are mounted onto
a glass bottle which contains the mercury.
Important: hold the syringe vertically as long as the tip of the capillary is inside the
calibration cell ! Otherwise there is the risk of contamination of the syringe with liquid
mercury which finally may result in a contamination of the calibration port of the UT-3000
analyzer.
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e) Purge the syringe with calibration gas by pulling and pushing the plunger slowly a few
times. Then pull the plunger a little bit further than it is necessary to get the desired
volume and pull the syringe vertically out from the septum.
f) Move the plunger exactly to the desired volume and push the tip of the syringe capillary
into the septum of the of the calibration port on the front panel of the UT-3000. Push it all
the way as far as possible to make sure the tip is at the correct position. Try to center the
capillary so that it can penetrate the calibration port without getting stuck. Inject the
calibration gas by pushing the plunger of the syringe slowly. Then pull the capillary out of
the calibration port and put the syringe down.
CAUTION: Contamination of parts of the syringe or the calibration port of the UT3000 with liquid mercury has strictly to be avoided ! Even smallest droplets of
mercury which cling to the syringe capillary or the septum of either the calibration
device or the calibration port will cause a severe contamination. Indication for a
contamination are: too high absorbance values of calibration points, erratically
scattered calibration points, unexpected high measurement peaks. In this case all
the equipment which may have been contaminated has to be exchanged, including
septa, syringe capillary or even the whole syringe if contaminated inside.
Figure: use closed cap for transportation (left) and septum cap for calibration (right)
Performing a manual calibration using the Static Calibration:
1. Make sure a new septum has been inserted in the calibration port of the instrument.
2. Check if for Cal. Mode X= aX is selected (recommended), now press F2- Enter µl in the
Manual Calibration menu.
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Manual Calibration
F1
Enter pg
F2
Enter µl
F2
Cal. Mode
Y=aX
ESC <<< Back
3. The temperature and the saturation concentration of the calibration cell will be displayed.
Type the volume of mercury which is to be injected and press ENT.
For the first calibration point it is recommended to enter “0” for the volume, in this case
no calibration gas has to be injected.
4. Inject the chosen volume of calibration gas following the steps a-f of the above
description of how using the static calibration source.
5. Press ENT. After a pause of 10 seconds the GoldTrap is automatically heated and the
measuring signal is recorded.
6. Repeat step 1-3 for additional calibration points.
7. Press F1 if no further calibration points should be measured.
Now the calibration data will be displayed as described in the following.
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FIGURE: PULLING A VOLUME OF CALIBRATION
GAS FROM THE CALIBRATION CELL WITH A 10 µL SYRINGE
.
NOTE: hold the syringe in a vertical position to avoid contamination !
FIGURE: INJECTION OF CALIBRATION GAS INTO THE CALIBRATION PORT OF THE UT-3000
4.4.3 Examples for calibration functions
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The calibration is linear over a wide range up to ca. 5000 pg Hg absolutely (equivalent to
5 µg/m³ for 1 litre sample volume or 0.5 µg/m³ for a 10 l sample volume). Above this range the
calibration is automatically calculated using a polynomial function which is useful up to ca.
15000 pg Hg (equivalent to 15 µg/m³ for a 1 litre sample volume).
Calibration UT-3000
06.12.2002 / Trap # 230
y = 0,0001x + 0,0005
R2 = 0,9998
0,07
Absorbance signal
0,06
0,05
0,04
0,03
0,02
0,01
0
0
100
200
300
400
500
600
700
Calibration gas injected Hg [ pg]
FIGURE: CALIBRATION GRAPH FOR 0 … 600 PG HG RANGE
Calibration UT-3000
06.12.2002 / Trap # 230
y = 9E-05x + 0,0079
R2 = 0,9995
0,3
Absorbance signal
0,25
0,2
0,15
0,1
0,05
0
0
500
1000
1500
2000
2500
3000
3500
Calibration gas injected Hg [ pg]
FIGURE: CALIBRATION GRAPH FOR 500 …3000 PG HG RANGE
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FIGURE: CALIBRATION GRAPH IN LOW RANGE (0-3,5 NG/M³) WITH CONFIDENCE RANGE
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4.5 Perform New Calibration: Automatic Calibration (Option)
The UT-3000 Ultratracer can be equipped with the Automatic Calibration Unit which is available
as an accessory. This unit has a Peltier element cooled mercury saturation chamber, from which
saturated air is drawn by means of a digital syringe. This air is injected automatically in a stream
of zero air entering the UT-3000.
It is recommended to place or mount this unit under the UT-3000.
It is important to install all connections between the Automatic Calibration Unit and
the UT-3000 before the system is set into operation !
FIGURE: AUTOMATIC CALIBRATION UNIT FOR UT-3000
4.5.1 Connecting the Automatic Calibration Unit with the UT-3000
a) The calibration gas outlet tubing of the Calibration Gas Unit has to be connected with the
calibration gas inlet tubing of the UT-3000 (see figure below).
b) The cable for the temperature sensor (two round 4-pin plugs) has to be connected with the
according sockets on the rear side of the UT-3000 and the Automatic Calibration Unit.
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FIGURE: CONNECTION OF TUBING ON BACK SIDE OF UT-3000 AND OF AUTOMATIC
CALIBRATION UNIT
4.5.2 Activating the Automatic Calibration Function
Switch on the Automatic Calibration Unit first, then switch on the UT-3000.
After Lamp has stabilized and the main menu is displayed press ESC and enter the code 777 +
ENT. Now activate the automatic calibration mode. Press ESC again to return to the main menu.
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4.5.3 Cal. Concentration
F2- Automatic Calibration is selected in the Calibration Mode menu.
Now press F1-Cal. Concentration to enter concentrations used for calibration. Up to twelve
calibration points can be entered.
If finished press ESC.
4.5.4 Cal. Interval
F2- Cal. Interval: calibration start time or interval between automatic calibrations:
You can enter either a time interval (1-24 hours) which determines the time between two
automatic calibrations or a fixed start time at which the automatic calibration will start daily.
The arrow indicates the active mode, it can be changed with the 68-keys.
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4.5.5 Manual Start of the Automatic Calibration
F3- Start automatic Calibration is selected in the Calibration Mode menu. Now an automatic
calibration is immediately started using the concentrations entered under F1-Cal. Concentration.
The following screens can be noticed consecutively:
After that the standard cleaning routine of the GoldTrap is done:
Trap Cleaning / Trap Cooling / Zeroing / Trap Cleaning / Trap Cooling / Zeroing /
Trap Cleaning / Trap Cooling
Now the routine for each calibration point is starting and repeated as often as your amount of
different concentrations.
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After that there is again a short cleaning sequence of the GoldTrap:
Heating / Trap Cooling / Zeroing / Trap Cleaning / Trap Cooling / Syringe Conditioning
The amount of indicated steps are calculated from the concentration levels you have fixed in the
calibration concentration menue (4.5.3).
After a another short zeroing you get the heating peak of the injected mercury concentration.
