V. 1.0 User Manual Microwave Digestion System with Built

Microwave Digestion System with
Built-in, Non-Contact
Temperature and Pressure Measurement
V. 1.0
User Manual
Copyright © 2004 Berghof Products + Instruments GmbH, All Rights Reserved
Copying, duplication or republication is prohibited without the express prior written permission of Berghof Products + Instruments GmbH
Liability Disclaimer
The contents of this publication have been checked for compliance with the described hardware and
software. Nonetheless, differences cannot be ruled out so that we can assume no liability for any differences which may arise. The information in this publication is reviewed regularly and any revisions that
may be required are included in subsequent versions. We welcome all comments regarding improvements to our products and publications.
We reserve the right to make technical changes.
Trademarks
speedwave and Berghof are registered and unregistered trademarks and service marks of Berghof
Products + Instruments GmbH.
Notes regarding this Handbook
Contents:
This handbook describes the microwave pressure digestion system speedwave four. It contains product specific information, current as of the date of publication of this handbook. This technical documentation is a reference and instructional manual. Each chapter is complete in and of itself.
This handbook guides the user in the safe and proper use of speedwave four system. Familiarity with
the relevant chapters of this handbook is required for safe and intended use of the equipment
Read this instructional manual carefully prior to operating the equipment. After unpacking, carefully check the equipment for mechanical damage and missing parts. Should you find any damage incurred during shipment, contact the manufacturer immediately and do not operate the equipment.
This instructional manual does not include repair instructions. Should repairs be required, please contact your dealer or Berghof Products + Instruments GmbH.
Order no.:
SW-4_53-0170-93-00-00-002
You can contact us at:
Germany:
Berghof Products + Instruments GmbH
Harretstr. 1
72800 Eningen
Telephone: +49 7121 / 894-202
Fax:
+49 7121 / 894-300
e-mail: [email protected]
www.Berghof-instruments.de
Berghof Products + Instruments GmbH are certified in accordance with DIN EN ISO 9001:2000.
Berghof Products + Instruments
speedwave four
Contents
1.
GENERAL NOTES ..................................................................................................... 5
1.1.
Danger Categories and Signal Words..................................................................................................5
1.2.
Qualified Users .......................................................................................................................................5
1.3.
Proper Use ..............................................................................................................................................6
1.4.
General Safety Information ...................................................................................................................7
1.5.
Safety and Emissions ............................................................................................................................9
1.6.
Informations on Disposal ....................................................................................................................10
1.7.
Warranty / Limitation of Warranty ......................................................................................................11
2.
DEVICE DESCRIPTION ........................................................................................... 13
2.1.
Basic Unit ..............................................................................................................................................13
2.2.
Temperature Monitoring ......................................................................................................................15
2.3.
Pressure Monitoring (Option) .............................................................................................................15
2.4.
Pressure Vessels and Rotor Systems................................................................................................16
2.5.
Technical Specifications .....................................................................................................................19
2.6.
Safety Equipment .................................................................................................................................21
3.
SETUP AND COMMISSIONING............................................................................... 23
3.1.
Standard Delivery.................................................................................................................................23
3.2.
Standard Delivery Start-up Packages ................................................................................................26
3.3.
Setup and Commissioning ..................................................................................................................27
3.3.1. Ambient Conditions....................................................................................................................27
3.3.2. Unpacking / Inspection...............................................................................................................27
3.3.3. Installation ..................................................................................................................................28
4.
HARDWARE AND SOFTWARE OPERATION ........................................................ 33
4.1.
Method Preparation..............................................................................................................................33
4.1.1. Information Regarding Digestion ...............................................................................................33
4.1.2. Controller....................................................................................................................................34
4.1.3. Modifying Application .................................................................................................................35
4.1.4. Developing a New Application ...................................................................................................38
4.2.
Performing a Digestion Procedure.....................................................................................................39
4.3.
Sample Loading....................................................................................................................................44
4.3.1. Handling the DAP-40+, DAP-30+, DAP-60+, and DAP-100+ Pressure Vessels ......................44
4.3.2. Handling DAQ-20H Pressure Vessels .......................................................................................47
4.3.3. Handling DAC-17 Pressure Vessels ..........................................................................................49
4.3.4. Handling DAK-100/4 Pressure Vessels .....................................................................................51
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4.4.
BERGHOF Products + Instruments
Sample Removal...................................................................................................................................54
4.4.1. Removing and Opening DAP-40+, DAP-30+, DAP-60+ and DAP-100+ Pressure Vessels .....55
4.4.2. Removing and Opening DAK-100/4 Pressure Vessels .............................................................56
4.5.
Data Reprocessing ...............................................................................................................................57
4.6.
Data backup / data export using USB ................................................................................................59
5.
OPTIONS ..................................................................................................................61
5.1.
Evaporating Unit ...................................................................................................................................61
5.1.1. Standard Delivery.......................................................................................................................62
5.1.2. Installation and Commissioning .................................................................................................62
5.1.3. Operation....................................................................................................................................63
6.
MAINTENANCE, TROUBLESHOOTING AND SERVICE ........................................65
6.1.
Cleaning.................................................................................................................................................65
6.2.
Maintenance..........................................................................................................................................68
6.3.
Alignment of Pressure Measurement.................................................................................................69
6.4.
Output power measurement................................................................................................................70
6.5.
Troubleshooting ...................................................................................................................................72
6.6.
Fuse Replacement................................................................................................................................73
6.7.
Repairs / Customer Service.................................................................................................................74
6.8.
Nameplate .............................................................................................................................................74
7.
APPENDIX ................................................................................................................75
7.1.
Tips and Tricks .....................................................................................................................................75
7.2.
Applications ..........................................................................................................................................77
7.2.1. Positioning of Vessels in the Turntable......................................................................................86
7.3.
Conformity Declaration........................................................................................................................88
7.4.
Conversion Table .................................................................................................................................89
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1.
General Notes
General Notes
Please read this instruction manual carefully before operating your high pressure
digestion system. Failure to follow these instructions could result in damage to the
equipment as well as personal injury.
Safety instructions are printed in boldface throughout and shown as illustrated in
section 'Danger Categories and Signal Words'. These safety notes must be heeded
in all cases!
1.1.
Danger Categories and Signal Words
The signal words described below are used in connection with warnings throughout
this manual. For your own safety and to avoid property damage, you must strictly
heed these warnings!
The safety signals are printed in boldface or are otherwise marked throughout this
manual and have the following meanings:
DANGER !
Means that failure to follow the safety instructions is likely to cause severe personal injury, death or severe property damage.
Warning !
Means that failure to follow the safety instructions may cause severe personal injury, death or severe property damage.
Caution
Means that failure to follow the safety instructions may cause personal injury or
some property damage.
Note:
This symbol indicates that this is important information regarding the product or
refers to a part of the manual, which requires particular emphasis.
1.2.
Qualified Users
Only Qualified Users should operate this equipment. Qualified Users with respect
to this manual are relevantly schooled and trained specialists with a basic knowledge of chemistry. They should be trained in the safe handling of chemicals.
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General Notes
1.3.
Berghof Products + Instruments
Proper Use
DANGER !
Explosion hazard!
The unit is not designed for extraction and metabolization procedures employing
organic solvents.
Warning !
Observe all operating instructions!
Since sample composition is generally not precisely defined, a certain residual risk
exists when performing pressure digestion processes. Careful working practices
and conscious compliance with safety regulations can only minimize this risk, not
totally eliminate it. Due to different degrees of mixing, even identical samples can
exhibit totally different behaviors during the course of the reaction!
Please strictly comply with the operating instructions, particularly when handling
the pressure vessels, that is, when removing and opening the vessels. Incorrect
handling of the hot, pressurized vessels can result in injuries from escaping acid
vapors!
The speedwave microwave digestion system has been designed to perform
chemical digestion procedures under extreme pressure and temperature conditions
in chemical laboratories. Digestion is understood to mean the decomposition of a
solid material by means of a suitable digestion reagent at increased temperature in
a vessel that is permeable with regard to microwaves. The digestion solutions are
directly heated through the absorption of the microwave radiation by the polar digestion reagent, which generally also contains ionic components.
Digestion reagents used include nitric acid (65%), hydrochloric acid, hydrofluoric
acid, phosphoric acid, and sulfuric acid, as well as mixtures of these acids. The
maximum initial weight for organic compounds depends on the digestion vessel being used and the sample’s carbon content, must always be observed. The use of
organic solvents is strictly prohibited in microwaves since the spontaneous combustion of any solvent vapors that escape into the oven chamber cannot be precluded.
Heating in the pressure vessel results in digestion temperatures in excess of 200
°C (392°F). The speedwave has been specially developed for sample preparation
for AAS and ICP spectroscopy procedures. Very temperature spikes >280 °C
(>536°F) such as can occasionally occur during the course of exothermic reactions
can result in irreversible damage to the Teflon vessels. Since such scorching cannot always be avoided, even with optimum microwave power regulation, damage of
this kind is excluded from the warranty! When quartz glass inserts are employed,
the greatest care must be taken when handling the glass as even the slightest
amount of damage to the surface can greatly diminish surface strength. For this
reason, glass components are excluded from the warranty!
Adapters for evaporating and concentrating digestion solutions are optionally available for all vessel types.
Qualified handling and, possibly, proper transport, storage, set-up, and use, as well
as conscientious maintenance are all prerequisites for the trouble-free and safe
operation of the speedwave microwave digestion system.
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General Notes
The system may only be used within the context of data and applications specified
in this documentation and the associated user manuals.
The digestion system may only be used:
Properly;
In a technically flawless condition;
Without unauthorized alterations or modifications;
By qualified users.
Please also observe all regulations published by professional/trade associations,
the TÜV, VDE regulations, or corresponding national regulations.
1.4.
General Safety Information
Performing microwave digestion procedures involves taking into account various
safety precautions which go beyond those for general laboratory practices. The following general safety information should therefore be read carefully prior to using
the system, and should be observed at all times.
The following information must be complied with when working with the associated
digestion vessels!
We can assume no liability for damages resulting from improper handling of a failure to comply with this information.
Warning !
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work which may
involve contact with chemicals, that is, when working with acids, pressure vessels,
during cleaning, etc.!
DANGER !
Explosion hazard!
Do not use perchloric acid.
No organic solvents (alcohols, hydrocarbons, etc.) may be placed in the pressure
vessels or the microwave.
Highly reactive substances which spontaneously react at higher temperatures or in
the presence of oxidizing agents or which may be nitrated and are potentially explosive may not be digested in the microwave. Examples of such substances include: explosives (TNT, etc.), perchlorates, ether, pyrophoric substances, etc.
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General Notes
DANGER !
Berghof Products + Instruments
Pressure vessels!
Use only digestion vessels and spare parts authorized by Berghof Products + Instruments GmbH for use with the speedwave. These can be obtained either from
your local dealer or directly from Berghof Products + Instruments GmbH (Refer to
the “Repairs / Customer Service” section for contact addresses).
Always wear safety glasses/goggles and protective gloves when working with the
pressure vessels!
Note any changes in the appearance of the pressure vessel which could indicate
possible material fatigue, e.g., deformation of the vessel, difficulty screwing on
lids, etc. even when the vessel is cold and not under pressure. All such vessels
should be immediately returned to Berghof Products + Instruments GmbH for inspection.
Never attempt to use force to open the vessels. Never use tools to open the vessels!
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Hot gases and vapors may be released from the digestion vessel when it is
opened! Always make sure the vent opening on pressure vessels faces away from
both yourself and other individuals!!
Only open the digestion vessel under a fume hood or other exhaust system. Particular care is required when working with hydrofluoric acid (HF). Observe all relevant data sheets and safety instructions!
Never use more than one rupture disc per vessel!
Note:
Renew the vessels after around 10,000 digestions to maintain reliable operating
conditions and to prevent negative influences on your analysis results (e.g. memory effects etc.).
Berghof Products + Instruments GmbH includes its digestion vessels in the warranty coverage. Nevertheless all of the vessels are subject to a certain aging
process, which also depends on the type and frequency of the application. Typically the service life is 10,000 digestion processes or at least 3 years.
Warning !
The unit employs high voltage and generates microwave radiation!
The speedwave four must always be carefully connected to a grounded conductor. Provided the wall outlet used is equipped with a ground connection, the supplied power cord will ensure proper connection. If it is necessary to use an extension cord to connect the system to the power supply, only a three-wire cord with a
ground connection may be employed.
The unit should not be set up near any devices which are sensitive to electromagnetic radiation. If necessary, a warning sign or label indicating “Caution, Microwave Emissions” should be applied or attached to the unit. Should there be any
suspicion or indication of increased levels of microwave radiation, please immediately inform the Service Department at Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for the contact address).
Repair and servicing of the equipment may only be performed by trained
personnel.
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Berghof Products + Instruments
1.5.
General Notes
Safety and Emissions
In the following situations, the unit must be disconnected from the mains
power supply and be locked out to prevent accidental use:
If the unit evidences visible signs of damage;
If unit parts or components are found to be loose;
If the unit fails to operate;
If the unit is to be stored for extended periods of time under unfavorable
conditions (e.g., outdoors, in very moist or humid environments).
The housing cover may only be removed by authorized trained personnel!
The unit must be disconnected from the mains power supply.
Caution
Safety information on the unit
GEFAHR!
DANGER!
DANGER!
¡PELIGRO!
Vor Öffnen des Gerätes Netzstecker ziehen.
Avant d´ouvrir l´appareil retirez la fichemâle.
Before opening disconnect mains.
Retirar el enchufe de red antes de abrir el equipo.
GEFAHR!
DANGER!
DANGER!
¡PELIGRO!
Hochspannung
Haute tension
High voltage
Alta tensión
VORSICHT!
ATTENTION!
CAUTION!
¡ATENCIÓN!
Nur Netzkabel mit Erdleiter verwenden.
N'utiliser que des câbles de secteur reliés à la terre.
Use only cable with plug and protectiveearth.
Utilizar exclusivamente un cable de red con conector de puesta a tierra.
VORSICHT!
ATTENTION!
Gefäß steht unter Druck – erst nach Abkühlung vorsichtig öffnen.
Le récipient se trouvant sous pression, ne l'ouvrir avec précaution qu'après qu'il ait refroidi.
Vessel under pressure – open carefully after cooling.
Recipiente bajo presión – Abrir cuidadosamente de spués de enfriar.
HIGH VOLTAGE
HIGH VOLTAGE
HIGH VOLTAGE
CAUTION!
¡ATENCIÓN!
EXPLOSIVE
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General Notes
Berghof Products + Instruments
European Community
This device has been designed and tested in accordance with the following IEC
publications:
IEC 61010-1:
IEC 60335-2-90:
CE designation
Safety requirements for electrical equipment
for measurement, control, and laboratory use.
Particular requirements for commercial
microwave ovens.
Products from Berghof Products + Instruments GmbH comply with the guidelines of
the VDE and the European Standards. The conformity tests performed by Berghof
Products + Instruments GmbH comply with the currently required standards for
electrical safety as well as the safety of microwave ovens. All limit values with respect to interference emission and interference protection have been maintained.
This device operates within the limit values set forth in the following standards:
Conformity
declaration
1.6.
EN 335-25 (microwave devices);
DIN EN 61010-1 (safety)
DIN EN 61326-1 (interference emissions);
DIN EN 61326-2 (interference resistance).
Refer to the Appendix
Informations on Disposal
European Union
Electrical and electronic products should not be mixed with general household
waste. Berghof Products + Intruments GmbH accepts its electrical and electronic
instruments from on a free of charge basis for proper treatment, recovery and recycling from their business users. If you wish to discard electrical and electronic
products, please contact your local dealer or Berghof Products + Intruments GmbH
([email protected]). They will provide further information.
