CEM iPrep, iPrep 12, iPrep 16 Series Manual
iPrep
®
High Performance Vessels
Manual
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Contents
Safety Notations
Safety Notations 1
Introduction
About the iPrep Vessels 2
Important Safeguards
Operating Parameters 3
Sample Preparation Safeguards 3
Vessel Safeguards 4
Microwave Safeguards 4
Compounds Unsuitable for Closed Vessel Microwave
Digestion 5
Vessel and Accessories Overview
Vessel Components 6
Accessories 7
New Liner and Plug Conditioning
Routine Maintenance
After Every Use 22
Monthly 22
Annually 22
Bake-out Procedure 22
Troubleshooting
Problems and Possible Solutions 23
Nitric Acid Liner and Plug Conditioning 8
Non-Nitric Acid Liner and Plug Conditioning 9
Perform a Digestion
Vessel Assembly 10
Turntable Setup 13
Load and perform a Method 14
Vessel Removal 14
Vessel Cleaning and Inspection
Liners and Plugs 17
Liner and plug Bake-out Procedure 17
Turntable, Frame, Load Disc, Screw & Racks 18
Sleeves 18
Vessel Distribution
12 Place Turntable 19
16 Place Turntable 20
Methods
Create a One Touch Method 21
Create a Classic Method 21
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Safety Notations
Safety Notations
This manual uses three safety alert words at points in the documentation where the user should be aware of
potential hazards. The safety alerts are shown in color-coded boxes. The three words–NOTE, CAUTION, and
WARNING–indicate differing levels of observation or action as described below:
NOTE
A NOTE is intended to provide emphasis of procedures that may be misinterpreted or overlooked, or to
otherwise clarify confusing situations.
CAUTION
A CAUTION is intended to provide essential information and to emphasize procedures which, if not strictly
followed, may result in improper instrument operation.
WARNING
A WARNING is intended to emphasize dangerous or hazardous conditions which may result in personal
injury to the user and damage the instrument.
1Safety Notations
Introduction
About the iPrep Vessels
The iPrep vessel is designed for microwave digestion in a MARS 6
is well suited for digestion of difcult matrices such as waste oils, APIs with multiple aromatic rings, polymers, and
geological samples. This vessel is also a great option when digesting 1 g or larger samples due to ppt detection
limit needs. Preinstalled methods take the guesswork out of method creation and sample preparation.
The MARS 6 requires the iWave temperature control with software version 1.43 or higher to operate iPrep vessels.
This Manual should be used in conjunction with the MARS 6 iWave Manual, PN 600832. Read and fully
understand all documentation before operating the instrument.
TM
with iWave®temperature control. This vessel
2 Introduction
Important Safeguards
Microwave sample preparation imposes a unique set of safety considerations beyond the basics of good laboratory
practice. Additional Safeguards for the MARS 6 instrument are included in the manual, PN 600832. General
guidelines for safe operation of the iPrep are presented below and all specic safety messages are located
throughout the manual.
Proper precautions must be taken to avoid contact with reagents or reagent vapors. Protective gear should be worn
as outlined in the user’s safety program for hazardous materials and the reagent manufacturer’s safety data sheet.
Refer to these guidelines for proper handling and disposal of the reagents.
Operating Parameters
iPrep 12 iPrep 16
iPrep Parameters Minimum Volume 5 mL 5 mL
Maximum Volume 30 mL 30 mL
Maximum Pressure 1500 psi 1500 psi
Maximum Hold Time 45 min 45 min
Maximum Temperature Maximum Programmable Temperature 300 ºC 300 ºC
Nitric Acid 250 ºC 250 ºC
Hydrochloric Acid* 250 ºC 250 ºC
Hydrouoric Acid* 250 ºC 250 ºC
Sulfuric Acid 300 ºC 300 ºC
Phosphoric Acid 300 ºC 300 ºC
Aqua Regia* 250 ºC 230 ºC
Water 180 ºC 180 ºC
Maximum Sample Weight Food, Plant, and Animal Tissue 1.5 g 1.5 g
Oil and Plastic 0.5 g 0.5 g
Pharmaceutical 1.5 g 1.5 g
Inorganic 1.5 g 1.5 g
Metallurgical 1.5 g 1.5 g
Clinical 1.5 g 1.5 g
* The maximum achievable temperature is 210 °C if running more than 6 vessels.