4.5.6 Automatic Start of the Calibration
The sequence of the calibration routine is the same than in the chapter before of the manual
starting. There is just one difference:
When you have fixed a calibration interval or a calibration time there is an automatic check
before the start of calibration whether the time span to the calibration is shorter than the next
measuring cycle. If this is the case there will be a stop of the measuring and it’s shown the
following screen:
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4.5.7 Empty Syringe
F4- Empty Syringe is selected in the Calibration Mode menu. By pressing F4 this function can
be switched on or off. If Empty Syringe is On, then after each mercury injection the syringe is
filled with air and re-injected into the gold trap.
4.5.8 Cal. Mode
Page 2 of the Automatic Calibration Menu, press F1- Cal. Mode. In this menu the kind of
calibration function calculated from the calibration results can be set: either a linear least square
regression (Y= aX+B) or a regression without intercept (Y= aX).
4.5.9 Activation of Automatic Span Calibration
This function has to be activated if an automatic one-point calibration should be performed. It is
also necessary to activate this function if an externally triggered span check should be carried
out.
Press ESC- Service in the Main menu. Enter the code 999 + ENT. Activate the Automatic
Calibration Mode (F1) or the Automatic Span Calibration (F2). The automatic calibration or the
automatic span calibration will be carried out at the pre-set time intervals or at the pre-set times if
measurement has been started.
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5. Service-Menu
If ESC- Service is pressed in the main menu the service code input mask will appear on the
display.
Enter the code 3 2 1 + ENT
Now the Service menu is displayed. In the centre of the bottom line the temperature of a
connected calibration device is indicated.
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5.1 Set Date and Time
Press F1- Set date / time in the service menu.
The date can be edited by pressing F1 and the time by pressing F2.
5.2 Device Data
In this screen information for the service engineer is displayed (operational hours, lamp
voltage, heating coil cycles, software version)
5.3 Show Flow
In this screen the flow for sampling and the flow during thermal desorption of the mercury from
the GoldTrap (heating flow) can be read.
a) Heating flow: press F1. Stop flow reading by pressing ESC.
b) Sampling flow: press F2. Stop flow reading by pressing ESC.
The allowed range for heating flow is 8.5 – 11.5 l/h, for sampling flow 38 – 42 l/h. An error
message will appear if the flow is out of these ranges. The value displayed on the right bottom is
the pump voltage. The allowed range for this voltage is 6 – 11 V. During measurement mode an
error message will appear if the voltage is out of this range.
5.4 Purge Repetitions (for Automatic Calibration Option only)
The parameter set for purge repetitions is only available when the automatic calibration mode has
been activated. It determines how often the automatic syringe is purged with calibration gas for
conditioning.
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5.5 Change Syringe (for Automatic Calibration Option only)
This function is only available when the Automatic Calibration function has been activated
(Service code 777). It is necessary for change of the syringe inside the Automatic Calibration
Unit. The command Change Syringe moves the piston of the syringe to a 50 % position which is
necessary to remove the syringe. The Reset command pushes the piston back again into the
syringe.
5.6 Set Calibration Data
In this window calibration parameters for the built in mass flow sensor and the parameters of the
analytical calibration can be set. This is useful if these values are lost due to service work.
Service
Mode
Set
Calibration
Data
F1
Set Flow-Calibration
F2
Set Meas-Calibration
F2
Set T-Cal. Cell Calib.
ESC <<< Back
5.6.1 Set Flow Calibration
By pressing F1 – Set Flow-Calibration you can enter manually the calibration data of the
internal mass flow controller, in case they are deleted (for example if the microprocessor-battery
is empty). You will find those data on the test-certificate of your UT-3000, which was in the
delivery amount.
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5.6.2 Set Measuring Calibration
By pressing F2 – Set Meas-Calibration you can enter manually the values of the measuring
calibration, in case they are deleted.
5.6.3 Set T-Cal. Cell Calibration
By pressing F3 – Set T-Cal.Cell Calibration you can enter manually the values for the
calibration of the temperature sensor of the calibration device (either manual or automatic
calibrator).
Service Mode
Y = .......X +/- 0.......
F1
Set gradient
F2
Set constant
ESC <<< Back
5.7 Trap Counter
This window displays the total number of heating cycles of the GoldTrap ever carried out.
5.8 Set RS232 Mode
As a standard the RS232 output delivers measurement data sequentially as ASCII characters.
Optionally data can be output following a protocol for data acquisition systems from ISEO
(France).
5.9 Set Zero Duration
The instrument performs an automatic zero adjustment before each trap heating step (see also
chapter 3.5). In this menu the duration of the zeroing can be set to a value between 11 seconds
and 250 seconds. Standard setting is 11 seconds. This parameter has to be increased if during
operation of the system with real sample it is found that the reading towards the end of zeroing is
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not close to 0.00000 and still decreasing. This may be due to extremely high mercury
concentration or high benzene concentrations in the sample.
5.10 Set Status
In this window the function of the status contacts can be programmed, so that they will be opened
or closed when activated.
Service
Mode Mode
Set Status
F1 Status active
opened / closed
ESC <<< Back
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5.11 Special Service Codes
Following codes are available:
Code: Function:
Standard Service Menu, see beginning of this chapter
321
Standard / Tedlar Bag Mode
191
222
333
753
777
881
987
999
Offset T Cal.Cell / Zero Offset / Heating Flow /
Heating Flow Regulate
Evaluation Graph on/off
Flow Calibration (10 l/min – 3 points; 40 l/min – 3
points)
Calib. Syringe on/off
Absorbance correction function (A-factor)
allows to actuate valves
Automatic Calibration / Span Calibration
Recommended Setting
n.a.
Standard (Tedlar Bag Mode is
an option for special
applications)
0.00 °C / 0.0000 / 10 l/h /ON
ON
Only to be used for service !!!
(service tools required !!!)
As required by user
1.000
For service only
As required
Remarks:
191: Tedlar-Bag-Mode is only used for instruments optionally equipped for this method to
determine Hg in natural gas or other gas samples.
222: Zero offset- for correction of the analytical zero value, this value is subtracted from the
measurement peaks.
Temp offset- for correction of the offset of an automatic or manual calibration device.
Heating Flow: allows to set heating flow, shall not be changed from standard setting except
for special applications (high measuring range).
Flow Regulate: For service purpose only, shall not be changed from standard setting.
If “Heating flow regulate= ON“ then the pump is controlled by the mass flow meter signal
within +/- 2 l/h of the set value.
If “Heating flow regulate= OFF“, then the pump is fed with a constant voltage (7.5 V) and the
flow may vary within a range of +/- 3 l/h.
If the Flow is out of range, a Repeat Zero will be performed up to 10 times, after this the system
will be halted and an error message will be displayed.
333: Shows the peak during System Evaluation when on; a horizontal line is displayed when off.
753: For calibration service of flow meter only!
777: Only on if an Automatic Calibration Unit is installed. Has to be on if an automatic
calibration should be performed.
881: For service only!
987: For service only!; allows to actuate valves and status contacts.
999: Mode of automatic calibration can be selected: multiple point calibration or one point span
calibration.