Disposing of this product correctly will help to protect our environment..
Countries outside the European Union
This regulation is only valid in the European Union
Note:
Berghof-Products are not used in private households.
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Berghof Products + Instruments
1.7.
General Notes
Warranty / Limitation of Warranty
Limited Warranty
Each product manufactured by Berghof Products + Instruments GmbH is warranted to conform to Berghof Products + Instruments GmbH’s applicable specifications on the date on shipment. The warranty period is twelve (12) months after the
date of delivery, unless another period is specified. The warranty does not extend
to damages due to improper installation, improper maintenance, abuse, accident,
negligence, alteration, misuse, ordinary wear and tear, or the like. Claims for replacement of parts caused by ordinary wear and tear are excluded, as are claims
for replacement of parts meant to be expended during the operation of the equipment.
Berghof Products + Instruments GmbH also includes its digestion vessels under
this warranty.
However, high temperatures >280 °C (>536°F), such as may briefly occur when
exothermic reactions take place can result in irreversible damage to the TFM vessels. Since such scorching cannot always be avoided even by optimal microwave
power regulation, the resulting damages are excluded from the warranty! Care
must also be taken when handling quartz glass or ceramic inserts as their reliability
can be seriously impaired by even minor damage to their surfaces. Therefore,
glass and ceramic components are also excluded from this warranty!
Remedies
Under the limited warranty, Berghof Products + Instruments GmbH repairs or replaces any products which Berghof Products + Instruments GmbH determines to
be defective and covered by this limited warranty. This is the sole and exclusive
remedy. If Berghof Products + Instruments GmbH determines that repair or replacement fails its essential purpose, the purchaser will, at its option, be entitled to
a refund of the purchase price for the products in question or a credit therefore.
All warranty claims must be accompanied by a description of the claim, which description must be attached to the equipment claimed to be defective. Claim descriptions must include the claimants name, address, department (if applicable)
and telephone number.
The equipment should be returned in its original packaging, to the extent possible.
We regret that Berghof Products + Instruments GmbH cannot be held responsible
for damage caused during shipping due to improper packaging.
LIMITATION OF
WARRANTY
EXCEPT AS EXPRESSLY SET FORTH ABOVE, THERE ARE NO OTHER
WARRANTIES HEREUNDER, WHETHER EXPRESSED OR IMPLIED, ARISING
BY OPERATION OF LAW OR OTHERWISE, INCLUDING WITHOUT
LIMITATION, THE WARRANTIES OF MERCHANTABILITY, FITNESS FOR A
PARTICULAR PURPOSE AND ANY WARRANTIES ARISING UNDER COURSE
OF PERFORMANCE, COURSE OF DEALING OR USAGE OF TRADE.
UNDER NO CIRCUMSTANCES WILL BERGHOF PRODUCTS + INSTRUMENTS
GMBH BE LIABLE FOR ANY CONSEQUENTIAL, EXEMPLARY, INCIDENTAL,
INDIRECT OR SPECIAL DAMAGES, OR LOST PROFITS, EXPENSES OR
LOSES ARISING OUT OF OR RELATED TO THE SALE OR USE OF ANY OF
ITS PRODUCTS REGARDLESS OF WHETHER THE LIABILITY RESULTED
FROM ANY GENERAL OR PARTICULAR REQUIREMENT OR NEED WHICH
BERGHOF PRODUCTS + INSTRUMENTS GMBH KNEW OR SHOULD HAVE
KNOWN OF.
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General Notes
Berghof Products + Instruments
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2.
Device Description
2.1.
Basic Unit
Device Description
The speedwave four microwave system is designed for pressure digestion
at temperatures up to 230° C (446° F) in continuous use (short term 300 °C /
572 °F) and, depending on the type of vessels employed, pressures up to a max.
of 100 bar (1450 psi).
This is a top loading microwave made of 1.4301 (SS 304) stainless steel and
equipped with a swiveling safety lid, electromechanical locking mechanism and a
circular sample chamber for uniform microwave distribution. The oven has a highly
chemicals resistant PFA coating protecting it from corrosion. Three overtemperature switches and three micro-switches guarantee the necessary operating
safety. The chamber is permanently ventilated by a special fan.
An DIRC thermometer that permits the temperature of the vessel contents to be
quickly determined and regulated is integrated in the microwave oven. The measurement physically determines the temperature radiation emitted by the vessel
contents, that is, the digestion solution. Radiation components emitted by the vessel walls and, in particular, the exterior of the vessel, are completely filtered out.
Optionally the system can be equipped with a contact-free pressure monitoring
system for either individual or for all vessels. This records the internal vessel pressure. If a vessel is approaching its maximum pressure, the system automatically
switches to a pressure-controlled mode for the microwave output.
An unpulsed regulated 2.45 GHz magnetron provides up to 1,450 W of microwave
power. The microwave is controlled by a separate controller with touch-screen. After entering the desired temperature profile, the microwave output is infinitely varied in accordance with the measured sample temperatures. The target and actual
temperatures of all samples are displayed on the screen in real time and saved to
memory.
Connections
As the following figures illustrate, the speedwave four is equipped with various
connection options.
Microwave oven
Swiveling lid with vent connection
Electr. connections
Separate control unit
Vent connection oven
Magnetron cooling
Electr. Cooling
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Device Description
Controller
Berghof Products + Instruments
A separate control unit with power PC 5200, 5.7” touch screen and graphics
display is used to control the microwave oven. The english, german or french
language software is preinstalled at the factory.
Main window
Key functions
Button:
Function
Application
Function for selecting or creating an application.
The active application is displayed (in the illustration
above “Calcite; Dolomite”).
Data
Function for viewing stored digestion data.
The most recently used file is displayed. (in the illustration above “data_file0”)
Open
Unlock door (only possible if magnetron is off)
Setup
Setup menu Access with 4-digit access code only.
(factory setting 4321)
Start
Start the microwave
Service
Service menu: Access for authorized service
technicians only
The version number of the control software is displayed in the header of the main
menu and in the footer the version number of the firmware of the speedwave four
and the status of the swivel lid.
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Connections
(basic instrument)
Connections
(control unit)
The mains power switch is located on the right-hand side of
the unit.
The switch is illuminated while
it is on.
Next to this are the fuses and
the RS-232 port for connecting with separate control unit.
The mains power switch is located on the back of the unit.
The switch is illuminated while
it is on.
Next to this are the fuses and
the ports for connecting wikth
basic instrument and ethernet.
Device Description
RS-232 port
fuses
power switch
RS-232 port
Ethernet-port
fuses
power switch
2.2.
Temperature Monitoring
The speedwave four is equipped with a temperature monitoring system. This system determines the temperature inside the pressure vessels by measuring the direct infrared radiation emitted by the sample. This allows the temperatures of all
samples to be determined. This information is forwarded to the power control module which uses the highest measured temperature to regulate the oven power.
Continuous adjustment of the magnetron output allows the temperature to be regulated on the basis of all vessel contents.
For measurement instrumentation reasons, only temperatures above 50° C (122°F)
can be displayed. Temperatures below 50° C (122°F) are indicated on
the display by “low”.
2.3.
Pressure Monitoring (Option)
Optionally, the speedwave four can be equipped with a pressure monitoring system. To achieve this, the pressure in the vessels is determined by using polarized
light to measure any change in the photoelastic behavior of a glass ring in the vessel lid. This allows the internal pressures of all or of individual vessels to be detected. This information is conveyed to the output control module, which can use
the highest measured pressure to regulate the output. By continuously adjusting
the magnetron output pressure regulation referenced to individual vessels can be
achieved while preventing other over-pressure safety devices (rupture discs) from
being activated.
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Device Description
2.4.
Berghof Products + Instruments
Pressure Vessels and Rotor Systems
All Berghof pressure vessels are manually operated. A rupture disc placed in the
vessel lid limits the interior pressure of all vessel types to the maximum permissible
value for the individual type. For all vessels except DAP-40+ acid vapors that escape when the rupture disc activates are guided to a collection system integrated
in the rotor. Thereby the vapors are vented or suctioned off through the PFA tube
connected to the swiveling lid.
DAP-40+
DAP-40+ vessels are made entirely of TFM. Aside from chemical resistance to all
mineral acids including hydrofluoric acid, this ensures a high level of mechanical
strength, even at high digestion temperatures.
- 24 pressure vessels made of TFM
- Rotor
DAP-30+/-60+/100+
DAP-30+, DAP-60+ and DAP-100+ vessels are made entirely of TFM. Aside from
chemical resistance to all mineral acids including hydrofluoric acid, this ensures a
high level of mechanical strength, even at high digestion temperatures.
- 12 pressure vessels made of TFM
- Rotor
- Gas collection system
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DAK-100/4
Device Description
TM
DAK-100/4 vessels are made of a TFM -pressure vessel with cap.
TM
Beside this, this vessel consists of a ceramic pressure jacket and a TFM -insert.
TM
- 8 pressure vessels made of TFM
- Rotor
- Gas collection system
DAQ-20H
For digestion of small sample weights quartz inserts may be placed into pressure
vessels DAP-60+ or DAP-100+.
- Quartz vessel
- TFM-cap
DAC-17
The DAC-17 are special high pressure inserts intended for digestion of small and
hard-to-digest samples.
- TFM-insert
- Ceramic pressure jacket
- DAP-100+ vessel
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Device Description
MT-System
Berghof Products + Instruments
For the digestion of small sample quantities or several samples at the same time in
a single DAP-100+ or DAK-100/4 pressure vessel it is possible to use these special
vessels.
- PFA-Insert
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2.5.
Device Description
Technical Specifications
Technical specifications for the speedwave four
Microwave oven
Power supply
230 V
Frequency
50 / 60 Hz
Current
15 A
Power consumption
2000 W
Fuses
2 x 15 AT, two-phase
Magnetron frequency
2450 MHz
Microwave power
1,450 W
Exterior dimensions (W x D x H)
640 x 570 x 430 mm
(25.2 x 22.4 x 16.9 inches)
Interior dimensions (ID)
360 mm
(14.2 inches)
Weight (approx.)
65 kg (143 lb) without vessels
Noise level
< 60 dB
DIRC temperature range
50° C – 300° C (122 - 572°F)
0 – 150 bar (2180 psi)
Display 0 - 100 bar (1450psi)
Pressure sensor range
Controls
Power PC 5200
5,7“ touch-screen, monochrom
Program memory
200 programs, 25 preprogrammed
Data file memory
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min. 500 data files
Display
320 x 240 pixel
Interface
RS-232, Ethernet, USB
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Device Description
Berghof Products + Instruments
Pressure vessels
®
Material
TFM , PEEK, quartz, aluminum oxide
Volume
Max.
pressure
Max.
temperature
max. sample weight
(organic)
Min. fill
volume
(acid)
< 300 mg
> 5ml
DAP-40+
40ml
40 bar
(580psi)
230° C
(446°F)
DAP-30+
30 ml
80 bar
(1160psi)
230° C
(446°F)
< 300 mg
> 5ml
DAP-60+
60 ml
#
40 bar
(580psi)
230° C
(446°F)
< 500 mg
> 5ml
DAP-100+
100 ml
40 bar *
(580psi)
230° C
(446°F)
< 500 mg
> 5ml
100 ml
100 bar
(1450psi)
230° C
(446°F)
< 1000 mg
> 5ml
DAQ-20
20 ml
100 bar
(1450psi)
230° C
(446°F)
< 300 mg
> 5ml
DAC-17
17 ml
130 bar
(1885psi)
300° C
(572°F)
< 200 mg
> 5ml
DAK-100/4
*25bar above 200°C
#
50bar with special rupture discs (not enclosed in standard delivery)
Short - term (max. 15 min.) heating to 260° C (500° F) is possible with all vessels.
Overpressure protection: Rupture disc for all pressure vessels
20
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Berghof Products + Instruments
2.6.
Device Description
Safety Equipment
Swiveling lid
Warning !
The system is equipped with a solid, PFA-coated, stainless steel housing with a
swiveling safety lid for maximum user safety. The electronic lid-locking mechanism
can only be opened by means of the software control. In addition, 3 interlock
switches are installed which shut the microwave off if the lid is opened by force
during microwave operation.
The unit emits microwave radiation!
Never operate the microwave oven if the swiveling lid or the related lock mechanism have been damaged. Contact your local, authorized dealer or Berghof
Products + Instruments GmbH to obtain the required service (Refer to the
“Repairs / Customer Service” section for contact addresses).
Rupture discs
Warning !
All vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case of excessive
vessel pressure. In some cases, such a spontaneous pressure release may occur
after the vessel has been removed from the microwave oven.
Rupture discs as overpressure protection!
Use only original Berghof rupture discs and protective cover sheets. These can
be obtained from your local, authorized dealer or Berghof Products + Instruments
GmbH (Refer to the “Repairs / Customer Service” section for contact addresses).
Never use more than one rupture disc per vessel!
Gas exhaust
Warning !
All pressure vessels are equipped with a sealed connection to a gas collection system which, in turn, must be connected to an exhaust system via a PFA vent tube.
The PFA tube is connected to the screw-on connection located in the center of the
top of the microwave. Any hot acid vapors released when the rupture disc activates
are safely removed through this PFA vent tube.
Hot acid vapors may be released.
The supplied vent tubes must therefore always be properly connected and attached to an exhaust system.
Make sure the PFA tube is securely attached so that it cannot pop off its connection fitting in case of a percussive pressure burst as occurs when a rupture disc
activates.
Temperature control
The system is equipped with a temperature control of all sample temperatures as
described in the section, “Temperature Monitoring”. An emergency shut-off occurs
in case of a rupture disc break.
Pressure control
Optionally, the system can be equipped with a pressure monitoring system for all
internal vessel pressures as described in the ‘Pressure Control’ section.
Over-temperature
protection
For safety reasons, the microwave automatically switches itself off in case the
magnetron, the microwave oven, or the high voltage transformer overheats.
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Device Description
Berghof Products + Instruments
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3.
Setup and Commissioning
3.1.
Standard Delivery
Setup and Commissioning
speedwave four microwave oven
with built-in DIRC temperature sensor, OPC optical pressure control
and separate control unit (part no. 5304000)
1x speedwave four control unit (part no. 5304800)
1x power cord (part no. 50003117)
1x power cord (part no. 500003107)
1x RS-232 cable (part no. 5303195)
1x PE-corrugated hose ∅65mm; 2,5m (part no. 5304044)
1x speedwave four manual german/english
(part no. 5304091/ 5304092)
a set (24) of DAP-40+ pressure digestion vessels (40ml, 40bar/ 580psi) (part no. 5303480)
24x DAP-40+ pressure vessels (part no. 5303270)
1x speedwave four rotor for DAP (part no. 5303449)
1x forming tool (part no. 5303437)
1x DAP-40 lid set, 10 each (part no. 5303446)
1x rupture disc set, 25 each (part no. 5303445)
and DAP-40+ cap for pressure control (part no. 5303790)
1x cap for DAP-40+ vessels with pressure sensor (part no. 5303790)
or a set (12) of DAP-30+ pressure digestion vessels (30ml, 80bar/ 1160psi) (part no. 5303680)
12x DAP-30+ pressure vessels (part no. 5303605)
1x speedwave four rotor for DAP (part no. 5303530)
1x vent tube for DAP (part no. 5303227)
1x forming tool (part no. 5709025)
1x DAP-30 lid set, 10 each (part no. 5709024)
1x rupture disc set, 25 each (part no. 5014616)
1x lip seal ring (part no. 5302962)
or a set (12) of DAP-60+ pressure digestion vessels (60ml, 40bar/ 580psi) (part no. 5303570)
12x DAP-60+ pressure vessels (part no. 5303603)
1x speedwave four rotor for DAP (part no. 5303530)
1x vent tube for DAP (part no. 5303227)
1x forming tool (part no. 5014612)
1x DAP-60 lid set, 5 each (part no. 5014617)
1x rupture disc set, 25 each (part no. 5014616)
1x lip seal ring (part no. 5302962)
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23
Setup and Commissioning
Berghof Products + Instruments
or a set (12) of DAP-100+ pressure digestion vessels (100ml, 40bar/ 580psi) (part no. 5303670)
12x DAP-100+ pressure vessels (part no. 5303672)
1x speedwave four rotor for DAP (part no. 5303530)
1x vent tube for DAP (part no. 5303227)
1x forming system (part no. 5303245)
1x DAP-80/100 lid set, 5 each (part no. 5300005)
1x rupture disc set, 25 each (part no. 5014616)
1x lip seal ring (part no. 5302962)
and a set (12) DAP cap without pressure sensor (part no. 5303540)
12x locking caps for DAP vessels without pressure sensor (part no.
