EasyPrep Series

High Performance Vessels

Manual
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Contents
Safety Notations Classic Method Creation 30

Safety Notations 1
Fiber Optic Temperature Control

Introduction Fiber Optic Installation 31

Fiber Optic Temperature Verification 32
About the EasyPrep™ Vessel Series 2
Fiber Optic Care 32

Important Safeguards
Routine Maintenance
Operating Parameters 3
After Every Use 33
Sample Preparation Safeguards 3
Daily 33
Vessel Safeguards 4
Weekly 33
Microwave Safeguards 4
Annually 33
Compounds Unsuitable for Closed Vessel Microwave
As Needed 33
Digestion 5

Troubleshooting
Vessel and Accessories Overview
Problems and Possible Solutions 34
EasyPrep iWave Vessel Components 7
Contact Information 35
EasyPrep Plus Vessel Components 8
EasyPrep Vessel Components 10
Glossary
Accessories 12
Glossary 36

New Liner and Cover Conditioning

Nitric Acid Liner and Cover Conditioning 13

Non-Nitric Acid Liner and Cover Conditioning 14

Perform a Digestion

Vessel Assembly 15
Turntable Setup 20
Load and Perform a Method 24
Vessel Removal 25

Vessel Cleaning

Liner 27
Liner Bake-out Procedure 27
Covers 28
Sleeves 28
Turntable, Frame, Load Disc, & Screw 28

Vessel Distribution

Even Vessel Distribution 29

Methods

One Touch Method Creation 30

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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.

Safety Notations 1
Introduction

About the EasyPrep™ Vessel Series

The EasyPrep, EasyPrep Plus, and EasyPrep iWave® vessels are designed for microwave digestion in a MARS 6™.
These rugged high performance vessels are good for preparing a wide variety of difficult to digest organic and
inorganic materials. These include many types of oils and polymers, ceramics and catalysts, pigments & toner,
coal, alpha alumina, or digestion of large organic samples like food and plant/animal tissues when lower detection
limits are critical. The EasyPrep vessel series are easy to assemble vessels with moderate throughput. 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
vessel. 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.

CEM recommends updating the MARS 6 and MARS 6 iWave system to software version 1.49 (or greater). Contact
CEM Corporation for assistance.

Depending on the instrument configuration, this Manual should be used in conjunction with the MARS 6 manual
(P/N 600284) or MARS 6 iWave Manual (P/N 600832). If your MARS instrument is not listed, contact your CEM
Representative for assistance.

Read and fully understand all documentation before operating the instrument.

For assistance regarding vessel inserts, view the 35 mL Quartz Vessel Insert Manual (P/N 600742 and P/N
600744), 3mL or 7mL Teflon Insert Manual (P/N 600769) or contact CEM Corporation.

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 MARS 6 manual (P/N 600284) or
MARS 6 iWave manual (P/N 600832). General guidelines for safe operation of the EasyPrep vessel series 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
EasyPrep EasyPrep Plus EasyPrep iWave
Parameters Minimum Volume 6 mL 5 mL 5 mL
Maximum Volume 30 mL 30 mL 30 mL
Maximum Pressure 800 psi 800 psi 800 psi
Maximum Hold Time 30 min 30 min 30 min
Maximum Temperature Maximum Programmable Temperature 310 ºC 310 ºC 310 ºC
Nitric Acid 230 ºC 230 ºC 230 ºC
Hydrochloric Acid 230 ºC 230 ºC 230 ºC
Hydrofluoric Acid 210 ºC 210 ºC 210 ºC
Sulfuric Acid 300 ºC 300 ºC 300 ºC
Phosphoric Acid 300 ºC 300 ºC 300 ºC
Aqua Regia 230 ºC 230 ºC 230 ºC
Water 200 ºC 200 ºC 200 ºC
Maximum Sample Weight Food, Plant, and Animal Tissue 1.0 g 1.0 g 1.0 g
Oil and Plastic 0.25 g 0.25 g 0.25 g
Pharmaceutical 1.0 g 1.0 g 1.0 g
Inorganic 1.0 g 1.0 g 1.0 g
Metallurgical 1.0 g 1.0 g 1.0 g
Clinical 1.0 g 1.0 g 1.0 g