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6. Maintenance
6.1 Spares and Accessories
ID #
Description of Part
101-07
101-21
201-04
203-02G
203-05
203-52
203-54
203-61
505-38
800-20
800-25
810-01
810-02
810-10
810-11
810-12
810-13
810-14
810-15
810-16
810-17
810-18
810-19
810-20
810-21
810-22
810-62
820-01
830-01
830-02
830-03
830-04
830-06
830-08
830-10
830-11
830-12
830-14
830-15
830-16
Particulate filter F400
Particulate filter, small version
Activated carbon cartridge
Optical cell
LC display
Microprocessor board
Detector module
UV lamp bulb (EDL)
Connector piece, for connecting UT-3000 and Auto Cal Unit
Sample bag, Tedlar, 10 l
Sample bag Tedlar, 3 l
Calibration set for manual calibration
Automatic Calibration Unit
Syringe, gas tight, 10 µl, for manual calibration
Capillary for 10 µl Syringe
Septa (pack of 10), 14 mm diam, for manual calibration set
Set of Septa (10 pcs), 6.5 mm diam, for UT-3000 Cal.Port
Ventilator for Automatic Calibration Unit
Syringe, gas tight, 25 µl, for Automatic Calibration Unit
PTFE piston for 25 µl syringe 810-15
Dryer cartridge, filled with desiccant, for Auto Cal Unit
Power supply, complete, for Automatic Calibration Unit
Closed cap for calibration cell
Septum cap for calibration cell
Saturation chamber, complete with insulating jacket
Peltier cooler block, complete with heat exchanger and Peltier element
Interface board
Protective and carrying case, for UT-3000 or Auto Cal Unit
Sample inlet dust filter, PTFE 0.25 µm, pack of 10
Valve, 2/3 way, for Goldtrap/Zeroing
Valve, 2/3 way, for heating/sampling flow
Electronic mass flow meter
Needle valve, brass, for sample flow adjustment
Needle valve, stainless steel, for heating flow adjustment
Pump, for sampling and heating gas flow
GoldTrap, complete with heating coil
Pt-100 converter module
Ventilator for UT-3000
Power supply, complete, for GoldTrap
Power supply board, for UT-3000
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830-17
830-20
830-24
830-95
830-96
830-98
840-02
840-03
840-04
page 56
Calibration port, complete, stainless steel
Holder for GoldTrap, incl. electronics
Particle filter, 60 µ; stainless steel
Tubing, complete set
Fuse set
Service kit
Pressure relief valve
T-joint
Backplane USB with 40p flatband-connection to interface board
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6.2 Technical drawings
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FIGURE: UT-3000 ID-NUMBERS OF PARTS
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UT-3000: ID-NUMBERS OF TUBING
REMARKS: 1. FOR TEDLAR BAG VERSION TUBING NO. 14 IS REPLACED BY TUBING NO.14T AND
TUBING NO. 15 IS OMITTED.
2. FOR VERSION WITH AUTOMATIC CALIBRATION UNIT TUBING NO. 2 AND 3 INCLUDING
COMPONENTS NO. 101-21/201-04 (WHICH ARE PLACED IN THE AUTOMATIC CALIBRATION
UNIT) ARE REPLACED BY TUBING NO.3S
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FIGURE: AUTOMATIC CALIBRATION UNIT, PART NUMBERS SEE SPARE PARTS LIST CHAPTER 8.4
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FIGURE: AUTOMATIC CALIBRATION UNIT, ID-NUMBERS OF TUBING
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6.3 Error messages
6.3.1 Lamp !
The installed electrodeless mercury lamp is monitored permanently. If its performance drops
under a certain limit the warning „LAMP!” indicates that it should be replaced within the next
days.
6.3.2 Sampling Flow out of Range!
This warning appears if the flow during sampling is out of the allowed range (38 – 42 l/h).
Possible reasons:
a) sample gas inlet filter plugged up
b) pump defective
c) needle valve for sample flow adjustment plugged up
Check filters, check if pump operates, re-adjust sampling flow (Chapter 6.9)
6.3.3 Heating Flow out of Range!
This warning appears if the flow during thermal desorption is out of the allowed range (8.5 –
11.5 l/h).
Possible reasons:
a) GoldTrap plugged up
b) pump defective
c) needle valve for heating flow adjustment plugged up
Check filters, check if pump operates, re-adjust heating flow (Chapter 6.9)
6.3.4 Temp. out of range ! See instruction manual!
This warning indicates, that the temperature of the connected calibration device is out of its
specified range.
6.3.5 Check heating coil !
This warning indicates, that the magnetic field sensor for the GoldTrap heating coil control has
detected, that no current is passing the heating coil. Cause may be a burnt coil or a defective
power supply.
6.3.6 T-Sensor not connected ! Connect T-Sensor of Calibration Cell!
This warning indicates, that the PT100 temperature sensor of a manual or automatic calibration
unit is not connected.
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6.3.7 Temp out of Range ! See instruction manual!
This warning indicates, that during calibration with a connected manual or automatic calibration
device the temperature is <6°C or >35°C.
6.3.8 Pump ! (flashing)
This warning indicates, that the flow counter is out of range (1-100 is correct) and pump voltage
is at its upper limit (12V)! Reason may be a malfunction of the pump, plugged valves 830-08 or
830-03, not correctly adjusted valves 830-08 or 830-03.
6.3.9 Lamp Stability!
This warning indicates that the UV lamp (which is checked during the last seconds of zeroing) is
unstable and needs to be checked by the service.
6.3.10 Logger full (flashing)
This warning indicates, that the remaining capacity of the data logger memory is zero.
6.3.11 No Sample!!!
This warning is for the NG (Natural Gas) version only. In case that no sample gas is delivered to
the sample inlet (for example sample line has been closed) this message warns the user. Twenty
seconds after sampling has started the flow is measured. If the Sampling Flow is then below
approx. 6 - 7 l/h the system automatically switches to zero air and counts down for one hour
before restarting measurement automatically.
6.3.12 EEP INIT; Warning No. 20:
Check Parameters! See Instruction Manual!
This warning indicates, that the EEPROM has been reset. Parameters (calibration, sample
volume, …) have to be checked and re-entered in case they have been lost.
6.3.13 Warning No. 50:
Check Calibration! See Instruction Manual!
This warning indicates, that the last calibration has been erased; a new calibration has to be
performed or entered in the service menu.
6.3.14 Warning No. 60:
Check Flow-Calibration ! See Instruction Manual!
This warning indicates, that the calibration of the flow meter has been erased; the parameters for
the flow calibration have to be entered in the service menu or the flow meter has to be recalibrated (by service).
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6.3.15 Warning No. 70; Check Calibration Data!
This warning indicates that the data of the last automatic calibration have been erased. A new
calibration has to be performed or manually entered in the service menu.
6.3.16 Warning No. 80; RS232 Communication Error; Connect Syringe!
This warning indicates, that a communication error between UT-3000 and the automatic
calibration module has occurred.
6.3.17 Warning No. 91; Check Calibration!
This warning indicates, that the parameters of the calibration are out of the feasible range:
slope should be between 0.00002 … 0.00015, offset should be between –0.001 … +0.001.
6.3.18 Repeat Zero
This warning indicates that the flow during Zeroing is out of range (< 8 l/h; > 12 l/h).
6.3.19 Low Sampling Flow
For UT-3000 with NG (natural Gas) software only!
This warning indicates, if a sample is measured from Tedlar Bag (Tedlar function in Service
menu, Code 191, =ON), that the sample flow is lower than 20 l/h.
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6.4 Troubleshooting
6.4.1 Unusual Measuring Peaks
An example for a non-typical peak is shown in the picture below.