5303540)
or a set (12) DAP cap for pressure control (part no. 5303590)
12x caps for DAP vessels with pressure sensor (part no. 5303580)
or a set (8) DAK-100/4 pressure digestion vessels (100ml, 100bar/1450psi) (part no. 5304980)
8x DAK-100/4 pressure vessels (part no. 5303279)
1x speedwave four rotor for DAK-100/4 (part no. 5304710)
1x vent tube for DAK (part no. 5303228)
1x forming station (part no. 5303245)
1x DAK lid set, 5 each (part no. 5302808)
1x rupture disc set, 5 each (part no. 5308030)
1x Opening station (part no. 5303625)
1x lip seal ring (part no. 5302962)
and a set (8) DAK-100/4 cap without pressure sensor (part no. 5304730)
8x locking caps for DAK-100/4 vessels without pressure sensor (part no.
5304740)
or a set (8) DAK-100/4 cap for pressure control (part no. 5304770)
8x caps for DAK-100/4 vessels with pressure sensor (part no. 5304760)
and a set (12) supplement DAC-17A (17ml, 130bar/1885psi) (part no. 5303340)
12x DAC-17 inserts complete (part no. 5303280)
or a set (12) supplement DAQ-20H (20ml, 100bar/1450psi) (part no. 5014412)
12x DAQ-10H quartz inserts complete (part no. 5014401)
1x forming tool (part no. 5014612)
or a set (24) multi tube system (10ml, 100bar/1450psi) (part no. 5308150)
24x MT-inserts made of PFA (part no. 5308054)
1x MT tube lifter (part no. 5308052)
1x MT rack (part no. 5308055)
24
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Berghof Products + Instruments
Options:
Setup and Commissioning
Evaporating set for DAP vessels (part no. 5303690)
12x lids for DAP vessels (part no. 5303226)
3x PP gas scrubber bottles (part no. 5005263)
2kg (4.4lb) marble granulate (part no. 5014622)
1x condenser, with lid (part no. 5302650)
11x blind plugs (part no. 5302817)
1x scrubber bottle screw-on lid (part no. 5302054)
2x scrubber bottle screw-on lids (part no. 5302055)
1x evaporating set vent tube (part no. 5302966)
1x drop collector (part no. 5303347)
Evaporating set for DAC vessels (part no. 5303950)
8x lids for DAC vessels (part no. 5302825)
3x PP gas scrubber bottles (part no. 5005263)
2kg (4.4lb) marble granulate (part no. 5014622)
1x condenser, with lid (part no. 5302650)
7x blind plugs (part no. 5302817)
1x scrubber bottle screw-on lid (part no. 5302054)
2x scrubber bottle screw-on lids (part no. 5302055)
1x evaporating set vent tube (part no. 5302966)
1x drop collector (part no. 5303348)
Forming system 6-fold for DAP-60+ (part no. 5303385)
Forming system 6-fold for DAP-100+ (part no. 5303275)
Forming system 6-fold for DAK-100/4 (part no. 5303386)
Weighing cup 2,0 ml, Set of 12 pcs. (part no. 5303612)
12x weighing cup 2ml (part no. 5303611)
Weighing cup 2,5 ml, Set of 12 pcs. (part no. 5303614)
12x weighing cup 2.5ml (part no. 5303613)
Stainless steel rupture disc for DAP-60+, 50bar Set of 20 pcs.
(part no. 5303740)
TFM-lid/rupture disc for DAP-60+, Set of 5 pcs. (part no. 5046180)
TFM-lid/rupture disc for DAP-100+, Set of 5 pcs. (part no. 5046170)
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25
Setup and Commissioning
3.2.
Berghof Products + Instruments
Standard Delivery Start-up Packages
Start-up Package speedwave four
with DIRC Temperature control and OPC Optical Pressure Control
for Routine Analysis of a wide range of sample types
and avarage sample throughput. (part no. 5304910)
1x speedwave four (part no. 5304000)
1x Turntable with DAP-60+ Pressure Vessels (part no. 5303570)
12x Closure caps for DAP-vessels without pressure control (part no.
5303540)
1x Closure caps for DAP-vessels with pressure control (part no. 5303580)
Start-up Package speedwave four
with DIRC Temperature control and OPC Optical Pressure Control
for Routine Analysis of a wide range of sample types
and avarage sample throughput. (part no. 5304920)
1x speedwave four (part no. 5304000)
1x Turntable with DAP-60+ Pressure Vessels (part no. 5303570)
12x Closure caps for DAP-vessels with pressure control (part no. 5303590)
Start-up Package speedwave four
with DIRC Temperature control and OPC Optical Pressure Control
for Routine Analysis of a wide range of sample types
and high sample throughput. (part no. 5304930)
1x speedwave four (part no. 5304000)
1x Turntable with DAP-40+ Pressure Vessels (part no. 5303480)
1x Closure caps for DAP-40+ vessels with pressure control (part no.
5303790)
Start-up Package speedwave four
with DIRC Temperature control and OPC Optical Pressure Control
for Routine Analysis of a wide range of sample types
with high pressure vessels. (part no. 5304940)
1x speedwave four (part no. 5304000)
1x Turntable with DAK-10/4+ Pressure Vessels (part no. 5304980)
8x Closure caps for DAK-100/4 vessels without pressure control (part no.
5304730)
1x Closure caps for DAK-100/4 vessels with pressure control (part no.
5304760)
Start-up Package speedwave four
with DIRC Temperature control and OPC Optical Pressure Control
for Routine Analysis of a wide range of sample types
with high pressure vessels. (part no. 5304950)
26
1x speedwave four (part no. 5304000)
1x Turntable with DAK-10/4+ Pressure Vessels (part no. 5304980)
8x Closure caps for DAK-100/4 vessels with pressure control (part no.
5304770)
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3.3.
Setup and Commissioning
3.3.1.
Ambient Conditions
Setup and Commissioning
The setup location must meet the following requirements:
Ambient temperature:
+10°C (50°F) to +35°C (93°F)
In addition, the temperature should lie between 40°C
(-40°F) and +70°C (158°F) during shipping and storage
Max. rel. humidity:
85%
Space requirements:
Approx. 80 x 100 x 90cm (DxWxH)
approx.31.5 x 39.4 x 35.4 inches (DxWxH)
Load bearing capacity:
At least 65 kg (143 lb)
Electrical connection:
230V; 50/ 60Hz
Make sure the vent opening on the back and left side of the unit are not covered.
The unit requires at least 15 cm of clearance on the back and left side.
The PFA tube inserted through the top of the oven should be vented to the outdoors or be connected to an exhaust system.
The oven must not be set up in wet conditions (it is not resistant to water sprays)
and not under the extraction hood / exhaust (increased risk of corrosion). We recommend setting the unit up next to the extraction hood / exhaust in order to lead
the vent hoses to this extraction hood / exhaust.
3.3.2.
Unpacking / Inspection
Open the shipping packaging and carefully remove it. Please save all packaging
in order to be able to return the unit to the manufacturer in its original packaging,
should service be required.
Two individuals should remove the microwave system from its packaging and
place it on a lab bench. Also remove all other components and accessories and
inspect the delivery to make sure it is complete.
Inspect the system for shipping damage such as cracks, scratches, dents, etc.
Warning !
Visible damage!
For safety reasons, never operate the unit if it exhibits visible signs of damage.
Contact your local, authorized dealer or Berghof Products + Instruments GmbH
to obtain the required service (Refer to the “Repairs / Customer Service” section
for contact addresses).
Note:
Should any components be missing or damages be detected, contact your local,
authorized dealer or Berghof Products + Instruments GmbH directly (Refer to the
“Repairs / Customer Service” section for contact addresses).
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27
Setup and Commissioning
3.3.3.
Berghof Products + Instruments
Installation
DANGER !
The unit employs high voltage and generates microwave radiation!
The speedwave must always be carefully connected to a grounded conductor.
Provided the wall outlet used is equipped with a ground connection, the supplied
power cord will ensure proper connection. If it is necessary to use an
extension cord to connect the system to the power supply, only a three-wire cord
with a ground connection may be employed.
The unit should not be set up near any devices which are sensitive to electromagnetic radiation. If necessary, a warning sign or label indicating “Caution, Microwave Emissions” should be applied or attached to the unit. Should there be
any suspicion or indication of increased levels of microwave radiation, please
immediately inform the Service Department at Berghof Products + Instruments
GmbH (Refer to the “Repairs / Customer Service” section for contact addresses).
Repair and servicing of the equipment may only be performed by trained
personnel.
Positioning
Position the system on the intended work surface. Make sure the vent opening on
the left side of the unit is not covered (at least 15cm (5.9inch) clearance).
A clearance of at least 50 cm (19.7”) that opens towards the front of the unit must
be available above the oven. The work surface must be able to support the weight
of the oven (approx. 65 kg; 143lb) and must have a surface area of approx. 60 x
100 cm (23,6 x 39,4 inch; LxW).
Exhaust
It is possible to feed or suck off acid fumes directly from the collecting vessel or
pressure vessels to an air extraction system via the PFA hose, which can be connected through the lid from above, (e.g. by means of a membrane or water-jet suction pump with an upstream wash bottle). In addition to this the oven chamber is
permanently sucked off and the gases must be conveyed to the extraction system
via the PE corrugated tube supplied.
Connection PFA exhaust air
extraction tube (ø 10 mm)
Connection PFA exhaust air
extraction tube (ø 62 mm)
Warning !
Hot acid vapors may be released.
The supplied vent tubes must therefore always be properly connected and attached to an exhaust system.
Make sure the PFA tube is securely attached so that it cannot pop off its connection fitting in case of a percussive pressure burst as occurs when a rupture disc
activates
28
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Setup and Commissioning
Note:
Users are responsible for assuring that appropriate ventilation of toxic gases is assured. Make sure that all ventilation procedures conform to applicable laws.
Connections
Power switch
(Basic device)
Power switch
(control unit)
Turntable installation
Use the supplied RS-232 cord to connect the basic unit with separate control unit
and connect both items with supplied power cord to a suitable 230V; 50 / 60Hz
power source.
The power switch is located
on the right-hand side of the
device
The switch is illuminated when
switched on.
The fuses and the RS-232
connection for the control unit
are next to it.
The power switch is located at
the rear of the device
The switch is illuminated when
switched on.
The fuses are located next to
it.
The
RS-232
connection
serves as the connection to
the basic device and the
Ethernet jack for connecting
up to a network.
RS-232 interface
Fuses
Power switch / plug
RS-232 interface
Ethernet connection
Fuses
Power switch / plug
Switch the control unit and then the device on at mains power switch and wait until
the main menu is set up on the screen. This may take a few seconds while the
screen remains dark.
Open the lid by pressing the open key on the keypad. A clearly audible clicking is
heard and unlocking is indicated on the screen. Then open the lid with the red
handle. The lid then swings to the right to its end stop. After 10 seconds the lid is
automatically locked again. In this case, again press open.
The rotor for the pressure vessels is preassembled on delivery. Remove the pressure vessels and insert the empty rotor into the microwave oven. By gently turning
the rotor on the axis, find the position at which the rotor again engages downwards.
The rotor is now correctly positioned in the microwave oven.
Accessories
The opening station for DAk-100/4 pressure vessels can be secured in an exhaust
hood / vent unit by means of the adhesives strips on its underside.
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Setup and Commissioning
Setup
Berghof Products + Instruments
Enter the setup window by pressing the Setup key. This area is passwordprotected. The default password is 4321.
The following parameters may be changed therein:
Parameter
Description
Factory
settings
T max set
Max. allowd temp. in programs
300°C
0°C
300°C
T min set
Min. allowd temp. in programs
50°C
0°C
300°C
P max set
Max. allowd pressure in programs
100 bar
0 bar
130 bar
p min set
Min. allowd pressure in programs
0 bar
0 bar
130 bar
Power max set
Max. allowd power in programs
100 %
0%
100 %
power min set
Min. allowd power in programs
0%
0%
100 %
Start with
application
Application, which is to be active
after the device is switched on
1
User password
The user can input a max. 4-digit
combination of numbers as a
password. This can be used as an
alternative to the default combination “4321”
0
0
9999
Pressure on/off
The OPC pressure measurement
on
can generally be activated or deactivated
Alarm time
Max. runtime of a temperature
program
0 min.
120 min
40 min.
min.
value
max.
value
The software can be changed to the relevant language by pressing a language
button.
30
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Setup and Commissioning
The date and time can be set by selecting the set time function. Time and date
have to be inserted precisely in the format below (DT#2008-06-12-17:20:41).
The system is now ready for use.
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Setup and Commissioning
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Hardware and Software Operation
4.
Hardware and Software Operation
4.1.
Method Preparation
4.1.1.
Information Regarding Digestion
The applied microwave energy causes the sample material to heat rapidly. The
speed of this heating process depends on the total volume of liquid in the oven as
well as on the amount of microwave radiation applied (power). The speedwave
four is controlled by continuously adjusting the microwave power. Sample temperature and sample pressure in each vessel are simultaneously acquired in a contactless process during every rotation of the sample turntable, and the microwave
power level is adjusted accordingly. In addition, microwave power is also controlled
on the basis of the number of samples actually present in the turntable. This graduated regulation concept leads to reproducable heating curves and therefore to reproducable results.
Heating the acid mixture results in the creation of vapor pressure. The degree of
this vapor pressure depends greatly on the temperature. All digestion vessels have
a maximum permissible pressure. If this maximum pressure is exceeded, the rupture disc in the pressure vessel activates, providing a rapid pressure release into
the collection vessel.
In addition to the vapor pressure, reaction gases (primarily carbon dioxide generated by samples containing carbon) also produce pressure. This pressure is therefore dependent on the sample amount, the vessel volume, as well as the carbon
content of the sample.
Together with the applied microwave radiation, digestion of organic substances
also releases reaction heat. These types of reactions frequently begin in the temperature range between 130 - 150°C (266 - 302°F). We therefore recommend holding the samples at this temperature for some time (3-5 minutes), in order to allow
this reaction heat to subside somewhat. The temperature should then be increased
to the desired maximum in a second stage in order to obtain optimum digestion
quality.
Caution
Reaching the maximum pressure!
Please note that the reaction pressure is only reached during the course of the reaction, in other words, several minutes after the maximum temperature has been
reached. Therefore, an activation of the rupture discs may be anticipated even after the temperature has reached a constant level.
Optionally the speedwave four can be equipped with pressure monitoring. With
this option the, internal vessel pressure determined and, when the preset maximum pressure is reached, the unit automatically switches to a pressure-controlled
mode. In this mode the microwave output is controlled so that the internal pressure
of the vessel does not exceed the maximum pressure.