Sample Preparation Safeguards

• Do not use water to dilute the acid(s) greater than 25% when running over 210 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 volume for the MARS 6 cavity is 10 mL of acid or 50 mL of water.
• Maximum sample weight varies per sample type. See "Operating Parameters" for weights.
• Never run an acid blank in the control vessel.
• Acid blanks cannot account for more than 25% of turntable when mixed with samples.
• 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 consumables, accessories, vessels and vessel components purchased directly from CEM or through its
authorized dealer network.
• The standard cover is recommended for applications using primarily HNO3, HF, H2SO4, and H3PO4.
• The Premium cover is recommended for non-HF applications where HCl and aqua regia are heavily used.
• All vessel components must be dry prior to use.
• Always condition new liners and covers.
• Ensure vessels are assembled properly.
• 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.
• Bake out liners to remove residual HNO3 & NOx gases
• See "Liner Bake-Out Procedure" for details.
• Bake out liners if TempGuard™ is triggered.
• Do not cool any of the vessel components in the freezer.
• The fully loaded turntable without sample may be heavy (>20 pounds (9 kg)). Use caution when lifting and
loading into the cavity. Do not place fingers beneath the turntable when placing in the cavity.

Microwave Safeguards
• Always use the TempGuard feature in the method for software versions < 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 < 230 °C.
• Set the TempGuard limit at 20 °C > control temperature if control temperature is > 230 °C.
• Limit TempGuard to 250 °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 230 °C.
• For non-iWave configurations, Duotemp must always be ON.
• Always use the Max Power Monitor and set the alarm time for 5 minutes.
• Maximum programmable temperature is 310 °C.
• Maximum temperature varies per acid. See "Operating Parameters" for temperatures.
• Maximum programmable Hold Time is 59 minutes.
• Maximum recommended Hold Time is 30 minutes.
• Observe the positioning and balance of the turntable.
• If applicable, ensure the pressure line and fiber optic probe are connected, in position and properly aligned.
• 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 for a minimum of 15 minutes.
• Vent vessels and reseal.
• Restart method from the beginning.
• Allow vessels to cool for a minimum of 15 minutes 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”.

The EasyPrep vessel cover assemblies (control and standard) are available with two types of rings – standard
composite and Titanium metal. EasyPrep covers with Titanium rings are referred to as “Premium”. The standard
composite ring is recommended for applications using primarily HNO3, HF, H2SO4, and H3PO4. The Titanium metal
ring is recommended for non-HF applications where HCl and aqua regia are heavily used.

WARNING
Only use consumables, accessories, vessels and vessel components purchased directly from CEM
or through its authorized dealer network. The use of consumables, accessories, 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.

EasyPrep Control EasyPrep Plus Control Vessel EasyPrep iWave Control &
Standard Vessel(s)

6 Vessel and Accessories Overview

EasyPrep iWave Vessel Components

Frame Sleeve Load Disc

P/N 514050 P/N 431740 P/N 131130
Supports sleeve, load disc, vessel Supports vessel liner Evenly distributes load from cover
liner, cover and screw

Vessel Liner Standard Cover Premium Cover

P/N 432175 P/N 131125 P/N 131126
Contains acid and sample. 110 mL Seals liner to contain acid and Seals liner to contain acid and
Liner (5 -30 mL working volume) sample sample. Recommended for use with
HCl.

Frame Screw EasyPrep iWave Turntable

P/N 144996 P/N 404305
Uniformly provides pressure seal Holds assembled vessels inside
among vessels when torqued MARS iWave cavity and provides
rotation

Vessel and Accessories Overview 7

EasyPrep Plus Vessel Components

Frame Control Frame Sleeve

P/N 514050 P/N 514060 P/N 431740
Supports sleeve, load disc, vessel Fiber Optic Temperature and Pressure Supports vessel liner
liner, cover and screw Control: Supports sleeve, load disc,
vessel liner, cover and screw

Load Disc Temperature Control Load Disc Vessel Liner

P/N 131130 P/N 131165 P/N 432175
Evenly distributes load from cover Fiber Optic Temperature Control: Contains acid and sample. 110 mL
Evenly distributes load from cover Liner (5 -30 mL working volume)

Standard Cover Premium Standard Cover Control Cover T only

P/N 131125 P/N 131126 P/N 131195
Seals liner to contain acid and Seals liner to contain acid and Fiber Optic Temperature control: Seals
sample sample. Recommended for use with liner to contain acid and sample
HCl.

8 Vessel and Accessories Overview

Control Cover T & P Premium Control Cover T only Premium Control Cover T & P
P/N 131120 P/N 131196 P/N 131121
Fiber Optic Temperature and pressure Fiber Optic Teperature control: Seals Fiber Optic Temperature and pressure
control: Seals liner to contain acid liner to contain acid and sample. control: Seals liner to contain acid
and sample Recommended for use with HCl and sample. Recommended for use
with HCl.