The peak is more of triangular shape and the signal drops to negative values after the peak.
Figure: Example for an non-typical desorption peak
The reason may be precipitation in the tubing at the outlet of the GoldTrap (= tubing which
connects GoldTrap and optical cell, see picture below).
In this case it is recommended to replace the contaminated tubing.
Figure: Tubing at outlet of GoldTrap. The arrow indicates the
position where precipitation might occur.
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6.5 Routine Maintenance
6.5.1 Replacement of Membrane Filter
Under normal circumstances the sample membrane filter has to be inspected regularly. If a
deposit of particulate matter or staining is visible, the filter has to be replaced. For filter
replacement, turn the filter slightly and pull it out. Insert the new filter into the filter holder and
push it carefully over the white nozzle in the centre of the filter holder. Turn the filter slightly.
6.5.2 Replacement of the filter cartridges
A) UT-3000 Unit
Inside the instrument there are two filter cartridges: one activated carbon cartridge and one
particulate filter cartridge. These should be replaced annually.
First loosen the two screws in the back of the UT-3000 photometer unit and remove top cover of
the case. Do not pull with force as a ground wire is mounted to the cover. The ground wire can
be disconnected by pulling the plug on one end. The filter cartridges are now visible and can be
removed from their holding clamps. To replace the cartridges, the connected hose has to be
pulled off.
FIGURE: OPENING OF THE TOP COVER OF THE INSTRUMENT AND REMOVING THE CARTRIDGES OF THE UT-3000
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B) Automatic Calibration Unit (option)
Inside the Automatic Calibration Unit there are four filter cartridges: two activated carbon
cartridges, one particulate filter cartridge, and one desiccant cartridge. These should be replaced
annually.
First loosen the two screws in the back of the Automatic Calibration Unit and remove top cover
of the case. Do not pull with force as an ground wire is mounted to the cover. The ground wire
can be disconnected by pulling the plug on one end. The filter cartridges are now visible and can
be removed from their holding clamps. To replace the cartridges, the connected hose has to be
pulled off.
FIGURE: OPENING OF THE TOP COVER OF CALIBRATOR AND REMOVING THE CARTRIDGES
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6.6 Fuses
The main fuse compartment is located on the rear of the instrument between the power cord
receptacle and the power switch. It contains two fuses.
Pull power plug before opening the fuse compartment!
Fuse type: the rating of the fuses to be used as spares depends on the operation voltage
indicated on the rating plate of the instrument:
230V Operation voltage: Fuse type T 1.6 A (time lag)
115V Operation voltage:
A third fuse (3.15 A medium time lag) is located on the power supply board inside the
photometer. It can be changed after opening the cover of the instrument.
Pull power plug before opening the photometer!
3.15 A fuse
FIGURE: POWER SUPPLY BOARD INSIDE PHOTOMETER
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The Automatic Calibration Unit has two main fuses which are located in the fuse compartment.
This is located on the rear of the instrument between the power cord receptable and the power
switch.
Pull power plug before opening the fuse compartment!
Fuse type: The rating of the fuses to be used as spares depends on the operation voltage
indicated on the rating plate of the instrument:
230V Operation voltage: Fuse type T 1.0 A (time lag)
115V Operation voltage:
6.7 Cleaning the GoldTrap
In some cases the sensitivity of the analyzer may be clearly reduced compared to the new
instrument and the measurement signal gets weak. One reason for this may be a contamination of
the GoldTrap. One may try to remove this contamination by rinsing the inside of the GoldTrap
with concentrated nitric acid.
WARNING: Nitric acid is a toxic, harmful, dangerous and corrosive
reagent. Only personnel which has been sufficiently trained in working
with such chemical substances is allowed to handle nitric acid and to
perform the following steps!
Concentrated acids shall be handled in a fume cupboard!
Protective laboratory clothes, safety goggles and laboratory gloves have
strictly to be worn!
The GoldTrap has to be uninstalled following the steps in chapter 7.6. Over both ends of the thin
ceramic tube which poke out from the aluminium cylinder a suitable plastic tubing (PVC,
Tygon®) is pushed so that a tight connection is formed. The plastic tubing on one end shall be
long enough to reach the bottom of a 50 ml or 100 ml glass beaker. The plastic tubing on the
other end is connected with the tip of a plastic syringe (a 10 ml medical syringe will work).
Approximately
20 ml of concentrated nitric acid are filled into the glass beaker (fume hood!). The GoldTrapSyringe assembly is positioned over the beaker so that the free end of the tubing dips into the
nitric acid. The piston of the syringe is pulled carefully and slowly so that nitric acid is sucked
through the GoldTrap and appears in the syringe. After waiting for approximately 30 seconds the
acid is pushed through the GoldTrap the other direction by pushing the piston of the syringe.
Care has to be taken that no acid splashes out from the beaker.
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After this the GoldTrap-syringe assembly is carefully removed from the beaker with nitric acid
and the open end of the plastic tube is immersed in a beaker with filled with water. The water is
pulled into the syringe thus rinsing the GoldTrap and removing the nitric acid. After that the
GoldTrap-syringe assembly is removed from the water filled beaker and placed over a sink or a
suitable container which shall hold the purge water (= acidic water). By pressing the piston of the
syringe the rinse water is released from the GoldTrap. This rinsing step is repeated at least five
times in order to remove any salts or acids. Then the GoldTrap is disconnected from the syringe
and all tubing is removed. It has to be dried with a flow of nitrogen or clean air before it is
installed into the instrument again.
CAUTION: the acid used for cleaning must only be in contact with the interior of the thin
ceramic tube in the center line of the GoldTrap and must never get into contact with the
cylindrical aluminium part or with the coil inside the aluminium cylinder or with the
connection cables and plug. This will damage the GoldTrap within a short time!
FIGURE: CLEANING OF THE GOLDTRAP WITH NITRIC ACID
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6.8 Replacement of the GoldTrap
The GoldTrap requires replacement if the slope of the calibration curve is below 0.00004. A new
GoldTrap (part No. 830-11) will be inserted instead of the used one which may be returned to the
manufacturer for regeneration.
Pull power plug before opening the photometer!
First loosen the two screws in the back of the UT-3000 photometer unit and remove top cover of
the case. Do not pull with force as an ground wire is mounted to the cover. The ground wire can
be disconnected by pulling the plug on one end. The GoldTrap is now visible.
Identify the power supply cable of the GoldTrap and disconnect it by pulling the small plug.
Carefully disconnect the tubing at the gas inlet and gas outlet of the GoldTrap (see picture
below). Try to push the end of the tubing with fingernails instead of pulling the tubing. Try to
balance force to both sides of the GoldTrap and avoid to pull the thin brown coloured ceramic
tube to one side, it should always stay centred.
After the plug and the tubing have been disconnected the GoldTrap can be removed from its
holding clamps and the new GoldTrap can be inserted. After that the tubing are connected to the
GoldTrap again and the cable is plugged in.
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Figure: opening of the top cover of the instrument and position of GoldTrap
FIGURE: DEINSTALLATION OF GOLDTRAP:
(LEFT UP) REMOVING THE PLUG
(RIGHT UP) REMOVING THE TUBING
(LEFT) REMOVING THE GOLDTRAP
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6.9 Flow Adjustment (for qualified personnel only)
After replacement of components which may influence the flow (GoldTrap, filters, pump) it may
be necessary to readjust the flow. Select from the Service Menu Show Flow (see chapter 5.3).