Caution
Rupture disc corrosion!
Depending on the acid being employed and the digestion parameters, the aluminum rupture discs are subject to more-or-less extreme wear. Replace the discs
regularly (after approximately ever 20 digestion procedures) to prevent the discs
from rupturing prematurely.
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Hardware and Software Operation
4.1.2.
Berghof Products + Instruments
Controller
The control unit is operated via a touch-screen. In order to trigger a function, briefly
press on the representative symbol on the screen. In the following text the key
fields of the touch-screen are shown in a frame, e.g., Application . Pressing the ok
or esc key always takes you from a submenu to the next higher menu
Main window
Switch the control unit and then the device on at mains power switch and wait until
the main menu is set up on the screen. This may take a few seconds (approx. 15
sec.) while the screen remains dark.
Operation
If a key is selected which request insertion of text or figures a keypad is displayed.
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Berghof Products + Instruments
Hardware and Software Operation
Key functions
4.1.3.
key:
Function
Application
Function for selceting or modifiing a stored application. Active application is displayed. (in example
above “Calcite; Dolomite”)
Data
Function to review stored digestion process data. Last
data file is displayed. (in example above “data_file0”)
Start
Start of microwave
Service
Service area
Access for authorized service technicians only.
Open
release the electronic lid locking (only possible when
microwave is stopped)
Setup
Setup. Access with 4-digid code
(factory setting 4321)
Modifying Application
The operator can select from a total of 200 applications, 25 of which are preinstalled.
After accessing the application function initially a selection of maximally 12 applications is displayed which the user can compile to form a "User Library". Furthermore, 3 standard applications are stored: pressure adjustment, power test and
function test.
To modify an application a method is selected and the detailed data modified using
modify. With “add all available” applications are displayed, one of which can also
be selected.
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Hardware and Software Operation
Berghof Products + Instruments
Select a application and the wkindow for programming and modifiing applications is
opened.
A program always comprises five steps, containing the parameters:
Select as your
application
With this it is possible to allocate disk space for the application in the “User Library”. Permissible range: 0 – 12
It must be borne in mind that applications can only be allocated to empty fields in
the Library. If an application is positioned in a disk space which is already occupied, the old application must first be deleted by using "0" before the new method
and be stored.
Temperature (°C)
Setpoint temperature, in °C (Refer to the “Appendix” for conversion)
Permissible range: 50-300 °C
Pressure (bar)
Max. pressure in bar (Refer to the “Appendix” for conversion)
Permissible range: 0-100 bar
Time (min)
Time in min. for which the setpoint temperature shall be kept constant
Permissible range: 0-59 min.
Slope (min)
Ramp time of the program step, in min.
Permissible range: 0-59 min.
Power (%)
Max. power in % which shall be applied in this step.
Permissible range: 0-100%
Vessel
Number of type of vessel, see table o n right hand side
Mag temp.
Max. allowed magnetron temperature
Permissible range: 0 -120°C
Typical range: 80 – 90 °C
Values <20°C are only used for evaporation programs, refer to ‘Appendix’
Total time
Total run time in min.
The maximum permitted runtime of a program is defined in Setup.
PI Parameter
The PI parameters define the system’s temperature regulation characteristics
based on the following relationship:
Power [%] = (Prop + I) * * Plimit
where
EN_Hard-Software Operation.doc
Prop
= ∆T * P-band
I
= Int + ∆T / Int
∆T
= Tsoll – Tist
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Berghof Products + Instruments
Hardware and Software Operation
P-band
Proportional amplification of the PI regulation
Int
Integral share of the PI regulation
Plimit
Means power % of corresponding program step
Exit this funtion by pressing exit or save + exit. .
25 programs have been preinstalled.
EN_Hard-Software Operation.doc
Program-No.
Description
1
Calcite, Dolomite
2
Cleaning, Vessel conditioning
3
Coal, DIN 22022-1
4
Complexation H3BO3
5
Evaporation
6
Feed
7
Feldspar
8
Filter, glass fiber
9
Fly Ash, DIN EN 14385
10
Food (no/low fat)
11
Food (High fat)
12
13
Glass, Quartz
Limestone
14
Oil, Lubricant
15
Plastic, PE, ROHs
16
Plastic, Waste DIN 22022-1
17
Soil ISO 11466, EN 13346
18
Soil EPA 3051
19
Soil, Sediment EPA 3052
20
Tissue, Blood
21
Vegetables, Leaves
22
Vegetable Oil
23
Water DIN EN 1189, ISO 6878
24
Water Aqua Regia
25
Water EPA 3015
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Hardware and Software Operation
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Note:
Program 5 evaporation is used for evaporation of acid solutions only! Times may
be changed only and and magT must be set to <20°C.
4.1.4.
Developing a New Application
Digestion of new sample material, that is, of samples for which you have no previous experience, requires a special, systematic procedure. We recommend the following process when developing such an application:
Check the “Appendix” to determine whether the application list already contains work instructions for the sample material in question or for a similar material then, if necessary, request a copy of the original process instructions from
your local, authorized dealer or from Berghof Products + Instruments GmbH.
Should you not be able to find your sample material, search through the relevant technical literature for a corresponding process instruction. You can also
request assistance from your local, authorized dealer or from Berghof Products
+ Instruments GmbH.
For safety reasons, initially reduce the specified sample amount by 30-50 %,
while still using the specified acid quantity and digesting with the defined temperature program.
Optimize the acid mixture and the temperature profile until you obtain a clear
solution.
In the final step you can gradually increase the sample amount until the
higher pressure causes the rupture disc to activate. The maximum sample
quantity to be used should be approx. 30 % of this amount.
If the pressure control system is installed the maximum sample quantity may
also be estimated from the measured pressures in the digestion vessels.
Note:
When digesting unknown sample materials (e.g., when developing methods) we
recommend digesting only single samples in the speedwave four.
The single sample is automatically positioned directly in front of the sensors and
rotor rotation is stopped. This simplifies continuous temperature and pressure
monitoring for this vessel.
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Berghof Products + Instruments
4.2.
Hardware and Software Operation
Performing a Digestion Procedure
Warning !
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work which may
involve contact with chemicals, that is, when working with acids, pressure vessels,
during cleaning, etc.!
DANGER !
Pressure vessels!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH (Refer to the “Repairs / Customer Service” section for contact addresses).
Always wear safety glasses/goggles and protective gloves when working with the
pressure vessels!
Note any changes in the appearance of the pressure vessel which could indicate
possible material fatigue, e.g., deformation of the vessel, difficulty screwing on
lids, etc. even when the vessel is cold and not under pressure. All such vessels
should be immediately returned to Berghof Products + Instruments GmbH for inspection.
Never attempt to use force to open the vessels. Never use tools to open the
vessels!
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Hot gases and vapors may be released from the digestion vessel when it is
opened! Always make sure the vent opening on pressure vessels faces away
from both yourself and other individuals!!
Only open the digestion vessel under a vent hood or other exhaust system.
Particular care is required when working with hydrofluoric acid (HF). Observe
all relevant data sheets and safety instructions!
Never use more than one rupture disc per vessel!
Note:
Renew the vessels after around 10,000 digestion processes to maintain reliable
operating conditions and to prevent negative influences on your analysis results
(e.g. memory effects etc.).
Berghof Products + Instruments GmbH includes its digestion vessels in the warranty coverage. Nevertheless all of the vessels are subject to a certain aging
process, which also depends on the type and frequency of the application. Typically the service life is 10,000 digestion processes or at least 3 years.
The speedwave four microwave oven can hold up to 24 DAP digestion vessels or
up to 8 DAK-100/4 vessels. Vessel types must not be mixed as this will result in extreme differences in sample heating.
The procedure employed for all vessel types is basically similar. This section therefore first describes the general procedures, while any differences between
the vessel types will be dealt with in detail in the following sections.
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Hardware and Software Operation
Sample amount
Caution
Berghof Products + Instruments
Weigh the sample material into the vessels, then add the acid. The maximum
sample quantity depends on the vessels employed and must be strictly observed
(refer to the “Technical Specifications” section).
Minimum fill amount!
In each pressure vessel, at least approx. 5ml of liquid should be employed so that
the temperature sensor can determine the sample temperature precisely.
The microwave oven requires a certain minimum load of approx. 20 ml of liquid. If
lower volumes of liquid must be used, at least four vessels must be used for each
run in order to achieve the required total load.
If the fluid amount employed is too small, the oven may be damaged during longer
operation! An inadequate liquid load can also result in rotor overheating and, in the
worst case, in rotor damage.
Lid placement
Visually inspect the rupture discs. In case of extensive traces of corrosion or other
visible damage to the rupture discs, they must be replaced for safety reasons.
A bulge in the center of the rupture disc after use is normal and will not affect its
functions.
Make sure the rupture disc is properly seated in the lid, that is, that its edge sits
uniformly in the lid groove.
Press the seal lip on the appropriate molded part to spread the seal ring on the
closure, then place the lid on the lower part of the vessel.
Lock the vessel
Lock the vessel with the coupling cap. Only slight pressure is needed to secure
the rupture disc. Proper vessel seal is ensured by the pressure supported seal lip,
even under maximum interior vessel pressure.
Vessel placement
The rotor should be loaded with the digestion vessels as symmetrically as possible
and the digestion vessels connected to the receptacle. The first vessel must be inserted in the position marked “1” and the rest arranged symmetrically (refer to the
“Attachment”).
Any unused positions on the collection vessel should be sealed with the supplied
blind stoppers or with lock screws in order to ensure the proper operation of the
gas removal.
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Berghof Products + Instruments
Close the microwave
Warning !
Hardware and Software Operation
Close the swiveling lid. Insert the vent tube
into the oven from above until it reaches its
stop and make sure that it is properaly connected to an exhaust system.
The vent tube can be connected to an acidresistant suction pump or can be connected
to an existing vent system (e.g., an exhaust
hood).
Close the oven door until the lock engages.
Hot acid vapors may be released.
The supplied vent tubes must therefore always be properly connected and attached to an exhaust system.
Make sure the PFA tube is securely attached so that it cannot pop off its connection fitting in case of a percussive pressure burst as occurs when a rupture disc
activates.
Note:
The desired program must be selected before the microwave oven is started.
Start program
After an appropriate application has been selected or created and the oven has
been filled with the desired number of vessels the digestion program is started with
“Start” in the main menu.
The following input window appears in which the program can again be
modified and a file name can be input. If file names are identical the index is
automatically raised by 1.
Note:
If the program is modified at this stage of operation the modification affects only
the current run, but not the stored application.
Number of samples
Again check if the setting is for the correct type of vessel and input the number of
samples.
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Hardware and Software Operation
Berghof Products + Instruments
Before file name may be modified the following dialog window is opened. Therein
file name be changed and indeces may be reset to 0.
Now start the application in line Start Digestion . The temperature profile will be
displayed graphically. After an initial period of approx. 20 sec. heating starts.
The program can be canceled at any time by pressing the stop key.
Note:
The magnetron cannot be switched on while the microwave is open!
If you wish to open the microwave, stop the program first!
The program can be canceled at any time by pressing the stop key.
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Berghof Products + Instruments
Real time display
Hardware and Software Operation
During digestion the highest sample temperature and pressure curve is displayed
as are all temperatures inside the vessels in the form of a bar graph. In addition the
target temperature/pressure is set and beneath this the maximum temperature/pressure displayed. As long as a temperature is below 50°C it is indicated only
as "low". No vapor pressures worth mentioning occur within this temperature
range.
Furthermore, the magnetron temperature, T-Mag and the microwave power
output power are displayed.
Besides the pressure, in the middle graph the microwave output or magnetron
temperature can be displayed optionally. For this purpose please press T-Mag or
power.
If the system is operated with pressure measurement, all internal pressures of the
vessels are represented as bars and the highest internal pressure of a vessel is
displayed.
Note:
When turntable DAP-40+ is used sample temperatures of the outer circle are monitored continuously and microwave power is controlled according to the highest
temperature. 12position display corresponds to the temperature distribution of the
16 vessels in the outer circle. Only pos. 1, 4, 7 and 10 give the correct temperatures of vessels 1, 5, 9 and 13.
Comment
After digestion has finished a comment can be input.
To enter the comment, select the appropriate comment line and enter the text
by means of the keyboard.
By pressing finish you return to the main window. All data are memorized automatically and can be reprocessed at any time as described under `Data Reprocessing´.
Note:
The magnetron cannot be switched on while the microwave is open!
If you wish to open the microwave, stop the program first!
The program can be canceled at any time by pressing the stop key.
Caution
If possible, do not operate the oven unsupervised, e.g., overnight.
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Hardware and Software Operation
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4.3.
Sample Loading
4.3.1.
Handling the DAP-40+, DAP-30+, DAP-60+, and DAP-100+ Pressure Vessels
The DAP pressure vessels are made up of a TFM pressure vessel, an aluminum
rupture disc, a TFM lid, and a coupling cap . The PP rotor can hold up to 12 DAP60+ vessels.
Weigh the sample material into the vessels. The maximal weighing-in quantity,
which depends on the vessels, must be borne in mind (see 'Technical Data' section).
Weighing-in using TFM To simplify the weighing process and
weighing cups
prevent loss of samples the samples
can be weighed directly into the Berghof
weighing cups made from TFM. These
are placed in the digestion vessel with
the sample and remain there during digestion. After digestion and thorough
rinsing with distilled water they can be
reused.
Adding the acid
Now add the acid mixture. Pay attention to the maximum and minimum filling quantity, which depends on the vessels. (Refer to 'Technical Data').
Small weighed-in
sample quantities
Rupture disc
DANGER !
Visually inspect the rupture disc. In case of extensive traces of corrosion or other
visible damage to the rupture disc, it must be replaced for safety reasons.
A bulge in the center of the rupture disc
after use is normal and will not affect its
functions. Make sure the rupture disc is
properly seated in the locking lid, that is,
that its edge sits uniformly in the lid
groove.
When using a TFM lid/rupture disk combination of the type offered especially for
digestion processes subject to maximum cleanness requirements, the rupture disk
is not required.
Rupture discs!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for contact addresses).
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Never use more than one rupture disc per vessel!
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Berghof Products + Instruments
Install the lid
Hardware and Software Operation
From time to time, press the locking lid
seal lip on the appropriate molded part to
spread it, and place the lid on the lower
part of the vessel.
Alternatively the sealing lip of the locking
lid can be dilated in the forming station.
The stamp is wound downwards as far as
possible. This station permits a more even
dilation of the sealing lip and is recommended in particular for DAP-100+, DAK17 and DAK-100/4.
Distinct resistance must be felt when the
lid is placed on the pressure vessel. If no
resistance is felt, the seal lip must be
spread as described above.
Close the vessel
After the sample has been weighed in and
the acid has been added, place the seal
lid on vessel and close it hand-tight with
the coupling cap. Only slight pressure is
needed to secure the rupture disc. Proper
vessel seal is ensured by the pressure
supported seal lip, even under maximum
interior vessel pressure.
Caution
The maximum sample quantity depends on the vessels employed and must be
strictly observed (refer to the “Technical Specifications” section).
Caution
Minimum fill amount!
In each pressure vessel, at least approx. 5ml of liquid should be employed so that
the temperature sensor can determine the sample temperature precisely.
The microwave oven requires a certain minimum load of approx. 20 ml of liquid. If
lower volumes of liquid must be used, at least four vessels must be used for each
run in order to achieve the required total load.
If the fluid amount employed is too small, the oven may be damaged during longer
operation! An inadequate liquid load can also result in rotor overheating and, in the
worst case, in rotor damage.
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Hardware and Software Operation
Vessel placement
Berghof Products + Instruments
Digestion vessels should be distributed as symmetrically as possible around the
rotor (see `appendix`).
