iPrep

High Performance Vessels

Manual
THIS PAGE INTENTIONALLY LEFT BLANK
Contents
Safety Notations Vessel Distribution

Safety Notations 1 12 Place Turntable 25

16 Place Turntable 26
Introduction

About the iPrep Vessels 2 Methods

Create a One Touch Method 27

Important Safeguards Create a Classic Method 27
Operating Parameters 3
Sample Preparation Safeguards 3 Routine Maintenance

Vessel Safeguards 4 After Every Use 28

Microwave Safeguards 4 Weekly 28
Compounds Unsuitable for Closed Vessel Microwave Annually 28
Digestion 5 As Needed 28

Vessel and Accessories Overview Troubleshooting

Vessel Components 6 Problems and Possible Solutions 29

Accessories 7 Contact Information 30

New Liner and Plug Conditioning

Nitric Acid Liner and Plug Conditioning 8

Non-Nitric Acid Liner and Plug Conditioning 9

Perform a Digestion

Vessel Assembly 10
Turntable Setup 14
Load and perform a Method 14
Vessel Removal 15

Vessel Cleaning

Liners and Plugs 17

Liner and Plug Bake-out Procedure 17
Sleeves 18
Turntable, Frame, Load Disc, Insulator Disc, Screw &
Racks 18

Vessel Inspection

Liner and Plug 19

Sleeve 22
Insulator Disc 24
Turntable, Frame, Load Disc, Screw & Racks 24
THIS PAGE INTENTIONALLY LEFT BLANK
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.

Safety Notations 1
Introduction

About the iPrep Vessels

The iPrep® vessel is designed for microwave digestion in a MARS 6TM with iWave®temperature control. This vessel
is well suited for digestion of difficult 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 One Touch™ methods take the guesswork out of method creation and sample preparation.

This manual is intended for use by both novice and experienced users for the operation and maintenance of the
iPrep Vessels. Additional information, including but not limited to: training notes and videos, application notes,
software updates, and parts can be viewed on CEM’s website at https://cem.com/iprep.

The MARS 6 requires the iWave temperature control with software version 1.43 or higher to operate iPrep vessels.
CEM recommends updating the MARS 6 iWave system to software version 1.49 (or greater). Contact CEM
Corporation for assistance.

This Manual should be used in conjunction with the MARS 6 iWave Manual (P/N 600832). Read and fully
understand all documentation before operating the instrument.

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 (P/N 600832). General
guidelines for safe operation of the iPrep are presented below and all specific safety messages are located
throughout the manual.

Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be worn as
outlined in the user’s safety program for hazardous materials and the acid manufacturer’s safety data sheet. Refer
to these guidelines for proper handling and disposal of the acids.

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
Hydrofluoric 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" section for weights
• Blanks
• Acid Blanks cannot account for more than 25% of turntable when mixed with samples
• Never run acid blanks above 220 °C and never run water blanks above 180 °C.
• Acid blanks cannot be run with samples when acid mixtures are > 50% hydrofluoric acid. Acid blanks must
be run separately

Important Safeguards 3
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
• Plugs should not freely fall into liners. Some resistance should be felt. Group liners and plugs with similar
resistance.
• Align tab on load disc in center notch of liner
• Look for vent hole through the frame
• Align liner and sleeve properly on insulator disc at bottom – liner and sleeve flush 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 (P/N 302070) 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 TempGuardTM is triggered

Microwave Safeguards
• Always use the TempGuard feature in the method for software versions 1.43 - 1.48. TempGuard is preset and
non-adjustable in version 1.49 (or greater).
• 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" section 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.)

Important Safeguards 5
Vessel and Accessories Overview

For a list of parts and part numbers, visit our website at www.cem.com. A list of parts can be found on the
“Products” page under “MARS 6”.

WARNING
Only use vessels and vessel components purchased directly from CEM or through its authorized dealer
network. The use of vessels and vessel components other than original CEM parts will put operators and
equipment at risk; therefore, CEM will not assume any liability for use of these parts and all warranties,
either written or implied, will immediately become void.