6.9.1 Heating Flow Adjustment
Read Heating Flow
Select F1- Heating Flow. Allow to stabilize for approximately one minute. The actual flow will
be indicated on the screen and should be between 9.8 l/h and 10.2 l/h. In the right bottom corner
the pump voltage will be displayed. It should be in the range of 6.5 … 10.0 Volts, optimum
7-8 Volts.
Maintenance work on the opened and powered instrument must
only be done by qualified personnel.
Parts of the instrument interior are under high voltage. UV-beams
are produced inside the instrument. If safety regulations are
ignored physical and/or material damages could occur.
Adjust Heating Flow
If adjustment is necessary, open the instrument cover (read warning above !) and adjust by
slowly turning the horizontally positioned setting knob of needle valve 830-08. Turning the knob
to the left will decrease the voltage. Turn until voltage is in the desired range and observe if flow
is in the range of 9.7 … 10.3 l/h.
6.9.2 Sampling Flow Adjustment
Read Sampling Flow:
Select F2- Sampling Flow. Allow to stabilize for approximately one minute. The actual flow will
be indicated on the screen and should be between 39.7 l/h and 40.3 l/h. In the right bottom corner
the pump voltage will be displayed. It should be in the range of 6.5 … 10.0 Volts, optimum
7-8 Volts.
Maintenance work on the opened and powered instrument must
only be done by qualified personnel.
Parts of the instrument interior are under high voltage. UV-beams
are produced inside the instrument. If safety regulations are
ignored physical and/or material damages could occur.
Adjust Sampling Flow
If adjustment is necessary, open the instrument cover (read warning above!) and adjust by slowly
turning the vertically positioned setting knob of needle valve 830-06. Turning the knob to the left
will decrease the voltage. Turn until voltage is in the desired range and observe if flow is in the
range of 39.7 … 40.3 l/h.
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FIGURE: NEEDLE VALVES FOR HEATING FLOW ADJUSTMENT AND
SAMPLING FLOW ADJUSTMENT
6.10 Gold Trap Assembly
The GoldTrap is snapped into holding clamps which are mounted on an angled metal plate. This
plate holds following electronic parts on its down side:
(a) A driver transistor that switches the power for the heating coil of the GoldTrap,
(b) An optical coupler,
(c) Two resistors.
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7. Technical Information
7.1 Technical specifications
Instrument type
Manufacturer
Measuring component
Measurement principle
Measurement wavelength
UV-source
Method of stabilising
Optical cell
Cell temperature
Measuring range a) lowest range
b) medium range
c) screening mode
Detection limit according DIN 32645
Linearity over the 0.2 to 15000 ng/m³ range
Reproducibility
Sampling flow
Goldtrap heating flow
Digital output signal
Data logger capacity
Electrical power consumption
Power supply
UT-3000
Mercury Instruments GmbH, Liebigstr. 5,
85757 Karlsfeld, Germany
Total Gaseous Mercury (TGM)
Atomic absorption, cold vapor method,
Preconcentration with GoldTrap
253.65 nm
electrodeless mercury discharge lamp
optically with reference beam; thermally
entirely of fused silica Suprasil, l= 230 mm
ca. 70 °C, heated
0.1 ng/m³-1000 ng/m³ at 10 l sample volume
1 ng/m³-3000 ng/m³ at 1 l sample volume
10 ng/m³ - 30000 ng/m³ at 0.1 l sample
volume
1 pg absolutely or 0.1 ng/m³
1.5 % or better
5 % or better at 14 pg Hg
1 % or better at 1500 pg Hg
40 l/h
10 l/h
Serial (USB/RS 232) for PC connection,
5000 data sets
Photometer: max. ca. 250 VA
Calibration Unit: ca. 70 VA
230 VAC / 50 Hz ; 115 VAC / 60 Hz
(option) ; 12 V DC (option)
Dimensions
45 x 15 x 35 cm (WxHxD) without filter
Weight
ca. 12 kg
7.2 Influencing effects
Operating temperature
Operating humidity
CE approval
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0 °C ... 40 °C
max. ca. 90 % R.H., no condensing
humidity
according to 89/336 and 73/23 EEC
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7.3 Storage and transport
The interior of the UT-3000 and the calibration device should be kept save from moisture
and hard shocks. Vibrations caused by transport in a car do not harm the UT-3000.
The Automatic Calibration Unit and the Manual Calibration Unit must
always be carried or transported horizontal, it must never be tilt or turned over. Hard
shocks must be avoided.
In case of damage that leads to a mercury spillage observe the material safety data sheet in
the appendix. Consult an expert!
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Bag Version)
page 80
8. Version for Hg determination in natural gas and other
hydrocarbon gases (Tedlar® Bag Version)
A special version of the UT-3000 analyser can be used for measurement of mercury in natural
gas and derivatives. For these applications special precautions have to be made to prevent
explosion. The appropriate safety regulations have strictly to be observed. This instrument must
not be operated in hazardous areas. Customized versions are available for installation in an
hazardous area, contact the manufacturer.
FIGURES: PLANTS FOR NATURAL GAS PRODUCTION. SPECIAL UT-3000 SETUP ALLOWS TO MEASURE HG CONTINUOUSLY
OR MANUALLY.
8.1 Sampling system for mercury determination in natural gas
The Natural Gas Sampling System is dedicated for taking a sample stream from a pressurized
natural gas source. This source may be a storage tank or a pipeline containing or conducting
compressed natural gas. The sample can be filled into a special sample bag (Tedlar bag) and
carried to the analyzer. Sample bags come as accessories with the UT-3000 Mercury Ultratracer.
The Natural Gas Sampling System reduces the primary high pressure of the sample source (up
to 200 bar) to a pressure below 1 bar so that the gas can be filled into a sample bag or fed to a
continuously operating analyzer (for example the UT-3000 Mercury Ultratracer). Pressure
reduction is performed with a high precision pressure regulator. To avoid condensation due to the
Joule-Thompson effect the pressure regulator is electrically heated. Especially for mercury
analysis it is important to precondition all surfaces of the system which come into contact with
the sample. To guarantee a suitable preconditioning the sampling system has a bypass stream at
the low pressure side. The bypass flow may be adjusted with a needle valve. The bypass flow is
indicated by a flow meter. With a ball valve at Sample IN the sampling system can be isolated
from the gas source. A second ball valve allows closing the outlet sample flow. In order to avoid
ingress of water droplets or aerosols into the sample bag or analyzer a special coalescing filter is
installed in the sample stream.