During placement, the vent fitting is simply screwed onto the associated collection vessel tube (it may be necessary to
first move the vessel into the proper position).
Any unused positions on the collection
vessel should be sealed with the supplied
blind stoppers or with lock screws in order
to ensure the proper operation of the gas
removal.
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Berghof Products + Instruments
4.3.2.
Hardware and Software Operation
Handling DAQ-20H Pressure Vessels
Warning !
Breakage hazard!
Hand-tighten the quartz glass lids.
Excessive tightening can destroy the vessels!
The procedure for the quartz glass inserts DAQ-20 with pressure vessels DAP-60+
or DAP-100+ is largely identical to the procedure for pressure vessels without
quartz glass inserts. Only the changes in the steps of the procedure are therefore
described here.
DAQ-20H pressure vessels consist of a quartz
insert (pressure vessel), a Monel rupture disc, a
rupture disc retainer ring, and a TFM lid.
The vessel structure is illustrated below.
Rupture disc
DANGER !
Visually inspect the rupture disc. In case of extensive traces of corrosion or other visible
damage to the rupture disc, it must be replaced
for safety reasons. A bulge in the center of the
rupture disc after use is normal and will not affect its functions. Make sure the rupture disc is
properly seated in the retainer ring.
Rupture discs!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for contact addresses).
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Never use more than one rupture disc per vessel!
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Hardware and Software Operation
Close the DAQ-10
Berghof Products + Instruments
Prior to every use, press the locking lid seal
lip on the appropriate molded part to spread
it, and place the lid on the glass insert.
Distinct resistance must be felt when the lid is
placed on the glass insert. If no resistance is
felt, the seal lip must be spread as described
above.
Insert the closed quartz vessel into the DAP60+ or DAP-100+ vessel.
Close the DAP-vessel hand-tight with the
coupling cap. Only slight pressure is needed
to secure the rupture disc. Proper vessel seal
is ensured by the pressure supported seal lip,
even under maximum interior vessel pressure.
Caution
The maximum sample quantity depends on the vessels employed and must be
strictly observed (refer to the “Technical Specifications” section).
Caution
Minimum fill amount!
In each pressure vessel, at least approx. 5ml of liquid should be employed so that
the temperature sensor can determine the sample temperature precisely.
The microwave oven requires a certain minimum load of approx. 20 ml of liquid. If
lower volumes of liquid must be used, at least four vessels must be used for each
run in order to achieve the required total load.
If the fluid amount employed is too small, the oven may be damaged during longer
operation! An inadequate liquid load can also result in rotor overheating and, in the
worst case, in rotor damage.
Warning !
Breakage hazard!
Hand-tighten the quartz glass lids. Excessive tightening can destroy the vessels!
The further procedure, beginning with “inserting the vessels into the microwave” is
identical with the procedure described in Handling the pressure vessels DAP-30+,
DAP-60+ and DAP-100+´ .
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Berghof Products + Instruments
4.3.3.
Hardware and Software Operation
Handling DAC-17 Pressure Vessels
The procedure for the DAC-17 inserts with pressure vessels DAP-100+ is largely
identical to the procedure for pressure vessels without inserts. Only the changes in
the steps of the procedure are therefore described here.
DAC-17 pressure vessels consist of a TFM insert (pressure vessel), a ceramic
pressure jacket, a Monel rupture disc, a rupture disc retainer ring, and a TFM lid.
The vessel structure is illustrated below.
Rupture disc
DANGER !
Visually inspect the rupture disc. In case of extensive traces of corrosion or other visible
damage to the rupture disc, it must be replaced
for safety reasons. A bulge in the center of the
rupture disc after use is normal and will not affect its functions. Make sure the rupture disc is
properly seated in the retainer ring.
Rupture discs!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for contact addresses).
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Never use more than one rupture disc per vessel!
Prior to every use, press the locking lid seal lip
on the appropriate molded part to spread it, and
place the lid on the TFM insert.
Close the DAC-17
Alternatively the sealing lip of the locking lid can
be dilated in the forming station. The stamp is
wound downwards as far as possible. This station permits a more even dilation of the sealing
lip and is recommended in particular for DAP100+, DAK-17 and DAK-100/4.
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Hardware and Software Operation
Berghof Products + Instruments
Distinct resistance must be felt when the lid is
placed on the TFM insert. If no resistance is felt,
the seal lip must be spread as described above.
First insert the vessel bolster, then the ceramic
pressure jacket and finally the closed DAC-17
vessel into the DAP-100+ vessel.
Close the DAP-vessel hand-tight with the coupling cap. Only slight pressure is needed to secure the rupture disc. Proper vessel seal is ensured by the pressure supported seal lip, even
under maximum interior vessel pressure.
Caution
The maximum sample quantity depends on the vessels employed and must be
strictly observed (refer to the “Technical Specifications” section).
Caution
Minimum fill amount!
In each pressure vessel, at least approx. 5ml of liquid should be employed so that
the temperature sensor can determine the sample temperature precisely.
The microwave oven requires a certain minimum load of approx. 20 ml of liquid. If
lower volumes of liquid must be used, at least four vessels must be used for each
run in order to achieve the required total load.
If the fluid amount employed is too small, the oven may be damaged during longer
operation! An inadequate liquid load can also result in rotor overheating and, in the
worst case, in rotor damage.
The further procedure, beginning with “inserting the vessels into the microwave” is
identical with the procedure described in Handling the pressure vessels DAP-30+,
DAP-60+ and DAP-100+´ .
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4.3.4.
Hardware and Software Operation
Handling DAK-100/4 Pressure Vessels
The DAK-100/4 pressure vessels consist
of the TFM pressure vessel, a Monel
rupture disc, a TFM lid, and a TFM coupling cap.
The PP rotor can hold up to 8 DAK100/4 vessels.
Rupture disc
DANGER !
Visually inspect the rupture disc. In case of extensive traces of corrosion or other
visible damage to the rupture disc, it must be replaced for safety reasons.
A bulge in the center of the rupture disc
after use is normal and will not affect its
functions. Make sure the rupture disc is
properly seated in the lid, that is, that its
edge sits uniformly in the lid groove.
Rupture discs!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for contact addresses).
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Never use more than one rupture disc per vessel!
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Hardware and Software Operation
Install the lid
Berghof Products + Instruments
From time to time, press the locking lid seal lip
on the appropriate molded part to spread it, and
place the lid on the lower part of the vessel.
Alternatively the sealing lip of the locking lid
can be dilated in the forming station. The
stamp is wound downwards as far as possible.
This station permits a more even dilation of the
sealing lip and is recommended in particular for
DAP-100+, DAK-17 and DAK-100/4.
Close the vessel
Distinct resistance must be felt when the lid is
placed on the pressure vessel. If no resistance
is felt, the seal lip must be spread as described
above.
After the sample has been weighed in and the
acid has been added, place the seal lid on
vessel and close it hand-tight with the coupling
cap. Only slight pressure is needed to secure
the rupture disc. Proper vessel seal is ensured
by the pressure supported seal lip, even under
maximum interior vessel pressure.
Caution
The maximum sample quantity depends on the vessels employed and must be
strictly observed (refer to the “Technical Specifications” section).
Caution
Minimum fill amount!
In each pressure vessel, at least approx. 5ml of liquid should be employed so that
the temperature sensor can determine the sample temperature precisely.
The microwave oven requires a certain minimum load of approx. 20 ml of liquid. If
lower volumes of liquid must be used, at least four vessels must be used for each
run in order to achieve the required total load.
If the fluid amount employed is too small, the oven may be damaged during longer
operation! An inadequate liquid load can also result in rotor overheating and, in the
worst case, in rotor damage.
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Berghof Products + Instruments
Vessel placement
Hardware and Software Operation
Digestion vessels should be distributed as symmetrically as possible around the
rotor (see `appendix`).
During placement, the vent fitting is simply screwed onto the associated collection vessel tube (it may be necessary to
first move the vessel into the proper position).
Any unused positions on the collection
vessel should be sealed with the supplied
blind stoppers or with lock screws in order to ensure the proper operation of the
gas removal.
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Hardware and Software Operation
4.4.
Berghof Products + Instruments
Sample Removal
After the microwave switches off, the vessels must remain in the oven for at least
10 minutes. After this time, all vessels can be removed (disconnect the vent tube
first!) and can be placed under an vent hood or other exhaust system for further
cooling. Acid vapors can leak out of the vessels during the cooling phase. This is
due to the flow behavior of TFM and, generally, does not result in any sample loss
or contamination.
The vessels may only be opened after an adequate cooling period. When the vessels are opened, their internal temperatures should not lie above 100°C (212°F).
The length of the cooling period depends on the heating time and the digestion
temperature. The total cooling time before the vessels are opened should be at
least half the digestion time and, if possible, somewhat more than this.
Warning !
Burn and acid burn hazard!
The digestion vessels must not be removed from the oven for at least 10 minutes
after the end of the digestion program. This will ensure that the samples have
cooled sufficiently to avoid rupture disc breakage caused by jarring during removal.
Always wear safety glasses/goggles and protective gloves when opening vessels!
Always work under an vent hood or other exhaust system!
Never point the gas outlet towards yourself or anyone else. Aggressive gases are
released from here when the vessels are opened or if the rupture disc activates!
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4.4.1.
Hardware and Software Operation
Removing and Opening DAP-40+, DAP-30+, DAP-60+ and
DAP-100+ Pressure Vessels
A total cooling time of at least 20 minutes is required for these vessels.
DANGER !
Pressure vessels!
Always wear safety glasses/goggles and protective gloves when working with the
pressure vessels!
Never attempt to use force to open the vessels. Never use tools to open the vessels!
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Hot gases and vapors may be released from the digestion vessel when it is
opened! Always make sure the vent opening on pressure vessels faces away from
both yourself and other individuals!!
Only open the digestion vessel under a vent hood or other exhaust system. Particular care is required when working with hydrofluoric acid (HF). Observe all relevant data sheets and safety instructions!
Warning !
Residual pressure in vessels!
Even after cooling, a residual pressure will remain in the vessels!
Always wear safety glasses/goggles and protective gloves when opening vessels!
Always work under an vent hood or other exhaust system!
Never point the gas outlet towards yourself or anyone else. Aggressive gases are
released from here when the vessels are opened or if the rupture disc activates!
Caution
Opening the vessels
If there is still a high residual pressure in the vessel, it will be difficult to unscrew
the lid. If in doubt, allow the vessel to cool for an additional period of time!
If the solution has a high CO2 content, opening the vessel too quickly can cause
the solution to foam up, resulting in sample loss!
To open the vessels, hold onto the coupling cap and slowly
turn the vessel clockwise. Make sure the gas outlet always
faces away from you.
As gases begin to escape from the vessel, wait a moment or
slightly close the vessel by turning it counterclockwise. Continue in this manner and gradually open the vessel.
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Hardware and Software Operation
4.4.2.
Berghof Products + Instruments
Removing and Opening DAK-100/4 Pressure Vessels
A total cooling time of at least 30 minutes is required for these vessels.
DANGER !
Pressure vessels!
Always wear safety glasses/goggles and protective gloves when working with the
pressure vessels!
Never attempt to use force to open the vessels.
The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw-on tube connections in case
of excessive vessel pressure. In some cases, such a spontaneous pressure release may occur after the vessel has been removed from the microwave oven.
Hot gases and vapors may be released from the digestion vessel when it is
opened! Always make sure the vent opening on pressure vessels faces away from
both yourself and other individuals!!
Only open the digestion vessel under a vent hood or other exhaust system. Particular care is required when working with hydrofluoric acid (HF). Observe all relevant data sheets and safety instructions!
Warning !
Residual pressure in vessels!
Even after cooling, a residual pressure will remain in the vessels!
Always wear safety glasses/goggles and protective gloves when opening vessels!
Always work under an vent hood or other exhaust system!
Never point the gas outlet towards yourself or anyone else. Aggressive gases are
released from here when the vessels are opened or if the rupture disc activates!
Caution
If there is still a high residual pressure in the vessel, it will be difficult to unscrew
the lid. If in doubt, allow the vessel to cool for an additional period of time!
If the solution has a high CO2 content, opening the vessel too quickly can cause
the solution to foam up, resulting in sample loss!
Opening the vessels
The vessel must be placed on the opening station and make sure
the gas outlet always faces away from you.
To open the vessels, slowly turn the vessel clockwise. As gases
begin to escape from the vessel, wait a moment or slightly close
the vessel by turning it clockwise. Continue in this manner and
gradually open the vessel.
Once the pressure has been completely released, you can open
the aluminum cap by hand and remove the TFM lid.
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Berghof Products + Instruments
4.5.
Hardware and Software Operation
Data Reprocessing
The temperature and pressure development during a digestion process is recorded
individually for each vessel and, if need be, saved after digestion has been completed. Prior to saving the index of the data file is automatically incremented.
Data in the main menu serves to plot stored temperature developments on the
screen. To start with the file system is opened. Several individual files can have
been stored under each file name. The number is displayed at bottom right.
OK is used to call a selected file and have it represented graphically. Exit takes
you back to the main menu. The file manager takes you to a representation of all
stored files incl. txt files that can be exported to Excel or a similar program.
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Hardware and Software Operation
File:
Berghof Products + Instruments
The current file name is displayed and by selecting this field it can be renamed.
OK
Exit the menu item to the main menu.
<< and >>
The entire time range can be scrolled through using the << and >> arrow buttons;
during this the selected point in time is displayed in the time window (bottom left). It
is always represented in a 60-minute window. If digestion takes longer, you change
to the next lower or higher time window using the << and >> arrow buttons.
In addition the target temperature/pressure are set and beneath this the maximum
temperature/pressure displayed.
Single curve
representation:
more
By selecting the corresponding vessel number in the lower bar chart the temperature and pressure development of this vessel is displayed.
Display of the temperature program and further information such as the date, time
and comments.
Note:
When turntable DAP-40+ is used sample temperatures of the outer circle are monitored continuously and microwave power is controlled according to the highest
temperature. 12position display corresponds to the temperature distribution of the
16 vessels in the outer circle. Only pos. 1, 4, 7 and 10 give the correct temperatures of vessels 1, 5, 9 and 13.
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Berghof Products + Instruments
4.6.
Hardware and Software Operation
Data backup / data export using USB
The file manager takes you to a representation of all stored files incl. txt files that
can be exported into Excel or a similar program.
To export data you plug a Memory Stick into the USB port and press USB.
In the following menu you can delete all files on the Memory stick, copy all of the
data from the speedwave four onto the Memory stick and remove the Memory stick
again. In all of the steps attention must be paid to the status message at top right.
Bear in mind that only the same Memory stick may be used all the time. If you wish
nd
to copy data onto a 2 Memory stick, the control unit must be switched off and on
again.
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Hardware and Software Operation
Berghof Products + Instruments
The digestion data are stored in a binary format which can only be read by means
of the speedwave four control unit.
Besides, all data are also stored in txt format, which can then be imported to Excel
or Word on your computer.
Txt-Datenformat:
90;90;90;90;90;90;90;90;85;85;85;85;85;50;72;3;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;0;34;
90;90;90;90;90;90;90;90;90;90;90;90;90;50;87;5;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;0;34;
90;90;85;85;85;85;85;85;90;85;85;85;90;50;102;7;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;54;34;
90;85;90;90;90;90;90;90;90;90;90;90;90;50;110;8;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;90;34;
95;90;90;90;95;95;95;95;95;95;95;95;95;50;125;10;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;90;34;
95;95;95;95;95;95;95;95;95;95;95;95;95;50;140;12;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;90;34;
95;95;95;95;95;95;95;95;95;95;95;95;95;50;155;14;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;90;34;
95;95;95;95;95;95;95;95;95;95;95;95;95;50;155;16;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;90;34;
100;95;95;95;95;95;95;95;95;95;95;95;100;50;155;17;50;0;0;0;0;0;0;0;0;0;0;0;0;0;0;50;90;34;
155;50;2;15;90;
200;50;10;30;90;
50;0;1;15;0;
50;0;1;1;0;
50;0;1;1;0;
20;20;77;3;120;
DT#2008-06-12-18:37:05;
Data records are recorded at 15-second intervals.