Vessel Components

6
1 3

Item Description
1 Frame Module Supports sleeve, load disc, vessel liner, plug and screw
2 Sleeve Supports vessel liner
3 Load Disc Evenly distributes load from plug
4 Vessel Liner Contains acid and sample
5 Plug Seals liner to contain acid and sample
6 Frame Screw Uniformly provides pressure seal among vessels when torqued
7 Insulator Disc Evenly supports load from liner

6 Vessel and Accessories Overview

Accessories

5 2

Item Description
1 Torque Tool Provides appropriate vessel seal. Includes plug removal tool
2 Vessel Liner Holder Holds up to a set of 16 vessel liners
3 12 Place Turntable Holds assembled vessels inside MARS 6 cavity and provides rotation
4 16 Place Turntable Holds assembled vessels inside MARS 6 cavity and provides rotation
5 Frame Carrier Holds up to 4 assembled vessels

Vessel and Accessories Overview 7

New Liner and Plug Conditioning

All new liners and plugs should be conditioned as a set prior to being put into service. The break-in procedure is
used to condition the Teflon® to ensure a proper seal. CEM recommends conditioning the plugs and liners based
on the acid type that will be used: HNO3, HCl, H2SO4, H3PO4, HF. Aqua Regia, or H2O2.

Nitric Acid Liner and Plug Conditioning

1. Use hot soapy water and foam brush to clean the liners and plugs. Rinse thoroughly with DI water and allow to
dry completely before use.

NOTE
Micro 90 Cleaner® liquid detergent works well on Teflon. Avoid detergents that contain ingredients that
could cause potential contamination such as Na and P. Avoid abrasive cleansers and stiff brushes which
can scratch the Teflon surface.

2. Place 0.25 g ± 0.05 g of tea leaves or appropriate sample into each liner. Never add sample or liquid to liner
with sleeve in place.

WARNING
Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be
worn as outlined in the user’s safety program for hazardous materials and the acid manufacturer’s safety
data sheet. Refer to these guidelines for proper handling and disposal of the acids.

3. Add 10 mL of HNO3 to each liner. Use the acid to rinse the inside of the liner to ensure that the sample is in
the base of the liner.
4. Wait 15 minutes to allow pre-digestion.
5. Assemble and torque each vessel. See “Vessel Assembly” section for detailed instructions.
6. Place the turntable into the MARS 6 cavity and symmetrically distribute vessels. See “Turntable Setup”section
and "Vessel Distribution" section for detailed instructions.
7. Select and load the “Plant Material” method from the One Touch directory.
8. Close the instrument door and run the preprogrammed “Plant Material” method.
9. After completion of the method, permit the vessels to cool in the automated sequence until the vessels cool to
below 80 ºC.

WARNING
Allow vessels to cool below 80 ºC before opening the microwave door.
To prevent the possibility of severe burns, ensure that gloves and protective gear as outlined in your safety
program are worn.

10. Remove the vessel assemblies from the turntable. See "Vessel Removal" section for detailed instructions.
11. If the normal method temperatures are greater than 230 °C AND new liners will be mixed with old liners, the
new liners will need to be conditioned three times using the method that exceeds 230 °C before mixing in.
12. Rinse the liners and plugs with deionized water.

8 New Liner and Plug Conditioning

Non-Nitric Acid Liner and Plug Conditioning
1. Use hot soapy water and foam brush to clean the liners and plugs. Rinse thoroughly with DI water and allow to
dry completely before use.

NOTE
Micro 90 Cleaner® liquid detergent works well on Teflon. Avoid detergents that contain ingredients that
could cause potential contamination such as Na and P. Avoid abrasive cleansers and stiff brushes which
can scratch the Teflon surface.

2. Place 0.25 g ± 0.05 g of your sample into each liner. Never add sample or liquid to liner with sleeve in place.

WARNING
Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be
worn as outlined in the user’s safety program for hazardous materials and the acid manufacturer’s safety
data sheet. Refer to these guidelines for proper handling and disposal of the acids.

3. Add 10 mL of the digestion acid to each liner. Use the acid to rinse the inside of the liner to ensure that the
sample is in the base of the liner.
4. Wait 15 minutes to allow pre-digestion.
5. Assemble and torque each vessel. See “Vessel Assembly” section for detailed instructions.
6. Place the turntable into the MARS 6 cavity and symmetrically distribute vessels. See “Turntable Setup” section
and "Vessel Distribution" section for detailed instructions.
7. Select and load the “Easy Prep Clean” method from the One Touch directory.
8. Close the instrument door and run the preprogrammed “Easy Prep Clean” method.
9. After completion of the method, permit the vessels to cool in the automated sequence until the vessels cool to
below 80 ºC.