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Bag Version)
page 81
Figure: Natural Gas Sampling System
schematic gas flow
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FIGURE: NATURAL GAS
SAMPLIN SYSTEM
FRONT VIEW
FIGURE: NATURAL GAS
SAMPLING SYSTEM
TOP VIEW, OPENED
FIGURE: SETUP OF SAMPLING SYSTEM AND UT-3000 ANALYZER FOR HG MEASUREMENT FROM A SAMPLE CYLINDER
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FIGURE: SAMPLING CONTINUOUS SAMPLING OF NATURAL GAS
(BENCHAMAS OFFSHORE PLATFORM; THAILAND)
8.2 Setup for continuous measurement of Hg in natural gas
For automatic 24 hours per day monitoring an optional setup for continuous measurement is
available. The analyser system is installed in a safe place out of the hazardous zone. The sample
is extracted from the gas pipeline with a heated sampling system (described under 8.1. The
sample is then guided to the analyser through a stainless steel/Teflon (PFA) capillary. The
analyser is purged with air to avoid formation of an explosive atmosphere in case of leakage. In
addition a built in gas sensor shuts the system down and stops the sample gas flow by closing a
valve which is installed in the sample line.
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8.3 UT-3000 version for analysis using a sample bag (Tedlar® Bag)
NOTE: the Tedlar Bag Method described in this chapter requires the corresponding
software which is installed as an option. The Tedlar Bag Method has to be activated in the
Service Menu by entering the Code 191 (see also Chapter 5.10).
The bag sampling technique offers a simple, low cost and yet precise method to determine the
mercury concentration in natural gas (or other gas samples).
A suitable sample bag (3 liters or 5 liters Tedlar® bag, available as an accessory) is filled with
the gas sample. The valve of the bag is closed (observe the instructions of the sample bag) and
the bag is transported to the UT-3000 analyzer which has been set up at a safe place.
If flammable gases are filled into the sample bag extreme care has to
be taken that the bag does not come into contact with hot surfaces,
sparks, open fire etc. which could cause ignition of the bag. Severe
physical or material damages could occur. Never use sample bags
which are damaged or may leak ! It has also strictly to be avoided that
air or oxygen can enter the sample bag. This could lead to the
formation of an explosive gas mixture. The bag has to be emptied
completely before filling with new sample. Do not store filled sample
bags in badly aerated rooms. Empty the sample bag after use
observing safety precautions for flammable gases.
FIGURE: CONNECTING A
SAMPLE FILLED TEDLAR
BAG TO THE UT-3000
SAMPLE INLET
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8. Version for Hg determination in natural gas and other hydrocarbon gases (Tedlar®
Bag Version)
page 85
8.3.1 Setup of the UT-3000 analyzer
Safety instructions – read carefully:
Place the UT-3000 onto a flat and dry surface (table). Take care that
the ventilation holes on the bottom side of the analyzer are not
covered by objects (like a sheet of paper, etc.) and air can free
ventilate. This is important that in case of an internal leakage of the
analyzer no explosive atmosphere can form inside the analyzer.
During sample aspiration into the analyzer flammable gas will blow
out from the gas outlet fitting on the rear side of the analyzer. Take
care that the gas which comes out from this fitting is led to a well
ventilated place without any ignition sources. It must be avoided that
this gas can accumulate in closed volumes. If necessary use small
tubing (ID 4 mm) to guide the gas away from the analyzer to a well
ventilated place. Do not use a tubing which is longer than 5 meters to
avoid accumulation of explosive gas inside the tubing.
It is a precondition that the instrument has been properly calibrated as described in chapter 4.
The sample volume has to be set at a value which is smaller than the volume which has been
filled into the sample bag.
Standard setting is 0.1 to 1 liter, depending on the expected concentration. For higher
concentrations the sample volume has to be set smaller, for lower concentrations the sample
volume should be higher, see table. To set the sample volume press F2 from the main menu (see
also chapter 3.4.1).
Concentration range
Sample Volume
Cycle Duration
0.001 µg/m3 – 0.5 µg/m³
10.0 liter
17.5 min
0.002 µg/m³ - 1 µg/m³
5.0 liter
10 min
0.01 µg/m³ - 5 µg/m³
1.0 liter
4 min
0.02 µg/m³ - 10 µg/m³
0.5 liter
3.3 min
0.05 µg/m³ - 25 µg/m³
0.2 liter
3 min
0.1 µg/m³ - 50 µg/m³
0.1 liter
3 min
> 50 µg/m³
0.01 liter
3 min
TABLE: SAMPLE VOLUME SETTINGS FOR DIFFERENT CONCENTRATION RANGES
According to the composition of the sample gas the built-in flow meter is automatically
calibrated before each measurement in order in order to achieve the correct sample volume.
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8. Version for Hg determination in natural gas and other hydrocarbon gases (Tedlar®
Bag Version)
page 86
8.3.2 Sampling of natural gas with the sample bag (Tedlar® bag)
The sample bag has to be completely empty before filling with sample gas. This may be done by
opening the valve of the bag, placing the bag onto a smooth and clean surface and running the
back of the hand over the bag until it is totally flat. Filling must be done by connecting the
sample bag with a source of positive pressure. Open the valve of the bag by turning its upper
portion counter-clockwise one revolution. It has under all circumstances to be avoided that air
can enter the sample bag because this could lead to formation of an explosive mixture in the
sample bag. For this reason do not use a pump for filling the bag. Do not inflate the bag too
much, avoid filling the bag more than 80 % of its maximum volume. Close the sample bag by
turning the upper portion of the valve clockwise until it is snug. Observe operating instructions
coming with the sample bags.
Transportation of the gas filled sample bag
Be careful when handling or carrying a filled bag as it contains flammable gas. It must be
avoided that air can enter the bag. Use smaller bags (for example 3 litre bags) whenever possible
to minimise risk. Keep the filled bag away from any ignition source.
8.3.3 Measuring the sample from the bag
After the instrument has been switched on and warmed up the user is asked to enter the sample
name. Use the numerical keys (0-9) to enter letters or numbers, use the left arrow button for
delete or the up arrow buttons to move the cursor right. Enter letters first and press ENT, then
enter numbers and press ENT if finished. With the F1 key the previous sample name can be
recalled.
A message on the display tells the operator to connect the sample bag and to open the sample bag
valve. Place the sample bag in front of the analyzer on the same table. Connect the sample bag to
the sample gas inlet nozzle of the UT-3000 analyzer using the Tygon tubing which has been
delivered with the instrument. The bag should be placed onto the same table where the analyzer
is set in order to avoid that it may disconnect from the analyzer thus causing a leak. Now open
the valve of the bag by turning its upper portion counter-clockwise one revolution.
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8. Version for Hg determination in natural gas and other hydrocarbon gases (Tedlar®
Bag Version)
page 87
Press F1-Start sampling to commence sample introduction into the analyzer. The instrument
will draw the preset volume of sample from the bag.
After the sampling has been completed the sample bag valve must be closed.
The end of sampling is indicated by a beeping sound and the message: Close sample bag valve
(clockwise); Remove Sample Bag. To close the sample bag turn the upper portion of the valve
clockwise until it is snug. The bag must be removed immediately.
Now analysis has to be started by pressing F1-Start heating.
After ca. one minute (depending on sample volume) the result is displayed on the screen.
After analysis the sample bag should completely be emptied observing above safety instructions.
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8. Version for Hg determination in natural gas and other hydrocarbon gases (Tedlar®
Bag Version)
page 88
FIGURE: TEDLAR BAG VALVE WITH CONNECTING
NOZZLE. OPEN AND CLOSE: HOLD THE
LOWER PART WITH NOZZLE WITH ONE
HAND AND TURN THE UPPER PART WITH
THE OTHER HAND.