Each line contains a complete data record of the vessel consisting of:
T-max; 12x T-ist; dummy; T-soll; dummy; dummy; p-max; 12x p-ist; p-soll; power;
magT;/ T-max; 12x T-actual; T-target; dummy; dummy; p-max; 12xp-actual;
p-target; power; magT;
Blank line
Program parameters with one program step represented per line
Date and time
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Berghof Products + Instruments
5.
Options
5.1.
Evaporating Unit
Options
DANGER !
Explosion hazard!
Do not use perchloric acid.
No organic solvents (alcohols, hydrocarbons, etc.) may be placed in the pressure
vessels or the microwave.
Highly reactive substances which spontaneously react at higher temperatures or
in the presence of oxidizing agents or which may be nitrated and are potentially
explosive may not be digested in the microwave. Examples of such substances
include: explosives (TNT, etc.), perchlorates, ether, pyrophoric substances, etc.
Warning !
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work which may
involve contact with chemicals, that is, when working with acids, pressure vessels,
during cleaning, etc.!
3-stage gas scrubber system
Connection for water cooling
Gas exhaust
PFA tube
After connecting the condensation unit to the vent tube, the unit can also be employed to evaporate acids. For this process, the pressure vessels are operated with
a special screw-on cap, without Teflon lid. The vent tube used for evaporating is
equipped with a temperature sensor which must be connected to the socket provided for this purpose on the rear of the unit.
The speedwave four microwave evaporating unit is used to concentrate acids or
sample digestion solutions obtained after digestion procedures employing HNO3,
HCl, HF, and water by means of distillation at ambient pressure. The escaping acid
vapors are condensed and neutralized in a 3-stage, water-cooled gas scrubber
system.
The unit is not suited for concentrating acids or liquids with a boiling point above
200°C (392°F) such as sulfuric and phosphoric acid. For safety reasons (explosion
hazards) the use of perchloric acid and organic solvents is prohibited.
Warning !
EN_Options.doc
Hot acid vapors are generated!
Hot acid vapors are generated during evaporating. Take particular care to ensure
that all connections are secure and do not leak. In particular, the tube connection
between the microwave and the gas scrubber must always be totally sealed.
Secure the tube appropriately to ensure that no acid vapors can escape in the direction of surrounding individuals, even when the screw-on connection is opened.
The microwave system, together with the gas scrubber, must be set up under a
vent hood.
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Options
5.1.1.
Berghof Products + Instruments
Standard Delivery
Refer to “Standard Delivery” in the “Setup and Commissioning” section.
5.1.2.
Installation and Commissioning
Ambient conditions
Aside from the requirements cited in the “Ambient Conditions” section of the chapter “Setup and Commissioning”, the operation of the gas scrubber also requires a
coolant water connection (approx. 0.5 liters/min. with an inlet temperature not exceeding 20°C, 68°F). In addition, there is also the need for an increased space of
53 x 27 cm (20.9 x 10.6 inch).
Due to the hot acid vapors generated, the microwave oven and the gas scrubber
system must be set up under a vent hood or other exhaust system. The exhaust
chamber must always remain securely closed during the entire evaporating process.
Gas scrubber
62
As illustrated in the figures below, add marble granulate to 2 of the gas scrubber
bottles (fill each approx. half-way) while filling the third bottle with NaOH solution
(at least 0.5 mol/l NaOH). Connect the bottles as illustrated in the figures and place
the bottles filled with marble granulate in the cooler. Connect the cooler to a coolant water system with a maximum water temperature of 20°C (68°F). The coolant
water flowrate must be approx. 0.5 liters/min.
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Berghof Products + Instruments
5.1.3.
Options
Operation
Warning !
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work which may
involve contact with chemicals, that is, when working with acids, pressure vessels,
during cleaning, etc.!
Lid replacement
DANGER !
After the samples have been digested and cooled in the microwave, they are
opened as described in the “Sample Removal” section. The lid for evaporating is
then screwed on.
Explosion hazard!
It is important that the lid with the rupture disc be removed for evaporating and that
it is never used for this procedure.
DAP-60+
DAK-100/4
Evaporating cap
Sample placement
Evaporating cap
Digestion lid
Place the vessels prepared for evaporating into the rotor. Any unused positions
must be sealed with blind stoppers. Then connect all vessels to the collection vessel.
Concentration must always be carried out with a fully filled rotor (8 vessels for
DAK-100/4 or 12 vessels for DAP-vessels).The sample volume must be nearly
equal in all vessels (e.g., 20 ml).
Gas scrubber
connection
EN_Options.doc
Close the microwave and connect the vent hose.
This connects the microwave to the gas scrubber. Check to make sure that sufficient coolant water is flowing at the gas scrubber (approx. 0.5 liters/min.).
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Options
Start the microwave
Berghof Products + Instruments
For fortification the magnetron temperature must be set to magT < 20°C in the
temperature program (typical values 5-10°C. The magnetron temperature is recorded continuously and is used to control the distillation process. The terminate
criterion is met if in step 5 the magnetron temperature rises by the specified value
compared to the temperature that arose in step 4.
The power specifications for step 4 and must be selected to be identical to obtain
an expedient terminate criterion. In steps 1-4 the microwave energy is not automatically cut off. The times these steps take depends on the total quantity of fluid
and must therefore be selected in such manner that the temperatures of all samples can stabilize. In step 5 the distillation process is stopped automatically as
soon as the terminate criterion is met. The entire control system is therefore independent of the type of acid.
Example
Start the microwave.
The samples are not evaporated until they are dry. As a rule, a residual volume of
1-2ml remains. In order to concentrate the sample still further, the times in step 1-4
must be increased.
Sample removal
The samples are removed as described in the “Sample Removal” section.
Maintenance
The evaporated acid is condensed and collected in the two gas scrubber bottles.
The acid is neutralized by the marble granulate. The liquid must be poured off as
soon as the gas scrubber bottles are approx. three-quarters full. The granulate can
continue to be used until it has gone completely into solution. The granulate can
neutralize approximately 2 liters of acid. A portion of the acid vapors are also concentrated in the rotor’s collection vessel. This liquid must be removed after every
fuming procedure (refer to the “Cleaning” section).
All TFM components must be cleaned with water and dried before they are again
used.
64
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Maintenance and Service
6.
Maintenance, Troubleshooting and Service
6.1.
Cleaning
DANGER !
Acid burn hazard!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for contact addresses).
Always wear safety glasses/goggles and protective gloves when working with the
pressure vessels!
Note any changes in the appearance of the pressure vessel which could indicate
possible material fatigue, e.g., deformation of the vessel, difficulty screwing on
lids, etc. even when the vessel is cold and not under pressure. All such vessels
should be immediately returned to Berghof Products + Instruments GmbH for inspection.
Warning !
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work which may
involve contact with chemicals, that is, when working with acids, pressure vessels,
during cleaning, etc.!
Oven chamber
The oven should be wiped out with a moist cloth at regular intervals as well as after
any rupture disc activation. All relevant safety measures should be observed in
case of contamination by acids, particularly hydrofluoric acid. Allow the oven to
thoroughly dry before again using it!
Display/Keyboard
Use only a dry cloth to wipe off the display and the keyboard.
Vessels
Since the vessels exhibit practically no memory effects it is generally sufficient to
thoroughly rinse out the vessels with distilled water after each digestion procedure
involving complete digestion.
If discoloration is noted or if carry-over is suspected, the vessels are cleaned by a
blank digestion using acid. In this case, the acid used for the particular application
is filled into the vessel, but no sample is added. After filling, the temperature program for the application in question is started.
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Maintenance and Service
Cap for pressure
control
Berghof Products + Instruments
From time to time the glass rings in the lids used to
measure pressure must be cleaned. This becomes
necessary when the signal from a given vessel significantly deviates from those from the other vessels.
To do this, first unscrew and remove the prism and
vent nipple and use the long, thin edge of the supplied
tool to push the TFM separating block out with the
long. All components can then be cleaned with water
and dried. Replace the silicon seals as required.
Reinstall the glass ring by laying it on the TFM separating block, then pushing the block into the lid. Using
the wide edge of the tool, which can be identified by
the two metal nipples, turn the separating block inside
the lid until the vent nipple can be screwed in.
Replace the polarisation foil at the prism and insert
prism again. Please observe correct orientation of the
prism.
Finally pressure measurement has to be aligned newly
(see chapter ´Alignement of pressure measurement´)
Cap for pressure control with
DAP-30/60/100+
Cap for pressure control with
DAP-40+
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Maintenance and Service
Cap for pressure control with
DAK-100/4
Rotor system
If a rupture disc has activated, perform the following procedure:
•
First, gases in the collecting system and hoses may be suctioned by connecting a acid-proofed pump to the exhaust tube (e.g. a water jet pump).
•
Remove all vessels from the rotor and open them as described in the
“Sample Removal” section.
•
Remove the collection system.
•
Rinse all components clean and allow them to dry.
•
Reinstall the rotor and the collection system.
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Maintenance and Service
6.2.
Berghof Products + Instruments
Maintenance
DANGER !
Acid burn hazard!
Use only digestion vessels and spare parts authorized by Berghof Products +
Instruments GmbH for use with the speedwave. These can be obtained either
from your local dealer or directly from Berghof Products + Instruments GmbH
(Refer to the “Repairs / Customer Service” section for contact addresses).
Always wear safety glasses/goggles and protective gloves when working with the
pressure vessels!
Note any changes in the appearance of the pressure vessel which could indicate
possible material fatigue, e.g., deformation of the vessel, difficulty screwing on
lids, etc. even when the vessel is cold and not under pressure. All such vessels
should be immediately returned to Berghof Products + Instruments GmbH for inspection.
Warning !
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work which may
involve contact with chemicals, that is, when working with acids, pressure vessels,
during cleaning, etc.!
Lip seal replacement
68
The lip seal on the collection system should be occasionally replaced. To do this, unscrew the pressure
screw in the collection vessel, replace the used lip
seal with a new one, then retighten the retaining
screw (hand-tighten only).
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6.3.
Maintenance and Service
Alignment of Pressure Measurement
Principle
Adjustment takes place according to the steam pressure curve of pure water
stored in the software.
Adjustment should be repeated
- Once a month,
- After the pressure gauge lid has been dismantled (cleaning).
Implementation
Each vessel is filled with 20 ml water and sealed by means of the adjustable pressure gauge lids.
Start the pressure adjust program from the operator library and follow the instructions in the program.
The pressure sensor is adjusted automatically.
Note:
Adjustment can be repeated any number of times with any number of vessels.
However, at least 2 vessels must be in the oven. If necessary a vessel without a
pressure gauge lid must be used as the second vessel.
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Maintenance and Service
6.4.
Berghof Products + Instruments
Output power measurement
Principle
The output power of the Magnetron has been thoroughly tested and certified by
Berghof Products + Instruments before it is delivered. However all Magnetrons are
subject to an aging process and it may become necessary to check the output
power. This is definitely advisable if the rate at which it heats becomes significantly slower.
To measure the output power 500 ml water is heated at full microwave power for
42 seconds and then the rise in temperature established. The output power can
be calculated from this.
Implementation
70
Start the power test program from the operator library and follow the instructions
in the program.
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Berghof Products + Instruments
Maintenance and Service
The output power should be at least 900 watts.
If values of less than 800 watts are determined, the Berghof Technical Support
should be contacted (refer to 'Repairs +Customer Service').
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Maintenance and Service
6.5.
Berghof Products + Instruments
Troubleshooting
Fault
Possible cause
Corrective action
Magnetron switches off
during digestion.
Magnetron overheated.
Insufficient liquid
Oven operated while empty.
Inform the Service Department!
The displayed temperature
is already in excess of 80° C immediately after the
program starts.
Faulty temperature measurement
Temperature sensor fault
Recalibrate the temperature offset.
Recalibrate the sensor.
Inform the Service Department!
Pressure reading too low or too
high
Realign pressure measurement
Check glass parts of cap
Microwave fails to start.
Faulty door interlock switch.
Door interlock has been
manipulated.
Inform the Service Department!
Rupture discs activate frequently.
Corroded rupture discs
Turntable not operating properly
Sample amount too large
Spontaneous reaction
Replace rupture discs more
frequently.
Check turntable operation.
Reduce the sample amount.
Lower the maximum temperature.
Rupture discs activate frequently.
Pressure reading too low
Realign pressure measurement
Check glass parts of cap
Oven chamber and, in particular,
the rotor become extremely hot.
Inadequate load
(at least 5ml per vessel required).
Use larger amounts of liquid
(at least 5 ml total).
Reduce total running time
(30 minutes max.).
Vessels leaking
Spread the lip seals on the lids
wider.
Replace any lids repaired with
PTFE seals with new lids.
Sparking in the oven
Inadequate load
(at least 5ml per vessel required).
Use larger amounts of liquid.
Lid jams during closing
Turntable not engaged correctly on Place the turntable correctly
drive axes
FI circuit breaker in the power
supply circuit trips frequently.
Faulty magnetron,
short-circuit in the unit
Inform the Service Department!
You can obtain technical support from your regional Berghof dealer or
directly from Berghof Products + Instruments GmbH by contacting:
Berghof Products + Instruments GmbH
Harretstr. 1
72800 Eningen / Germany
Phone: +49/(0)7121/894-202
Fax: +49/(0)7121/894-300
E-mail: [email protected]
Please provide your unit’s serial number with all repair questions or repair orders.
The serial number is located on the nameplate.
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6.6.
Maintenance and Service
Fuse Replacement
Unplug the power cord at the wall outlet. Unplug the fuse holder. The unit is protected by two 12.5 AT fuses. Always replace both fuses. Make sure the fuse holder
is oriented in the proper direction when reinstalling it!
If the fuses again trip after being replaced, please inform the Service Department.
Procedure
Remove the power cord. The mains plug and the fuse holder form a single unit
and are located on the right side of the device. The holder contains two fuses.
Using a screwdriver, turn the plastic screw counterclockwise until it pops out.
The fuse holder can now be removed for fuse replacement.
Insert a new fuse in the plastic screw and reinstall the screw in the fuse holder.
Use a screwdriver to tighten the screw by turning it clockwise.
Note:
Use only OEM fuses in accordance with the description below.
Fuse type
Size: 20 x 5mm; 250 VAC; 12.5 AT
Order no.: 5001091
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Maintenance and Service
6.7.
Berghof Products + Instruments
Repairs / Customer Service
DANGER !
The unit employs high voltage and generates microwave radiation!
Any repair and service work may only be performed by properly trained and qualified personnel.
Always unplug the unit from the power supply before beginning any repair or maintenance work.
The high voltage condenser may still carry a charge even after the mains power
plug has been pulled. It must therefore be discharged by bridging the terminals,
e.g., with a well insulated screwdriver. Make sure you are not in contact with any
metal while discharging.
Never alter the settings of the contact switches. However, should it be necessary
to do so, the proper function of the switches must be checked before the unit is
again taken into service. Proper switch function must then be confirmed by measuring the unit’s microwave leakage radiation. This value must lie below the limit
2
value of < 5 mW/cm .