WARNING
Allow vessels to cool below 80 ºC before opening the microwave door.
To prevent the possibility of severe burns, ensure that gloves and protective gear as outlined in your safety
program are worn.

10. Remove the vessel assemblies from the turntable. See "Vessel Removal" section for detailed instructions.
11. Rinse the liners and plugs with deionized water.

NOTE
When using HCl, if a dark ring appears in liner, use hot soapy water and foam brush to clean. Rinse
thoroughly with DI water and allow to dry completely before use.

New Liner and Plug Conditioning 9

Perform a Digestion

Vessel Assembly
1. Condition new liners and plugs before first use. See “New Liner and Plug Conditioning” section for details.
2. Place liners in vessel liner holder. All vessel components must be dry prior to use.

CAUTION
Never add sample or liquid to liner with sleeve in place. Use the vessel liner holder.

3. Add sample to the liner(s).

WARNING
Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be
worn as outlined in the user’s safety program for hazardous materials and the acid manufacturer’s safety
data sheet. Refer to these guidelines for proper handling and disposal of the acids.

3.1. Weigh and place the sample into the liner. The maximum sample weight varies per sample type. See
"Operating Parameters" section for specific weights.
3.2. Add the acid (5 mL - 30 mL working volume). Use the acid to rinse the inside of the liner to ensure
that the sample is in the base of the liner. If running more than one vessel, you must run similar
samples and the same acids and acid volume in each vessel. See "Sample Preparation Safeguards"
section for information regarding acid blanks along with additional safeguards.
3.3. Ensure that the acid covers the sample and the base of the liner (5 mL minimum).

CAUTION
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.

Do NOT batch old liners with new liners unless new liners have been conditioned with at least 3 runs.

4. Wait 15 minutes to allow pre-digestion.

5. Install the plug into the liner. Slight resistance should be felt when placing the plug into the liner. If resistance
is not felt, try using another plug. Group liners and plugs with similar resistance.

10 Perform a Digestion
 CAUTION
If multiple plugs fall freely into liner, discard liner. Invert sleeves between tests to prevent liners from
stretching.

6. Carefully slide the liner into the sleeve.

NOTE
Invert the vessel sleeves after every test to help maintain uniformity of the liner and sleeves.

Run 1 Run 2 Run 3 Run 4

Perform a Digestion 11
7. Place the load disc on the plug with the tab on the disc facing downward so that it fits into the center notch of
the liner.

8. Ensure that the insulator disc is located in the bottom of the frame and pressed all the way in.
9. Position the sleeve into the frame. Verify vertical placement by ensuring the sleeve is aligned on the disc at the
bottom of the frame.

10. Tighten the screw onto the top of the load disc until it is finger tight.

11. Use the provided torque block and tighten the screw until a single click is heard or felt.

12 Perform a Digestion
 WARNING
Vessel torquing is critical to optimize controlled venting of the system and for the integrity of the vessel.
Over or under torquing may lead to sealing issues. If any issue is noted, contact CEM Corporation

12. Verify the vessel alignment by looking through the viewing port located on the vessel frame. A tiny vent hole
aligned with the window should be visible.

Perform a Digestion 13
Turntable Setup
1. Verify the floor mat positioning, ensuring that the mat is not covering the iWave sensors.

2. Load the empty turntable into the instrument by aligning position “1” with the front of the instrument.
3. The turntable must be seated down on drive lug.

NOTE
CEM suggests that the iPrep vessel set be loaded into the turntable inside the instrument due to the
weight and height of the vessels.

4. Load the vessel assemblies into the turntable one by one, ensuring that the notch in the bottom rear of the
frame engages the locking ring on the turntable. For assistance in loading the vessels, use the Turntable Icon
in the upper right corner of the MARS 6 screen to rotate the turntable. See “Vessel Distribution” section
of this manual for optimal vessel distribution.
5. With the door open, use the Turntable Icon to rotate the turntable. Observe the positioning and balance of
the turntable. Make adjustments by reseating the turntable if necessary.

Load and perform a Method

1. Verify Max Power Monitor is enabled and the alarm time is programmed for 10 minutes (Settings > Run > Max
Power Monitor).
2. Select/load the method from the directory, One Touch or Classic. See "Methods" section or contact CEM Cor-
poration if assistance is needed creating a new method.
3. Close the instrument door.
4. Select “Start” to run the method. The instrument will begin the method according to the selected parameters
– initializing, ramping, holding, cooling, etc. During the run, the user can select the applicable image on the left
side of the screen. If the line graph is selected, the user can select the icons on the right side of the screen to
display the desired parameter(s).