FIGURE: ATTACHING THE CONNECTION TUBING TO
THE TEDLAR BAG NOZZLE
FIGURE: POSITION OF THE TEDLAR BAG DURING SAMPLING
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Bag Version)
page 89
FIGURE: FLOW OF SAMPLE FROM TEDLAR BAG THROUGH ANALYZER DURING SAMPLING STEP
FIGURE: FLOW OF CARRIER AIR AND DESORPTION OF MERCURY FROM GOLDTRAP HEATING/MEASURING STEP
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8. Version for Hg determination in natural gas and other hydrocarbon gases (Tedlar®
Bag Version)
page 90
8.4 Select Pump Type
The system can be equipped with two different pump types: a rotary vane pump or a membrane
pump. According to the installed pump “rotary vane” or “membrane” has to be selected by
pressing the F3-key in the service menu (3 2 1-code) on page 3.
Background information for service: if “membrane pump” has been selected as pump type, the
“heating flow regulate” function in service menu 222 is void.
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9. Communication with external data acquisition system (option)
page 91
9. Communication with external data acquisition system
(option)
The UT-3000 is prepared for connecting to an external data acquisition system. In this case the
data acquisition system will be the master and the UT-3000 the slave. The master can send
queries and commands. Results of measurements, calibration, and the set parameters can be read
out, a zero check and a span check will be carried out on demand.
9.1 Parameter settings for remotely triggered zero and span check
In order to prepare the system for a remotely triggered zero check and span check the parameters
shown in the table below have to be set.
Parameter
Value
Service Code 777
Service Code 999
Span Calibration Menu
Automatic Calibration Module ON
F2- Span Calibration activated
Time Interval for Span Check: 0
9.2 UT- 3000 external data access (version 04.05.2004)
Parameters, status and logger data can be transferred to an external master via the USB/RS232
port.
The UT-3000 software controls this port port regularly and in the case of an inquiry the data are
transmitted immediately.
The actual cycle of the UT-3000 is generally not interrupted during data handling and has
priority.
The actual measurement cycle will be terminated if a span check or zero check command is sent
to the UT-3000.
External transmission and data handling is only possible, when the UT-3000 is in the
automatic measuring mode. Otherwise the USB/RS232-port is not controlled.
RS232 parameter setting: 38 400 baud, 8 data bits, 1 stop bit, no parity
All data are ASCII-Characters, between the characters is a semicolon (;)
Telegram for inquiry and transfer (without logger data transfer):
<STX>;command type; command ;<CRC>;<ETX>
<STX>
;
command type
command
<CRC>
<ETX>
1 Byte
1 Byte
1 Byte
1 Byte
5 Byte
1 Byte
Start of text (02Hex)
separator semicolon
inquiry logger or status or parameter or system control
Checksum CRC16, max. 5 bytes
End of text (03Hex)
If the checksum is wrong, the UT-3000 answers:
9. Communication with external data acquisition system (option)
<STX>;E;13827;<ETX>
page 92
13827 = CRC16
E= error command
valid for every checksum-error
If the external master recognises a checksum-error, the master has to repeat the inquiry, not to send the error
command to the UT-3000.
If the UT-3000 does not recognise the command or an unknown command is send,
the UT-3000 answers:
<STX>;X;26122;<ETX>
Type of command: L:
S:
P:
C:
26122 = CRC16
logger, read, reset
status
inquiry of parameters
system control
Logger Command:
Inquiry: <STX>;L;S;<CRC>;<ETX>
external inquiry for logger status
Answer: <STX>;L;0;<CRC>;<ETX>
0 = Logger off
<STX>;L;1;A;B;C;<CRC>;<ETX>
Example:
1 = Logger on
A = start date, 6 bytes (year, month, day)
B = start time, 4 bytes (hour, minute)
C = number of logged data
5 bytes (max. 5000 data records)
data no 1 = first registered data
<STX>;L;S;23038;<ETX>
<STX>;L;0;43478;<ETX>
<STX>;L;1;040228;1530;123;23598;<ETX>
23038 = CRC16
43478 = CRC16
date = 28.02.04
time = 15:30
number of logged data = 123
Inquiry: <STX>;L;R;<CRC>;<ETX>
command to reset the logger
Answer: <STX>;L;R;<CRC>;<ETX>
same as the inquiry
Example:
<STX>;L;R;51711;<ETX>
Inquiry: <STX>;L;D;index;<CRC>;<ETX>
51711 = CRC16
index = number of data records, max. 4 bytes
Answer: <STX>;L;date;time;sample volume;concentration;<CRC>;<ETX>
one data record is transferred = logger data transfer
date = day, month, year (6 bytes)
time = hours, min.
(4 bytes)
sample volume (max. 5 bytes)
concentration (max. 6 bytes)
Example:
<STX>;L;D;23;20443;<ETX>
<STX>;L;280204;1630;2.0;2.3;58784;<ETX>
Mercury Instruments
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23 = no. of data record
date = 28.02.04
time = 16:30
sample volume = 2.0
concentration = 2.3
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9. Communication with external data acquisition system (option)
page 93
Status Command:
Inquiry: <STX>;S;<CRC>;<ETX>
S = system status
Answer: <STX>;S; letter 1;letter 2;<CRC>;<ETX>
Letter 1:
H = Heating
C = Calibration
S = Sampling
O = Cooling
Z = Zero
E = Evaluation
X = unknown status
Letter 2:
O = OK, no error message at the display
L = „Lamp“ at the display
P = „Pump“ at the display
T = „Temp“ at the display (temp of calibration cell)
Example:
<STX>;S;22029;<ETX>
<STX>;S;H;O;13041;<ETX>
22029 = CRC16
13041 = CRC16
H = Heating
O = no error
Parameters Command:
Inquiry: <STX>;P;letter;<CRC>;<ETX>
Letter:
P = parameters
M = actuel mode (answer: V = volume mode; T = time mode)
H = operating hours
L = lamp voltage
T = temperature of calibration cell (°C)
K = calibration-mode (answer: E = single cal.; A = auto cal.)