Frame Screw Control Frame Screw Pressure Nut

P/N 144996 P/N 144995 P/N 431311
Uniformly provides pressure seal Fiber Optic Temperature Control: Seals Pressure connector when ESP-
among vessels when torqued Uniformly provides pressure seal 1500+ not in use
among vessels when torqued

Sapphire Thermowell Thermowell Nut EasyPrep and EasyPrep Plus

Turntable
P/N 131173 P/N 325029 P/N 432100
Protects fiber optic temperature probe Secures sapphire thermowell to Holds assembled vessels inside
Control Cover MARS 6 cavity and provides rotation

Vessel and Accessories Overview 9

EasyPrep Vessel Components

Frame Control Frame T only Control Frame T & P

P/N 514050 P/N 514070 P/N 514055
Supports sleeve, load disc, vessel Fiber Optic Temperature Control: Fiber Optic Temperature and Pressure
liner, cover and screw Supports sleeve, load disc, vessel Control: Supports sleeve, load disc,
liner, cover and screw vessel liner, cover and screw

Sleeve Load Disc Temperature Control Load Disc

P/N 431740 P/N 131130 P/N 131165
Supports vessel liner Evenly distributes load from cover Fiber Optic Temperature Control
Vessel: Evenly distributes load from
cover

Vessel Liner Standard Cover Premium Standard Cover

P/N 432175 P/N 131125 P/N 131126
Contains acid and sample. 110 mL Seals liner to contain acid and Seals liner to contain acid and
Liner (6 -30 mL) working volume) sample sample. Recommended for use with
HCl

10 Vessel and Accessories Overview

Control Cover T only Control Cover T& P Premium Control Cover T only
P/N 131200 P/N 131205 P/N 131201
Fiber Optic Temperature only control: Fiber Optic Temperature and pressure Fiber Optic Temperature control:
Seals liner to contain acid and control: Seals liner to contain acid Seals liner to contain acid and
sample and sample sample. Recommended for use with
HCl

Premium Control Cover T & P Frame Screw Control Frame Screw

P/N 131206 P/N 144996 P/N 144995
Fiber Optic Temperature and pressure Uniformly provides pressure seal Fiber Optic Temperature Control:
control: Seals liner to contain acid among vessels when torqued Uniformly provides pressure seal
and sample. Recommended for use among vessels when torqued
with HCl.

Pressure Nut EasyPrep and EasyPrep Plus

Turntable
P/N 431311 P/N 432100
Seals Pressure connector when ESP- Holds assembled vessels inside
1500+ not in use MARS 6 cavity and provides rotation

Vessel and Accessories Overview 11

Accessories

Torque Tool Vessel Loosening Wrench Torque Stand

P/N 514140 P/N 430660 P/N 144925
Provides appropriate vessel seal (84 Removes frame screw. Holds Vessels in place while torquing
inches per pound (7 ft-lbs))

Vessel Liner Holder

P/N 166222
Holds up to a set of 16 vessel liners

12 New Liner and Cover Conditioning

New Liner and Cover Conditioning

All new liners and covers 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 covers and liners based
on the acid type that will be used: HNO3, HCl, H2SO4, H3PO4, HF. Aqua Regia, or H2O2.

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.

Nitric Acid Liner and Cover Conditioning

1. Use hot soapy water and foam brush to clean the liners and covers. 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. The liner containing the highest amount of weighed sample will be the control vessel.
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” for detailed instructions.
6. Select and load the “Plant Material” method from the One Touch directory.
7. Place vessels on turntable and insert the turntable into the cavity. See “Turntable Setup” and "Vessel Distribu-
tion" for detailed instructions.
8. Close the instrument door and run the preprogrammed “Plant Material” method. Verify that vessel count, type
and position are correct. It is normal for vessels to vent during digestion.
9. After completion of the method, permit the vessels to cool in the automated sequence until the vessels cool
for a minimum of 15 minutes.

WARNING
Allow vessels to cool for a minimum of 15 minutes 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" for detailed instructions.
11. Rinse the liners and covers with deionized water.

New Liner and Cover Conditioning 13

Non-Nitric Acid Liner and Cover Conditioning
1. Use hot soapy water and foam brush to clean the liners and covers. 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.
The liner containing the highest amount of weighed sample will be the control vessel.
3. Add 10 mL of the digestion acid type 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.

NOTE
For non-acid applications, use 20 mL of water. The minimum cavity load for water is 50 mL so more than
one vessel is required.