NOTE
If a run is stopped during the digestion, do not restart the method with hot vessels. Allow vessels to cool
< 80°C, vent vessels and reseal, and restart method from the beginning.

14 Perform a Digestion
 CAUTION
Observe the entire digestion sequence when establishing a procedure for the first time.

5. Verify that vessel count, type and position are correct.

6. After completion of the method, permit the vessels to cool in the microwave cavity below 80 ºC.

Vessel Removal
1. Allow the vessels to cool below 80 ºC before opening the microwave door.

WARNING
To prevent the possibility of severe burns, ensure that gloves and protective gear as outlined in your safety
program are worn.

Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be
worn as outlined in the user’s safety program for hazardous materials and the acid manufacturer’s safety
data sheet. Refer to these guidelines for proper handling and disposal of the acids.

2. Remove the vessel assemblies from the turntable one by one, keeping the vent hole pointed away from the
user, and load them into the vessel carrier rack. Keep the vent holes facing away from the user during trans-
portation of the rack.

3. Place the vessel carrier rack into a fume hood, keeping the vent hole pointed away from the user.
4. Use the torque block to carefully loosen the vessel screws, allowing them to vent.
5. Remove the vessels from the frame carrier rack.
6. Place the liner and plug into the liner holder rack.

Perform a Digestion 15
7. Use the plug removal tool to remove the plug from each liner.

8. Transfer the digested sample from liner and proceed with work-up.

CAUTION
Never pour sample or liquid from liner with sleeve in place.

9. Clean vessels as outlined in “Vessel Cleaning ” Section.

16 Perform a Digestion
Vessel Cleaning

WARNING
Proper precautions must be taken to avoid contact with acids or acid vapors. Protective gear should be
worn as outlined in the user’s safety program for hazardous materials and the acid manufacturer’s safety
data sheet. Refer to these guidelines for proper handling and disposal of the acids.

Liners and Plugs

1. Rinse the liners and plugs with deionized water and allow to dry completely before use.
2. If measuring ppm, ppb and/or ppt analyte levels, proceed with steps below.
3. Clean liners and plugs with hot, soapy water and foam brush. Rinse thoroughly with deionized water and allow
to dry completely before use.

NOTE
Micro-90® cleaning solution works well on Teflon. Avoid detergents that contain ingredients that could
cause potential contamination such as Na and P. Avoid abrasive cleansers and stiff brushes which can
scratch the Teflon surface.

4. Clean liners and plugs using the microwave as outlined below. All vessel components must be dry before use.
4.1. Add 10 mL of acid that had been used for sample digestion, HNO3, HCl, H2SO4, H3PO4 or HF.
4.2. Prepare vessel and turntable as outlined in manual.
4.3. Depending on acid type, select and run the appropriate method in the One Touch directory.
• HNO3, HCl or HF: Select “Easy Prep Clean.”
• H2SO4 or H3PO4: Select “High Temp Clean”. If “High Temp Clean” is not available, create a One Touch
method with the following parameters: Temperature=240 °C, Sample Type=Organic, Hold Time=15
minutes and TempGuard=270 °C (if applicable).
4.4. Wait for vessels to cool below 80 °C before opening microwave door.
4.5. Discard acid and rinse the liners and plugs with deionized water.

Liner and Plug Bake-out Procedure

As needed: The bake out procedure can be used to remove residual acid vapors and other trapped gases from the
Teflon® material. Trapped gases can potentially cause uneven heating between new and used liners.

The bake out procedure can be used to remove residual NOx gases from liners following digestion with HNO3 that
may interfere in subsequent runs. This procedure has been successfully used to remove sulfur contamination from
the Teflon following digestion of samples with high sulfur content.

Vessel Cleaning 17
Procedure:
1. Place the plugs and liners on their side in an air oven at room temperature.

CAUTION
Only the plugs and liners should be placed in the air oven at 210 ºC. Sleeves can be placed in an air oven
no greater than 105 °C. See "Sleeves" section for more detail.