You can obtain technical support and information regarding spare parts (order no.
and prices) from your regional Berghof dealer or directly from Berghof Products +
Instruments GmbH by contacting:
Berghof Products + Instruments GmbH
Harretstr. 1
72800 Eningen / Germany
Phone: +49/(0)7121/894-202
Fax: +49/(0)7121/894-300
E-mail: [email protected]
Please provide your unit’s serial number with all repair questions or repair orders.
The serial number is located on the nameplate.
6.8.
Nameplate
5. Model
1. Manufacturer and address
6. Supply voltage
2. a. CE designation
b. Microwave frequency
7. Serial number
8. Article number
3. Berghof part number
9. WEEE Registration No.
4. Barcode identification no.
10. Manufacturing date
74
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7.
Appendix
7.1.
Tips and Tricks
Appendix, Applications
Small sample quantities With the MT or quartz glass inserts small sample quantities <100mg can be digested in a reduced acid volume. This also makes it possible to enhance the detection sensitivity of the entire process.
Multiple samples
per vessel
Higher sample
throughput
Cooling down samples
EN_Appendix_Applications.doc
The MT system makes it possible for 2-3 samples to be digested in a single DAP
100+ or DAK-100/4 digestion vessel at a reduced original sample weight and acid
volume. This enables the sample throughput and productivity of the speedwave
four to be raised.
Cross-contamination from one sample to another is prevented by pre-filling the
same acid mixture into the outer vessel as in the inner vessel. If the acid volume on
the outside is selected so that the liquid level is higher than in the MT vessel, this
also guarantees that the sample is heated up gently.
The sample throughput can also be increased by removing the vessels from the
speedwave four approximately 5 minutes after completion of the last heating stage
and replacing them with new samples. Therefore no time is wasted on cooling
down the samples and idle time in the microwave is restricted to a minimum.
As a rule, the samples cool down in 15-20 min. to the point at which they can be
opened. However, the cooling-down time can reduced to 5-10 min. if the digestion
vessels are placed in a water bath containing cold water.
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Appendix, Applications
Dilating sealing lips
Stainless steel
rupture disk
TFM rupture disks
Berghof Products + Instruments
The sealing lips of maximally 6 caps can be dilated fast and simply in the 6-fold dilation tool.
For specific applications Berghof offers stainless steel rupture disks to be used with
the DAP-60+ vessels. Applications are, for example, the digestion of ROHs samples or plastic materials up to 250 mg original sample weight
For specific applications Berghof offers TFM caps with the DAP-60+ and DAP100+
vessels, which are used without additional metallic rupture disks. Potential applications are, for example, digestions for ultra-trace analytics such as those performed
in the semiconductor industry.
When using these TFM caps/rupture disks it must be borne in mind that the rupture
pressure depends on the temperature and the time digestion takes. The reason for
this is the reduced strength of the TFM material at higher temperatures. Metallic
rupture disks do not demonstrate this dependency in the temperature range
< 300°C, which is why it the standard rupture disks used at Berghof are metallic
ones.
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7.2.
Appendix, Applications
Applications
The data listed below are only to be viewed as reference values. Basically, the reaction progression depends on a series of not always predictable factors (distribution of the substances, surface area, catalytic effects of additives), so that spontaneous reactions may occur and result in activation of the rupture disc.
All applications are also available as individual documents. Please contact your
local, authorized dealer or Berghof Products + Instruments GmbH (refer to the
“Repairs / Customer Service” section for contact addresses).
Sample
α−Al2O3
Weight
Vessel
Acid
200 mg DAC-17
Activated Carbon
50 mg DAP-60+
Al2O3 + TiC
10 mg DAC-17
Al2O3
200 mg DAP-30+
DAK-100/4
Al2O3 95%
HCl, H2SO4,
HF, HNO3
Temp.
Time
File
280 °C 55 min
MWS-a-Al2O3.pdf
220 °C 45 min
MWSActivated_Carbon.pdf
HNO3, HF, HCl, 280 °C 50 min
H2SO4
MWS-Al2O3-TiC.pdf
HNO3
HNO3, HF
270 °C 60 min
MWS-Al2O3.pdf
200 mg DAP-60+
H3PO4,
H2SO4, HF
240 °C 20 min
MWS-Al2O3 95%.pdf
Alloy Cr-Mo-Co
100 mg DAP-60+
HNO3, HCl,
NH4F
200 °C 30 min
Alloy Cr-Mo-Ni
100 mg DAP-60+
HNO3, HCl
200 °C 30 min
MWS-Cr-Mo-Ni-Alloy.pdf
Alloy Cr-Ni-Pd
100 mg DAP-60+
HNO3, HCl,
NH4F
200 °C 30 min
MWS-Cr-Ni-Pd-Alloy.pdf
Alloy Cr-W-Co
100 mg DAP-60+
HCl
200 °C 30 min
MWS-Cr-W-Co-Alloy.pdf
MWS-Cr-Mo-CoAlloy.pdf
Alloy Fe-Nb
50 mg DAP-60+
HCl, HF, HNO3
240 °C 35 min
MWS-Fe-Nb-Alloy.pdf
Alloy Fe-Ti
50 mg DAP-60+
HCl, HF, HNO3
220 °C 45 min
MWS-Fe-Ti-Alloy.pdf
Alloy Pt-Ir
50 mg DAK-100/4
HNO3, HCl
200 °C 45 min
MWS-Pt-Ir-Alloy.pdf
Alloy Rh-Ir
300 mg DAK-100/4
HCl, H2O2,
H2SO4
250 °C 65 min
MWS-Rh-Ir-Alloy.pdf
Alloys Pt-Ir
100 mg DAK-100/4
HCl, HNO3, Br2 210 °C 45 min
MWS-Pt-Ir-Alloys.pdf
Aluminium
150 mg DAP-60+
HNO3, HCl
175 °C 20 min
MWS-Aluminium.pdf
Ash
200 mg DAP-60+
HNO3, HF
200 °C 45 min
MWS-Ash-B.pdf
Ash
300 mg DAP-60+
HNO3, HF, HCl
220 °C 33 min
MWS-Ash-A.pdf
Asphaltite
200 mg DAK-100/4
HNO3, HF
200 °C 75 min
MWS-Asphaltite.pdf
EN_Appendix_Applications.doc
speedwave_four_EN-Version1_0.doc
77
Appendix, Applications
Sample
Vessel
Acid
Temp.
Time
File
Bakelite
500 mg DAP-60+
HNO3, HCl
180 °C 35 min
MWS-Bakelite.pdf
Bark
500 mg DAP-60+
HNO3, HCl
200 °C 35 min
MWS-Bark.pdf
Bauxite
50 mg DAP-60+
HNO3, H3PO4,
HCl
250 °C 50 min
MWS-Bauxite.pdf
300 mg DAP-60+
HNO3, H2O2
190 °C 25 min
MWS-Beet-Roots.pdf
2 ml DAP-60+
/DAQ-20
HNO3
190 °C 15 min
MWS-Blood.pdf
Body Lotion
300 mg DAP-60+
HNO3
190 °C 35 min
MWS-Body Lotion.pdf
Bones
300 mg DAP-60+
HNO3, HCl
190 °C 30 min
MWS-Bone.pdf
Boron Carbide B4C
100 mg DAK-100/4
HNO3, HF,
H2SO4
220 °C 30 min
MWS-B4C.pdf
Bran
400 mg DAP-60+
HNO3, H2O2
190 °C 20 min
MWS-Bran.pdf
Brass
100 mg DAP-60+
HNO3
210 °C 30 min
MWS-Brass-B.pdf
Brass
100 mg DAP-60+
HNO3, HF
180 °C 30 min
MWS-Brass-A.pdf
Bronze
100 mg DAP-60+
HNO3, HF
180 °C 30 min
MWS-Bronze-A.pdf
Bronze
100 mg DAP-60+
HNO3
210 °C 30 min
MWS-Bronze-B.pdf
Cacao
300 mg DAP-60+
HNO3, H2O2
190 °C 25 min
MWS-Cacao.pdf
Calcites+Dolomite
100 mg DAP-60+
HNO3, HF
200 °C 45 min
Caoutchouc
250 mg DAP-60+
HNO3
200 °C 60 min
MWS-Caoutchouc.pdf
Car Catalyst
50 mg DAP-30+
HCl, H3PO4
260 °C 45 min
MWS-Car-Catalyst.pdf
Beet Roots
Blood
78
Weight
Berghof Products + Instruments
MWS-CalciteDolomite.pdf
Catalyst
150 mg DAK-100/4
HNO3, HCl, HF
220° C 60 min
MWS-Catalyst.pdf
Cement
300 mg DAP-60+
HNO3, HCl, HF
210 °C 15 min
MWS-Cement.pdf
Cigarette
300 mg DAP-60+
HNO3, HCl
210 °C 25 min
MWS-Cigarette.pdf
Clay
100 mg DAP-60+
HNO3, HF
210 °C 30 min
MWS-Clay.pdf
Coal
150 mg DAP-60+
HNO3, HF
200 °C 20 min
MWS-Coal.pdf
Coal
400 mg DAK-100/4
HNO3, HF
200 °C 70 min
MWS-Coal-B.pdf
Coal Fly Ash
250 mg DAK-100/4
HNO3, HF
200 °C 35 min
MWS-Coal-Fly-Ash.pdf
Cobalt Tungstate
100 mg DAP-60+
HNO3, HF
240 °C 65 min
MWS-Cobalt Tungsta-
speedwave_four_EN-Version1_0.doc
EN_Appendix_Applications.doc
Berghof Products + Instruments
Sample
Weight
Vessel
Appendix, Applications
Acid
Temp.
Time
File
te.pdf
Coffee
400 mg DAP-60+
HNO3, H2O2
180 °C 15 min
MWS-Coffee-B.pdf
Coffee
300 mg DAP-60+
HNO3
200 °C 12 min
MWS-Coffee-A.pdf
HNO3, H2O2
160 °C 20 min
MWS-Cognac.pdf
Cognac
500 µl DAP-60+
Coke
100 mg DAC-17
HNO3, H2SO4
260 °C 40 min
MWS-Coke.pdf
Copper Wire
500 mg DAK-100/4
HNO3
190 °C 20 min
MWS-Copper-wire.pdf
100 mg DAP-60+
HNO3, HF
200 °C 45 min
Dried Plants
300 mg DAP-60+
H2SO4, H2O2
190 °C 10 min
MWS-Plants-C.pdf
Dried Plants
400 mg DAP-60+
HNO3
190 °C 15 min
MWS-Plants-A.pdf
Electronic Parts
500 mg DAP-60+
HNO3, H2SO4
175 °C 20 min
EVA Foam
400 mg DAK-100/4
HNO3
190 °C 20 min
MWS-EVA-Foam.pdf
EVOH ethylene vi500 mg DAK-100/4
nyl alcohol copolymer
resins
HNO3
180 °C 15 min
MWS-EVOH.pdf
Dolomites + Calcites
MWS-CalciteDolomite.pdf
MWS-electronic
parts.pdf
Face Creme
250 mg DAP-60+
DAQ-20H
HNO3
190 °C 35 min
MWS-Face Creme.pdf
Feldspar
250 mg DAK-100/4
HCl, HF,
H3BO3
200 °C 35 min
MWS-Feldspar.pdf
Flour
400 mg DAP-60+
HNO3, H2O2
190 °C 20 min
MWS-Farine.pdf
200 mg DAP-60+
HNO3, H2O2
170 °C 15 min
Feed
300 mg DAP-60+
HNO3, HBF4
215 °C 15 min
MWS-Feed-B.pdf
Feed
300 mg DAP-60+
HNO3
230 °C 15 min
MWS-Feed-A.pdf
Fishmeal
500 mg DAP-60+
HNO3, H2O2
200 °C 40 min
MWS-Fishmeal.pdf
220 °C 40 min
MWS-Fly-Ash.pdf
HNO3
190 °C 25 min
MWS-DAP-40-Food.pdf
HNO3, H2O2
200 °C 25 min
MWS-Fruite-Juice.pdf
HNO3, H2O2
210 °C 25 min
MWS-Fruits.pdf
Fatty Acid of Coconut
Fly Ash
Food
50 mg MT
500 mg DAP-40+
Fruite Juices
Fruites (dried)
HNO3, HF,
H2SO4
5 ml DAP-100+
250 mg DAP-60+
EN_Appendix_Applications.doc
speedwave_four_EN-Version1_0.doc
MWS-Coconut Fat Acid.pdf
79
Appendix, Applications
Sample
Weight
Berghof Products + Instruments
Vessel
Acid
Temp.
Time
File
Garnet
100 mg DAP-60+
HNO3, HF,
H3BO3
245 °C 45 min
MWS-Garnet.pdf
Gas Coal
150 mg DAK-100/4
HNO3, HF,
H3BO3
200 °C 35 min
MWS-Gas-Coal.pdf
Gingseng
500 mg DAP-60+
HNO3, H2O2
190 °C 30 min
MWS-Gingseng.pdf
Grab paste
300 mg DAP-60+
HNO3, H2O2
190 °C 30 min
MWS-Grab_Paste.pdf
Hair
250 mg DAP-60+
DAQ-20
HNO3
190 °C 20 min
MWS-Hair.pdf
Hardmetal Scrap
100 mg DAP-60+
HNO3, HF
240 °C 65 min
Herbs
500 mg DAK-100/4
HNO3, H2O2
210 °C 30 min
MWS-Herbs.pdf
Ink
250 mg DAP-60+
HNO3
200 °C 30 min
MWS-Ink.pdf
In-Sn-Oxides
500 mg DAP-60+
HCl, HF,
H3BO3
190 °C 25 min
MWS-In-Sn-Oxide.pdf
Ionomer
100 mg DAP-60+
HNO3
190 °C 35 min
MWS-Ionomer.pdf
Iron Ores
100 mg DAP-60+
240 °C 30 min
MWS-Iron-Ores.pdf
Ironstone
100 mg DAP-60+
HNO3, HCl
220 °C 50 min
MWS-Ironstone.pdf
Kaolinit
100 mg DAP-60+
H2SO4, HF
240 °C 50 min
MWS-Kaolinit.pdf
LaB6 Lanthanium
boride
200 mg DAK-100/4
HNO3
230 °C 10 min
MWS-LaB6.pdf
Laboratory Dust
75 mg DAP-60+
HNO3, HF
200 °C 15 min
MWS-Dust.pdf
Lead Zirconate Titanate
100 mg DAP-60+
HNO3, HF
240 °C 65 min
Lime
300 mg DAP-60+
HNO3, H2O2
190 °C 20 min
MWS-Lime.pdf
Limestone
150 mg DAK-100/4
HCl, HF
220 °C 20 min
MWS-Limestone.pdf
Line Seed
500 mg DAP-60+
HNO3, H2O2
190 °C 15 min
MWS-Line-Seed-A.pdf
Line Seed
400 mg DAP-60+
HNO3, H2O2
180 °C 15 min
MWS-Line-Seed-B.pdf
Lipstick
250 mg DAP-60+
HNO3, HF
190 °C 35 min
MWS-Lipstick.pdf
Lithium Titanates
100 mg DAP-60+
HNO3, HF
200 °C 35 min
MWSLithiumTitanate.pdf
80
H2SO4,
H3PO4, HF
speedwave_four_EN-Version1_0.doc
MWS-Hardmetal Scrappdf
MWSLeadZirconateTitanate.pdf
EN_Appendix_Applications.doc
Berghof Products + Instruments
Sample
Weight
Vessel
Appendix, Applications
Acid
Temp.