I = automatic calibration interval or calibration unit
D = date and time of the last calibration
C = data of the calibration curve (equation, const., correlation coefficient)
V = last concentration with date and time
Answer: <STX>;P;number;<CRC>;<ETX>
number: according value or
E, A or
V, T or
P= pg or
U= µl when manual calibration has been
chosen or date, time, calibration data
Example:
<STX>;P;M;27120;<ETX>
<STX>;P;V;39418;<ETX>
27120 = CRC16
V = volume mode
<STX>;P;H;14835;<ETX>
<STX>;P;32;57166;<ETX>
operating hours = 32
<STX>;P;L;63985;<ETX>
<STX>;P;3.2;29145;<ETX>
lamp voltage = 3.2 V
<STX>;P;T;63995;<ETX>
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9. Communication with external data acquisition system (option)
<STX>;P;19.2;43850;<ETX>
temp. of calibration cell = 19.2 °C
<STX>;P;K;51699;<ETX>
<STX>;P;E;43511;<ETX>
E = single (manual) calibration
<STX>;P;I;43506;<ETX>
<STX>;P;U;27130;<ETX>
<STX>;P;P;14841;<ETX>
<STX>;P;4;63955;<ETX>
<STX>;P;1130;44505;<ETX>
page 94
U = µl (when manual calibration has been chosen)
P = pg (when manual calibration has been chosen)
calibration. interval = 4 hours (when Auto. Calibration has
been chosen)
start time of calibration. = 11:30 (when auto calibration. Has
been chosen)
<STX>;P;D;14838;<ETX>
<STX>;P;280204;1250;56724;<ETX>
date = 28.02.04
time = 12:50 ( of last calibration)
<STX>;P;C;2548;<ETX>
<STX>;P;1.23456789;2.34567;3.45678;10851;<ETX>
<STX>;P;V;39418;<ETX>
<STX>;P;1.2;280204;1040;708;<ETX>
calibr. Data (equation; const;
correlation coefficient)
last concentration = 1.2, date = 28.02.04,
time= 10:40
System control command:
Inquiry:
<STX>;C;S;<CRC>;<ETX>
C = control
S = start span-check
Answer:
<STX>;C;S;<CRC>;<ETX>
span-check will be started
Example:
<STX>;C;S;19965;<ETX>
<STX>;C;S;19965;<ETX>
19965 = CRC16
span-check will be started
Inquiry:
<STX>;C;S;V;<CRC>;<ETX>
C = control
S = span-check
V = value (= read span-check value)
Answer:
<STX>;C;V;conc;<CRC>;<ETX>
V = value
conc = meas. concentration in ng/m³
Example:
<STX>;C;S;V;55038;<ETX>
<STX>;C;V;1.3;14490;<ETX>
55038 = CRC16
14490 = CRC16
1.3 = concentration
Inquiry:
<STX>;C;Z;<CRC>;<ETX>
C = control
Z = start zero-check (sample volume= 1litre)
Answer:
<STX>;C;Z;<CRC>;<ETX>
zero-check will be started
Example:
<STX>;C;Z;7675;<ETX>
<STX>;C;Z;7675;<ETX>
7675 = CRC16
zero-check will be started
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9. Communication with external data acquisition system (option)
Inquiry:
<STX>;C;Z;V;<CRC>;<ETX>
C = control
Z = zero-check
V = value (= read zero-check value)
Answer:
<STX>;C;V;conc;<CRC>;<ETX>
V = value
conc = meas. Concentration in ng/m³
Example:
<STX>;C;Z;V;19197;<ETX>
<STX>;C;V;1.1;22683;<ETX>
19197 = CRC16
22683 = CRC16
1.1 = concentration
Inquiry:
<STX>;C;C;<CRC>;<ETX>
C = control
C = continue sampling
Answer:
<STX>;C;C;<CRC>;<ETX>
continue sampling
Example:
<STX>;C;C;36336;<ETX>
<STX>;C;C;36336;<ETX>
36336 = CRC16
continue sampling
page 95
For span check and zero check the „rising time“ and the „falling time“ have to be considered. The „rising time“ and
the „falling time“ according to the set sample volume of the UT3000 are shown in the table below.
In the following the maximum times are shown:
ZERO:
Sample volume:
0.1 l
1l
2l
3l
10 l
rising time
425 sec.
275 sec.
275 sec.
275 sec.
275 sec
falling time
331 sec.
262 sec.
352 sec.
442 sec.
532 sec
first sample reading after zero check
161 sec.
242 sec.
332 sec.
422 sec.
1052 sec.
SPAN:
Sample volume:
0.1 l
1l
2l
3l
10 l
rising time
1672 sec.
1522 sec.
1522 sec.
1522 sec.
1522 sec.
falling time
331 sec
262 sec.
352 sec.
442 sec.
532 sec.
first sample reading after span check
935 sec.
1016 sec.
1106 sec.
1196 sec.
1826 sec.
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page 96
INDEX
accessories 55
Applications 7
Auto Range 19
automatic calibration 43
Automatic Calibration Unit
connection 14
bag sampling 84
calibration
automatic 43
manually 32
Calibration Data
Set 51
connection
Automatic Calibration Unit 14
data output 11
electrical 11
RS232 11
Data Logger
send data to PC (Hg-Transfer) 26
Declaration of Conformity 97
desiccant cartridge
replacement 69
Device Data 50
dryer tube
replacement 69
EC-Declaration 97
error messages 64
filter
replacement of 68
filter cartridges
replacement 68
flammable gas
safety instructions 85
flammable gases 84
flow
show 50
Flow
adjustment 75, 76
fuses 70
gas flow
schematic 81
GoldTrap
Cleaning 71
replacement 71
Heating Flow
Adjustment 75
installation 10
main menu 15
maintenance 55
measuring
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start 19
Measuring principle 9
membrane filter
replacement 68
natural gas 80
sampling system 80
parts list
Automatic Calib Unit 62
UT-3000 58
power supply 11
principle
of measurement 9
print function 16
Purge Repetitions 50
Repeat Zero 54
replacement
filter cartridges 68
Safety 2
Safety instructions
flammable gas 85
sample bag 84
sample volume
set 17
Sampling Flow
Adjustment 75
Service Codes 54
service menu 49
set
date and time 50
Set
Calibration Data 51
cycle duration 18
sample volume 17
Settings
basic 17
show flow 50
spare parts 55
specifications 78
Static Calibration Set 36
storage 79
syringe positioning 51
Tedlar bag 84, 90
transport 79
Trap Counter 52
tubing
ID numbers 59
turning on
UT-3000 15
unpacking 10
Warnings 2
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page 97
APPENDIX
EC-Declaration of Conformity
The Company:
Declares that the product:
Intended purpose:
Mercury Instruments GmbH
Liebigstrasse 5
D-85757 Karlsfeld
Germany
UT-3000 Mercury Ultratracer
Automatic measurement of mercury at trace
concentration levels in air and other gases
conforms with the basic requirements of the relevant EC directives.
A conformity assessment method as provided in the directives has been executed.
For verification in accordance with the directives 89/336/EEC, 73/23/EEC and the other relevant
provisions the following harmonized standards were applied:
EN 61326 :1997+A1 :1998+A2 :2001
EN 55014-1 :2000+A1 :2001
(Tests: EN CISPR 15-1 :1993; CISPR 16-2 :1996 ; EN 61 000-4-6:1996 / ENV 50
204:1995,EN 61000-3-2:2000+ Corrigendum 1:2001; EN 61000-3-3:1995+
Corrigendum: 997+A1:2001)
EN 61326:1997+A1:1998+A2:2001
(Tests : EN 61000-4-2 :1995+A1 :2001; EN 61000-4-3 :2002 ; EN 61000-44 :1995+A1 :2001+A2 :2002; EN 61000-4-5 :1995+A1 :2001; EN61000-46 :1996+A1 :2001; EN 61000-4-11 :1994+A1 :2001)
The tests regarding above standards have been conducted by Intertek Deutschland GmbH,
Kaufbeuren/Germany (Test Report Nr. 04KFE003157-01). The test documents are available for
inspection.
This declaration is submitted by:
Karlsfeld, 18nd August, 2008
Mercury Instruments
Analytical Technologies
Dr. Alfred Sauerer
UT-3000-E_V2.11.docx
31.07.12
page 98
(CEO)
Mercury Instruments
Analytical Technologies
UT-3000-E_V2.11.docx
31.07.12
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