2. Set the oven temperature to 210 °C and let the liners warm slowly. Do not exceed an oven temperature of 215
°C.
3. Leave the liners in the oven for a minimum of 6 hours. Leaving them in overnight is acceptable.
4. After the heating time is complete, turn the oven off and let the liners cool slowly back to room temperature
inside the oven. It is important to let the liners cool slowly back to room temperature following the bake out
procedure.
5. Remove the liners from the oven. The liners should be white in color, comparable to new liners with no acid
history.

Sleeves
1. If water or acid gets on a sleeve, wipe it off with a damp paper towel and allow to dry. Never soak sleeves.

CAUTION
Never soak sleeves in water or detergent.

Remove composite sleeves before adding acid to vessel liners or before pouring digested solutions out to
prevent liquid from wicking into the composite material.

Turntable, Frame, Load Disc, Insulator Disc, Screw & Racks

1. Wash in hot, soapy water as needed and allow to dry completely before use.

18 Vessel Cleaning
Vessel Inspection

All iPrep components should be inspected on a weekly basis. The component lifetime will be based upon
temperatures being run and hold times at high temperatures. View the guidelines below to determine if it is ok to
continue to use the part or if it needs replacement. It is imperative to replace worn vessel parts to prevent vessel
failure.

Liner and Plug

Description: Liners and plugs should be smooth and white. Liners should be straight and even in diameter
throughout the length until the lip at the top.

Rough in texture on the outside (alligator skin)

Cause: High heat and pressure that pushes the liner against the sleeve.
Continue Use?: Maybe. The liners might be ok to run but will need to be grouped with like vessels.
Preventative Measures: See “Operating parameters” for maximum temperatures.

Vessel Inspection 19
Liner: Stretch, Flare, extrude, visible dark line along top

Cause: Excessive pressure.

Continue Use?: No. Replace liner. Discard plug if damage is noticed.
Preventative Measures: See “Operating parameters” for maximum temperatures.

Liner: Bow or flare at bottom

Cause: High pressure during use and/or not inverting sleeves after each run.
Continue Use?: Maybe. If you can insert the liner into the most resistant end of sleeve, then continue use.
Preventative Measures: Invert sleeves after every run to extend lifetime and promote better sealing & even
heating.

20 Vessel Inspection
Liner: Raised spot at bottom

Cause: Excessive pressure.

Continue Use?: No. Also might need to replace insulator disc.
Preventative Measures: See “Operating parameters” for maximum temperatures.

Liner and Plug: Very white on the inside

Cause: Extreme heat (>300 °C)

Continue Use?: No. Replace liner/plug.
Preventative Measures: See “Operating Parameters” for maximum temperatures.

Vessel Inspection 21
Liner and Plug: Plug falls freely inside

Cause: Not inverting/flipping sleeves after every run.

Continue Use?: Maybe. Slight resistance should be felt when placing the plug into the liner. If resistance is not
felt, try using another plug. Discard liner if there is not a plug to match.
Preventative Measures: Invert sleeves after every run to extend lifetime and promote better sealing & even
heating.

Sleeve
The most critical part is the vessel sleeve as it provides the mechanical strength of the vessel. For applications
running organic samples at 240 ºC or higher CEM strongly recommends replacement of these sleeves every 50
runs.

Description: Smooth, golden brown, even in diameter from top to bottom.

22 Vessel Inspection
Discoloration

Cause: Temperatures greater than 250 ºC for long periods of time or normal wear and tear.
Continue Use?: No. Replace sleeves that are white
Preventative Measures: N/A

Flaring

Cause: Not inverting/flipping sleeves after every run.

Continue Use?: No. Replace sleeves if flared or if it is not possible to insert any liner into the sleeve. Inspect
liners.
Preventative Measures: Invert sleeves after every run to extend lifetime and promote better sealing & even
heating

Wet
Cause: Sleeve submerged in water.
Continue Use?: No. Discard sleeves that have been submerged.
Preventative Measures: Never soak sleeves. If water or acid gets on a sleeve, wipe it off with a damp paper towel
and allow to dry.

Vessel Inspection 23
Insulator Disc
Description: Smooth, clear and flat on surface where disc comes in contact with the liner.

Insulator disc indented where contact is made with liner

Cause: Excessive pressure during use.

Continue Use?: No. Also might need to replace liner and frame. Contact CEM Corporation.
Preventative Measures: See “Operating Parameters” for maximum temperatures.

Turntable, Frame, Load Disc, Screw & Racks

Inspect the turntable, frames, load discs, and screw for acid marks, cracks or discoloration.