Sample Preparation Safeguards
• Do not use water to dilute the acid(s) greater than 25% when running over 220 ºC or to add volume before
digestion. This can cause uneven heating of vessels
• Run similar sample types with the same acid(s) and acid volume in each vessel
• Optimal Sample Volume is 10mL and will result in more even heating
• Minimum acid volume is 5 mL
• Maximum volume is 30 mL
• Maximum sample weight varies per sample type. See "Operating Parameters" for weights
• Acid blanks cannot account for more than 25% of turntable when mixed with samples
• Acid blanks cannot be run with organic samples > 230 °C
• Acid blanks cannot be run with samples when acid mixtures are > 50% hydrouoric acid. Acid blanks must
be run separately
3Important Safeguards
Vessel Safeguards
• Only use vessels and vessel components purchased directly from CEM or through its authorized dealer
network.
• All vessel components must be dry prior to use
• Always condition new liners and plugs
• Do not batch old liners with new liners unless new liners have been conditioned with at least 3 runs using
the customer’s sample
• Ensure vessels are assembled properly
• Align tab on load disc in center notch of liner
• Look for vent hole through the frame
• Align liner properly on insulator disc at bottom – liner ush with tab
• Use torque block
• Invert sleeves after every run to extend lifetime and promote better sealing & even heating
• Slide liner into the end of the sleeve with most resistance felt if unsure which side was previously
used
• CEM recommends using a high temperature pen to mark sleeves for a visual reference.
• Try to group liners with similar sample history and usage
• Segregate liners for HNO3 and non-HNO3 applications
• Do not use a new liner with a set of liners that has been run consistently until the new liner has
been conditioned with that sample type
• Pull ones that run 20 ºC hotter than average and run them together
• Bake out liners and plugs to remove residual HNO3 & NOx gases
• Use Bake Out procedure for iPrep vessels (210 °C for 6 hrs – overnight)
• Bake out liners if TempGuard
TM
is triggered
Microwave Safeguards
• Always use the TempGuard feature in the method
• Set the TempGuard limit at 30 °C > control temperature if control temperature is < 250 °C.
• Set the TempGuard limit at 20 °C > control temperature if control temperature is > 250 °C
• Limit TempGuard to 270 °C for digestion of organics with HNO3 (primarily)
• Limit TempGuard to 300 °C for H3PO4/H2SO4 (primarily) applications
• Limit control temperature of organics with HNO3 to 250 °C
• Choose Sample Type in method with software version 1.45 or higher as follows:
• Standard = Any acid mixture other than HCl or HF dominant
• HCl = aqua regia or acid mixtures that are ≥ 75% HCl
• Always use the Max Power Monitor and set the alarm time for 10 minutes
• Maximum programmable temperature is 300 °C
• Maximum temperature varies per acid. See "Operating Parameters" for temperatures
• Maximum programmable Hold Time is 45 minutes
• If a run is stopped or paused for more than 30 seconds during the digestion, do not restart the method
with hot vessels
• Allow vessels to cool < 80 °C
• Vent vessels and reseal
• Restart method from the beginning
• Allow vessels to cool below 80 ºC before opening the microwave door.
4 Important Safeguards
Compounds Unsuitable for Closed Vessel Microwave Digestion
WARNING
CEM will not be responsible for damage to equipment and facilities or personal injuries resulting from
microwave digestion of samples that are deemed unsuitable for closed vessel microwave digestion.
Acid decomposition of certain chemical compounds or types of samples constitutes unreasonable, hazardous
misuse of CEM microwave digestion systems. The classes of compounds listed below are unsuitable for closed
vessel microwave digestion because they are highly reactive with oxidizing acids and/or may become nitrated and
potentially explosive. Absence of a particular chemical compound from this list does not imply microwave acid
decomposition of such a sample is safe under all conditions.
• Explosives (TNT, Nitrocellulose, etc.)
• Propellants (Hydrazine, Ammonium Perchlorate, etc.)
• Pyrophoric chemicals
• Hypergolic mixtures (Nitric Acid and Phenol, Nitric Acid and Triethylamine, Nitric Acid and Acetone,
etc.)
• Animal Fats (Esters of glycerol capable of nitration and the formation of nitroglycerin or other nitrated
organic compounds)
• Aviation Fuels (JP-1, etc.)
• Acetylides
• Glycols (Ethylene Glycol, Propylene Glycol, etc.)
• Perchlorates (Ammonium, Potassium, etc.)
• Ethers (Cellosolve - Ethylene Glycol Phenyl ether, etc.)
• Lacquers
• Alkanes (Butane, Hexane, etc.)
• Ketones (Acetone, Methyl Ethyl Ketone, etc.) and alcohols (methanol, etc.)
5Important Safeguards
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