Time
File
Milk Powder
500 mg DAP-60+
HNO3, H2O2
190 °C 30 min
MWS-Milk-Powder-D.pdf
Milk Powder
200 mg DAP-60+
HNO3
200 °C 30 min
MWS-Milk-Powder-A.pdf
Monomer
500 mg DAP-60+
HNO3, H2O2
200 °C 35 min
MWS-Monomer.pdf
1,000 DAP-60+
mg
HNO3, H2O2
170 °C 25 min
MWS-Muffin.pdf
1,000 DAK-100/4
mg
HNO3, H2O2
210 °C 50 min
MWS-MultiitaminTablets.pdf
200 mg DAP-60+
HNO3, HF
245 °C 25 min
MWS-NbS2.pdf
50 mg DAP-60+
HNO3, HF
200 °C 45 min
MWS-Nist-1633.pdf
Muffins
Multivitamin and
Multielement Tablets
Niobiumdisulfide
NIST 1633
Nylon
400 mg DAK-100/4
HNO3, H2SO4
190 °C 35 min
MWS-Nylon.pdf
Oils
100 mg DAP-60+
HNO3, HCl, HF
180 °C 30 min
MWS-Oil-B.pdf
Oils
100 mg DAP-60+
HNO3, HF
190 °C 35 min
MWS-Oil-A.pdf
Olive Leaves
500 mg DAP-60+
HNO3, H2O2
190 °C 30 min
MWS-Olive Leave.pdf
Vegetable Oil
700 mg DAK-100/4
HNO3, H2O2
210 °C 30 min
MWS-Vegetable-Oil.pdf
Paint
0,75 ml DAK-100/4
HNO3, H2O2
190 °C 35 min
MWS-Paint.pdf
Palmnut Flakes
300 mg DAP-60+
HNO3, H2O2
190 °C 25 min
MWS-PalmnutFlakes.pdf
Paprika Powder
300 mg DAP-60+
HNO3, H2O2
180 °C 15 min
MWS-Paprika-B.pdf
Paprika Powder
300 mg DAP-60+
HNO3
200 °C 15 min
MWS-Paprika-A.pdf
PEEK
100 mg DAP-60+
HNO3, H2SO4
220 °C 15 min
MWS-PEEK.pdf
PET
250 mg DAP-60+
HNO3, H2SO4
220 °C 35 min
MWS-PET-C.pdf
PET
150 mg DAP-60+
HNO3, H2SO4
225 °C 45 min
MWS-PET-B.pdf
Petrol Coke
300 mg DAK-100/4
HNO3, H2SO4,
HF
250 °C 70 min
MWS-Petrolcoke.pdf
Pharma Raw Materials
250 mg DAK-100/4
HNO3
210 °C 30 min
MWS-Raw-MaterialsPharma.pdf
Pharma Raw Materials
250 mg DAK-100/4
HNO3, H2O2
210 °C 30 min
MWS-Raw-MaterialsPharma-B.pdf
220 °C 25 min
MWSPhosphate_rock.pdf
Phosphate Rocks
200 mg DAP-60+
EN_Appendix_Applications.doc
HNO3, HF,
H3BO3
speedwave_four_EN-Version1_0.doc
81
Appendix, Applications
Sample
Platinum Ores
Weight
Berghof Products + Instruments
Vessel
Acid
Temp.
Time
File
50 mg DAP-60+
HNO3, H2SO4,
H3PO4, HF
240 °C 65 min
MWS-Platimum Ore.pdf
Polyester
250 mg DAP-60+
HNO3, H2SO4
215 °C 40 min
MWS-Polyester-A.pdf
Polyethylene PE
150 mg DAP-60+
HNO3, H2SO4
220 °C 45 min
MWS-PE-A.pdf
Polyethylene PE
300 mg DAP-60+
HNO3, HCl
220 °C 40 min
MWS-PE-B.pdf
Polyethylene PE
(Film)
200 mg DAP-60+
HNO3, HF
170 °C 40 min
MWS-PE-Film.pdf
Polypropylene PP
250 mg DAP-60+
HNO3, H2SO4
200 °C 30 min
MWS-PP-A.pdf
PVC-Granules
750 mg DAK-100/4
210 °C 50 min
MWS-PVC-B.pdf
Quartz and Glass
500 mg DAP-60+
HNO3, HF
200 °C 30 min
MWS-Glass-QuartzA.pdf
Quartz and Glass
500 mg DAP-60+
HNO3, HF,
HBF4
200 °C 30 min
MWS-Glass-QuartzB.pdf
Refractory Material
100 mg DAP-60+
H3PO4,
H2SO4, HF,
HNO3
240 °C 30 min
MWS-Cr2O3-FeOAl2O3.pdf
Refractory Material
100 mg DAP-60+
H3PO4,
H2SO4, HF
240 °C 75 min
Rhodium
100 mg DAK-100/4
Rice
82
1,000 DAP-60+
mg
Rubber
250 mg DAP-60+
Secondary Fuel
200 mg DAK-100/4
HNO3, H2O2,
H2SO4
MWS-Refractory.pdf
HCl, HNO3, Br2 210 °C 45 min
MWS-Rh.pdf
HNO3, H2O2
180 °C 30 min
MWS-Rice.pdf
HNO3
200 °C 60 min
MWS-Rubber.pdf
HNO3, H2SO4,
HF
250 °C 70 min
MWS-Secondary
fuel.pdf
Sediment
1,000 DAP-60+
mg
HNO3, HCl, HF
175 °C 30 min
MWS-Sediment-D.pdf
Sediment
1,000 DAP-60+
mg
HNO3, HCl
175 °C 10 min
MWS-Sediment-E.pdf
Sediment
1,000 DAP-60+
mg
HNO3, HF
175 °C 30 min
MWS-Sediment-A.pdf
Sewage Sludge
500 mg DAP-100+
HNO3, HCl, HF
175 °C 30 min
MWS-Sludge-F.pdf
Sewage Sludge
500 mg DAP-100+
HNO3, HCl
175 °C 30 min
MWS-Sludge-E.pdf
Sewage Sludge
500 mg DAP-100+
HNO3, HF
175 °C 30 min
MWS-Sludge-D.pdf
speedwave_four_EN-Version1_0.doc
EN_Appendix_Applications.doc
Berghof Products + Instruments
Sample
Weight
Vessel
Appendix, Applications
Acid
Temp.
Time
File
Sewage Sludge
500 mg DAK-100/4
HNO3
180 °C 40 min
MWS-Sludge-B.pdf
Sewage Sludge
250 mg DAP-100+
HNO3
180 °C 40 min
MWS-Sludge-A.pdf
Shampoo
300 mg DAP-60+
HNO3
190 °C 35 min
MWS-Shampoo.pdf
Shoe Sole
200 mg DAP-60+
HNO3, HF
220 °C 30 min
MWS-Shoe-sole.pdf
Shredded Paper
500 mg DAP-60+
HNO3
170 °C 10 min
MWS-Paper.pdf
Silicon
300 mg DAP-60+
HNO3, HF
185 °C 10 min
MWS-Silicon.pdf
50 mg DAC-17
HNO3, HF,
H2SO4
290 °C 70 min
MWS-SiC.pdf
100 mg DAP-60+
H3PO4,
H2SO4, HF,
HNO3
240 °C 30 min
MWS-SiO2-Al2O3.pdf
SiO2 + Al2O3 +
B2O3
100 mg DAP-30+
DAK-100/4
HF, H3PO4,
HCl
250 °C 25 min
MWS-SiAlB-Oxide.pdf
SiO2 + Al2O3 +
ZrO2
150 mg DAP-30+
DAK-100/4
HF, H3PO4,
HCl
240 °C 25 min
MWS-SiAlZr-Oxide.pdf
Slag (Blast Furnace)
100 mg DAP-60+
HNO3, HF
200 °C 45 min
MWS-Slag-BlastFurnace.pdf
Slag (Electric Furnace)
100 mg DAP-60+
H3PO4,
H2SO4, HF
240 °C 75 min
MWS-Slag-ElectricFurnace.pdf
Slag + Fly Ash
100 mg DAP-60+
HNO3, HF
240 °C 65 min
MWS-Slag + Fly Ash.pdf
Soap
250 mg DAP-60+
HNO3, HF
190 °C 35 min
MWS-Soap.pdf
Silicon Carbide SiC
SiO2 + Al2O3
Soil
4,000 DAP-100+
mg
HNO3, HF
175 °C 20 min
Soil
4,000 DAP-100+
mg
HNO3, HCl
180 °C 25 min
MWS-Soil-A.pdf
Soil
1,000 DAP-100+
mg
HNO3, HCl
140 °C 15 min
MWS-Soil-B.pdf
600 mg DAK-100/4
HNO3, H2O2
190 °C 25 min
MWS-Sugar-B.pdf
350 mg DAP-30+
DAK-100/4
HNO3, HF, HCl
220 °C 25 min
Talcum Powder
250 mg DAK-100/4
HNO3, HF
210 °C 35 min
MWS-Talcum.pdf
Tar
500 mg DAK-100/4
HNO3
210 °C 30 min
MWS-Tar-pdf
Tea
500 mg DAK-100/4
HNO3
190 °C 40 min
MWS-Tea.pdf
Sugar
Sun Protection
Creme
EN_Appendix_Applications.doc
speedwave_four_EN-Version1_0.doc
MWS-SoilEPA3051A.pdf
MWSSunProtectionCreme.pdf
83
Appendix, Applications
Sample
Textiles
Vessel
Acid
Temp.
Time
File
300 mg DAP-60+
HNO3
190 °C 15 min
MWS-Textiles.pdf
100 mg DAK-100/4
HNO3, HCl, HF
230 °C 30 min
MWS-TiB2-pdf
Tinctures
500 mg DAP-60+
HNO3, H2O2
190 °C 30 min
MWS-Tinctures.pdf
Tire body
200 mg DAP-60+
HNO3
230 °C 55 min
MWS-Tire-Body.pdf
Tissue
250 mg DAP-60+
DAQ-20
HNO3
190 °C 20 min
MWS-Tissue.pdf
Titanium Carbide
200 mg DAK-100/4
HNO3, HF
245 °C 25 min
MWS-TiC-A.pdf
Titanium Carbide
200 mg DAK-100/4
HNO3, H2SO4
190 °C 25 min
MWS-TiC-B.pdf
Titanium Disulfide
200 mg DAK-100/4
HNO3, HF
245 °C 25 min
MWS-TiS2.pdf
Tomato Leaves
500 mg DAP-60+
HNO3, H2O2
190 °C 30 min
MWS-Tomato-LeavesB.pdf
Toothpaste
250 mg DAP-60+
HNO3, HF
190 °C 35 min
MWS-Toothpaste.pdf
Tungsten
300 mg DAK-100/4
HNO3, HCl, HF
250 °C 60 min
MWS-tungsten.pdf
Vanilla Dessert
400 mg DAP-60+
HNO3
200 °C 15 min
Vegetables
400 mg DAP-60+
HNO3, H2O2
200 °C 25 min
MWS-Vegetables.pdf
200 °C 20 min
MWS-Effluents-P.pdf
TiB2 Titanium Boride
30 ml DAP-100+
Water, Effluents
30 ml DAP-100+
HNO3, H2O2
200 °C 20 min
MWS-Effluents-HMA.pdf
Water, Effluents
30 ml DAP-100+
HNO3, HCl
180 °C 25 min
MWS-Effluents-HMB.pdf
Water, Effluents
20 ml DAP-100+
NaOH, K2S2O8 200 °C 20 min
MWS-Water-P-N.pdf
HNO3
240 °C 30 min
MWS-Wax.pdf
HNO3, HF,
H3BO3
180 °C 35 min
MWS-glass-filters.pdf
HNO3, HCl
200 °C 20 min
MWS-VesselCleaning.pdf
250 °C
MWS-vesselconditioning.pdf
Glass Fiber Filters
(Whatman 934H)
300 mg DAP-60+
DAP-100+
Vessel Cleaning
all types
Vessel Conditioning
all types
Wheat
1,000 DAP-60+
mg
H2SO4,
K2S2O8
MWS-VanillaDessert.pdf
Water, Effluents
Wax
84
Weight
Berghof Products + Instruments
HNO3, H2O2
12 h
170 °C 25 min
speedwave_four_EN-Version1_0.doc
MWS-Wheat.pdf
EN_Appendix_Applications.doc
Berghof Products + Instruments
Sample
Weight
Vessel
Appendix, Applications
Acid
Temp.
Time
File
Whey-Powder
500 mg DAK-100/4
HNO3, H2O2
210 °C 30 min
MWS-Whey-Powder.pdf
WO3
600 mg DAK-100/4
HNO3, HF
175 °C 35 min
MWS-WO3.pdf
Wood
600 mg DAP-60+
HNO3
150 °C 15 min
MWS-Wood-A.pdf
Wood chips
500 mg DAK-100/4
HNO3, HF
200 °C 30 min
MWS-Wood-B.pdf
Yogurt
500 mg DAK-100/4
HNO3, HCl
190 °C 25 min
MWS-yogurt.pdf
Zeolites
100 mg DAP-60+
HNO3, HCl, HF
240 °C 20 min
MWS-Zeolite.pdf
Zinc Oxide
500 mg DAP-60+
HNO3, HF
210 °C 30 min
MWS-Zinc Oxide.pdf
EN_Appendix_Applications.doc
speedwave_four_EN-Version1_0.doc
85
Appendix, Applications
7.2.1.
Berghof Products + Instruments
Positioning of Vessels in the Turntable
In the followingfigures the optimal positioning of the vessels in the rotor is illustrated.
DAP-Vessels
Sample
number
Position in rotor
2
12 1
3
9
7
6
12 1
2
11
4
7
6
12 1
2
11
7
6
12 1
2
11
7
6
12 1
2
11
7
7
6
12 1
2
11
12 1
2
3
4
5
11
7
6
12 1
2
11
3
4
10
9
5
8
12
7
6
12 1
2
11
3
4
10
5
9
8
7
6
3
4
10
9
5
8
86
6
8
5
8
7
9
4
9
4
5
10
3
10
3
11
5
8
6
10
4
9
2
8
3
10
12 1
9
5
8
6
10
4
9
7
11
3
10
5
9
5
8
4
5
8
4
9
3
9
3
10
2
10
5
8
12 1
11
4
10
Position in rotor
8
2
11
3
Sample
number
7
6
speedwave_four_EN-Version1_0.doc
EN_Appendix_Applications.doc
Berghof Products + Instruments
DAC-100 vessels
Sample
number
Appendix, Applications
Position in rotor
2
Position in rotor
6
1
8
Sample
number
1
2
7
8
3
4
6
3
5
7
1
8
2
6
4
7
3
1
8
2
6
4
7
3
5
4
5
8
1
8
2
6
4
7
3
5
5
4
6
5
3
2
7
1
8
2
6
4
7
3
5
1
8
2
7
3
4
6
5
EN_Appendix_Applications.doc
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87
Appendix, Applications
7.3.
88
Berghof Products + Instruments
Conformity Declaration
speedwave_four_EN-Version1_0.doc
EN_Appendix_Applications.doc
Berghof Products + Instruments
7.4.
Appendix, Applications
Conversion Table
Temperature
°C =
°F =
(°F – 32°) / 1.8
1.8 * °C +32°
Length
1 cm =
1 inch =
0.3937 inch
2.540 cm
Volume
1 ml =
3
1 inch =
1 gallon =
0.06102 inch
16.387 ml
3785 ml
= 2.642*10 gallon
-4
= 43.29*10 gallon
3
= 231 inch
Pressure
1 bar =
1 psi =
1 Mpa =
14.504 psi
0.06895 bar
10 bar
= 0.1 Mpa
= 0.0068948 Mpa
= 145.04 psi
Weight
1 kg =
1 lb. =
2.2046 lb.
0.4536 kg
EN_Appendix_Applications.doc
3
-4
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89