24 Vessel Inspection
Vessel Distribution

12 Place Turntable
Even vessel distribution is required for optimal performance. Proper spacing will eliminate hot spots, issues
regarding turntable balance, and provide optimal temperature sensing.

2 vessels 3 vessels 4 vessels

5 vessels 6 vessels 7 vessels

8 vessels 9 vessels 10 vessels

11 vessels 12 vessels

Vessel Distribution 25
16 Place Turntable
Even vessel distribution is required for optimal performance. Proper spacing will eliminate hot spots, issues
regarding turntable balance, and provide optimal temperature sensing.

2 vessels 3 vessels 4 vessels 5 vessels

6 vessels 7 vessels 8 vessels 9 vessels

10 vessels 11 vessels 12 vessels 13 vessels

14 vessels 15 vessels 16 vessels

26 Vessel Distribution
Methods

Pre-installed One Touch Methods take the guesswork out of method creation and sample preparation. If there is
not a current One Touch Method to digest a sample, visit our website for Method and Application Notes.

Create a One Touch Method

The MARS 6 has preinstalled methods to cover a large variety of samples. If there is not a current One Touch
Method to digest a sample, a One Touch method can be programmed as outlined below. See “Operating
Parameters” section for details when selecting parameters.
1. From the MARS 6 home screen, select “One Touch Methods.”
2. Select “+” at the top of the screen to begin creating a One Touch Method.
3. Select “Method Name” and enter in a name.
4. Select “Temperature” and enter the desired temperature.

CAUTION
Limit control temperature of organics with HNO3 to 250 °C. Higher temperatures will permanently damage
liner and sleeve

5. Select “Sample Type” and select the appropriate type.

• Acid mixtures greater than 50% HCl, contact CEM Corporation.
• Acid mixtures less than 50% HCl or all other acids select "organic"
6. Select “Hold Time” and enter in the appropriate hold time.
7. For software versions 1.49 (or greater) proceed with step 8. For software versions 1.43 - 1.48, enable “Temp-
Guard” as outlined below.
• Always use TempGuard
• 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
• Limit TempGuard to 300 °C for H3PO4/H2SO4 applications
8. If applicable, select “Sample Prep Notes.”
9. The MARS 6 will complete all other necessary information to perform the method.
10. Select “Next.” View the method by scrolling down. If any parameters require revisions, select “Previous” and
make appropriate revisions.
11. Once the method parameters are entered properly, select the Save icon located in the top right corner.
12. Once the method is saved, the method may be run by selecting the Play icon. To view method parameters,
select the method and select the Information icon located at the top of the screen.

CAUTION
Observe the entire digestion sequence when establishing a procedure for the first time.

Create a Classic Method

Contact CEM Corporation before creating Classic Methods.

Methods 27
Routine Maintenance

A routine maintenance protocol is vital for the long-term operation of the iPrep vessels. For maintenance
instructions for MARS 6 instrument, see the MARS 6 iWave manual (P/N 600832).

After Every Use

• Clean all vessel components. See “Vessel Cleaning” section of this manual.
• Wipe inside of MARS 6 cavity, including the iWave sensors, with a lint free damp cloth.

Weekly
• Inspect Vessel Components. See "Vessel Inspection" section of this manual for acceptable wear on these
components.

Annually
• Contact CEM Service Department, local CEM subsidiary or distributor for information on CEM Service contracts.

As Needed
• Bake-out liners and plugs - See "Liner and Plug Bake-out Procedure" section for instructions. The bake out
procedure can be used to remove residual acid vapors and other trapped gases from the Teflon® vessel liner
material. Trapped gases can potentially cause uneven heating between new and used liners.

28 Routine Maintenance
Troubleshooting

Problems and Possible Solutions

Problems Possible Cause Possible Solutions
TempGuard message appears during run Some vessels are hotter • See “Liner and Plug Bake-out Procedure” section to reduce
than others differences in liners
• Do not batch old and new liners. Run in separate turntables
TempGuard variables • Set the TempGuard limit at 30 °C > control temperature if
programmed incorrectly control temperature is < 250 °C.
(software versions 1.43 • Set the TempGuard limit at 20 °C > control temperature if
-1.49) control temperature is > 250 °C
• Limit TempGuard to 270 °C for digestion of organics with
HNO3
• Limit TempGuard to 300 °C for H3PO4/H2SO4 applications
Uneven bar graphs during run Acid diluted with water Do not dilute acids greater than 25% when running over 220 ºC
Not enough similarity in Select samples with similar properties or use same in all vessels
sample type or sample and similar sample amounts
weight
Different acid(s) or acid Run the same acid and acid volume in each vessel in the
volumes being used in turntable
vessels
Some vessels are hotter See “Liner and Plug Bake-out Procedure” section to reduce
than others differences in liners
Some vessels contain See "Sample Preparation Safeguards" section for specific
acid blanks details when running acid blanks.
Liner not getting as hot Pair liners with plugs that offer resistance. Invert sleeves after
due to leaking every test
Vessel Liner or sleeve appearance has Dark ring along bottom Liner needs cleaning - See “Vessel Cleaning” section
changed of liner
Liner not fitting into Determine if liner or sleeve is problem. Invert sleeves after every
Sleeve run to extend lifetime of liner and sleeve
Alligator skin on outside Result of high heat/pressure. May be ok to run but will need to
of liner be grouped with like vessels
Stretching along top of Discard liner - See “Operating Parameters” section for maximum
liner along with visible temperature to prevent excessive pressure buildup
dark line
Sleeve distorted or flared
Discard Sleeve - Invert sleeves after every run to extend lifetime
of liner and sleeve
Sleeve has turned white Replace sleeve. To prevent sleeve damage, avoid high
(no longer golden brown) temperatures for long periods of time.
Max Power Monitor message appears Max Power Monitor Verify Max Power Monitor is enabled and the alarm time is
during run variables programmed programmed for 10 minutes (Settings > Run > Max Power
incorrectly Monitor)
Vessels leaking Vessels possibly not assembled properly or not torqued using
torque tool

Troubleshooting 29
Contact Information
• Applications Support: Contact CEM at (800) 726-3331 (US/Canada), (704) 821-7015, or by email at
[email protected].
• Technical Support: Contact CEM Service at (800) 726-5551 (US/Canada) or (704) 821-7015, or by email at
[email protected].
• Additional contact information: Located on the back cover of this manual.

30 Troubleshooting
THIS PAGE INTENTIONALLY LEFT BLANK
 USA:
CEM Corporation (Headquarters)
PO Box 200
Matthews, NC 28106
United States
800-726-3331
704-821-7015
Fax: 704-821-7894
[email protected]
www.cem.com
France:
CEM μWave S.A.S.
Immeuble Ariane
Domaine Technologique de Saclay
4, rue Rene’ Razel, 91892 ORSAY Cedex
33 (01) 69 35 57 80
Fax: 33 (01) 60 19 64 91
[email protected]
Germany, Austria, Switzerland:
CEM GmbH
Carl-Friedrich-Gauss-Str.9, 47475 Kamp-
Lintfort
(49) 2842-9644-0
Fax: (49) 2842-9644-11
[email protected]
Ireland:
CEM Technology (Ireland) Ltd.
Sky Business Centre, 9a Plato Business Park,
Damastown, Dublin 15
+353 (0) 1 885 1752
Fax: +353 (0) 1 885 1601
[email protected]
Italy:
CEM S.R.L.
Via Dell’ Artigianato, 6/8
24055 Cologno al Serio (Bg)
(39) 35-896224 • Fax: (39) 35-891661
[email protected]
Japan:
CEM Japan K.K.
2-18-10 Takanawa, Minato-ku, Tokyo 108-
0074
+81-3-5793-8542 • Fax: +81-3-5793-8543
[email protected]
United Kingdom:
CEM Microwave Technology Ltd.
2 Middle Slade, Buckingham Industrial Estate,
Buckingham MK181WA
(44) 1280-822873
Fax: (44) 1280-822873
[email protected]

For a complete list of distributors of CEM

products, including contact information, go to
the CEM website (http://www.cem.com)

Copyright 2019 by CEM Corporation iWave and iPrep are registered trademarks Part Number 600856
All Rights Reserved. This guide contains of CEM Corporation. MARS 6, TempGuard July 29, 2019
proprietary information which shall not and One Touch are trademarks of CEM Rev. 5
be reproduced or transferred to other Corporation. Copyright CEM Corporation 2019
documents or disclosed to others without Teflon is a registered trademark of the
prior written permission of CEM Corporation. Dupont Corporation.