4. Wait 15 minutes to allow pre-digestion.

5. Assemble and torque each vessel. See “Vessel Assembly” for detailed instructions.
6. Select and load the “Easy Prep Clean” method from the One Touch directory.
7. Place vessels on turntable and insert the turntable into the cavity. See “Turntable Setup” and "Vessel Distribu-
tion" for detailed instructions.
8. Close the instrument door and run the preprogrammed “Easy Prep Clean” method. Verify that vessel count,
type and position are correct. It is normal for vessels to vent during digestion.
9. After completion of the method, permit the vessels to cool in the automated sequence until the vessels cool
for a minimum of 15 minutes.

WARNING
Allow vessels to cool for a minimum of 15 minutes 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" for detailed instructions.
11. Rinse the liners and covers with deionized water.

14 New Liner and Cover Conditioning

Perform a Digestion

In addition to the instructions below, view the “EasyPrep Vessels” video located in the MARS software (System
Settings -> Video -> EasyPrep Vessels.)

The EasyPrep Vessels have multiple configurations available for the Standard and Premium covers: MARS 6
EasyPrep Temperature Only, MARS 6 EasyPrep Temperature and Pressure, MARS 6 EasyPrep Plus Temperature only,
MARS 6 EasyPrep Plus Temperature and Pressure, and EasyPrep Plus iWave.

Vessel Assembly
The images below are used for a visual reference. Not all covers have the temperature and/or pressure option as
shown in images outlined below. Unless otherwise indicated, the assembly procedures are the same for the vessel
configurations.
1. Liners and covers must be conditioned before use. See “New Liner and Cover Conditioning” for details.
2. 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. Place liners in vessel liner holder.

4. 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.

4.1. Inspect liners for abnormalities.

4.2. Weigh and transfer the sample into the liner. The maximum sample weight varies per sample type. See
"Operating Parameters" for specific weights. If a control vessel is required, use the liner containing the
highest amount of weighed sample as the control vessel.

CAUTION
Never run an acid blank in the control vessel.

4.3. Add the acid. Use the acid to rinse the inside of the liner to ensure that the sample is in the base of
the liner. See "Operating Parameters" for minimum and maximum volumes.
4.4. Ensure that the acid covers the sample and the base of the liner.
4.5. Prepare remaining vessels. 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" for information
regarding acid blanks along with additional safeguards.

Perform a Digestion 15
 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.

5. Wait 15 minutes to allow pre-digestion.

6. If applicable, assemble the Easy Prep Plus Control Cover.

6.1. Insert the open end of the thermowell into the control cover until it stops.

CAUTION
Do not force thermowell into control cover as it is fragile and may break.

6.2. Slide the nut onto the thermowell and tighten the nut until finger tight.
7. Place the cover on the liner. If a control vessel is required, use the liner containing the highest amount of
weighed sample as the control vessel.

8. Carefully slide the liner into the sleeve.

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

9. Place the load disc on the cover with the tab on the disc facing downward so that it fits into the center notch of
the cover. The fiber optic temperature control cover requires the load disc with a hole in the center.

10. Position the sleeve into the correct frame.

Perform a Digestion 17
• The control vessel requires the taller frame (except EasyPrep with temperature control only)
• The standard vessels and EasyPrep with temperature control only require the shorter frame.
• If the cover has pressure control, select the "Easy Prep Plus" control frame and position the pressure connector
so it passes through the frame and aligns toward the outside of the frame.
11. Verify vertical placement by ensuring the sleeve is aligned on the disc at the bottom of the frame.

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

18 Perform a Digestion
13. Position the vent hole or pressure connector away from the frame and neighboring vessels.

14. Torque the vessels.

14.1. Place the assembled vessel into the vessel stand. Use the vessel stand to torque the vessels. The
vessel stand can be affixed securely in any location by placing double sided tape on the bottom of the
stand.
14.2. If the cover has pressure control, ensure pressure connector is not touching the frame before or after
torquing.
14.3. Use the provided torque wrench and tighten the screw until a single click is heard or felt. The EasyPrep
vessel series requires a torque setting of 84 in-lbs (7 ft-lbs).

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.

15. Verify the vent hole alignment. If a vessel vents, the acid should not get on the frame or other vessels. If nec-
essary, loosen the screw and realign the vent hole.

Perform a Digestion 19
Turntable Setup
1. If applicable, load the control vessel in the "Control Vessel" or "1" position of the turntable.

1.1. If the control vessel has pressure control, connect the ESP-1500+ pressure connector and tighten
until finger tight. If the ESP-1500+ pressure option is not available, tighten the nut until finger tight.

1.2. If the control vessel has fiber optic temperature control, insert the fiber optic probe into the control
vessel.
• The fiber optic probe should slide easily into the thermowell through the frame screw and load disc
until the probe reaches the bottom of the thermowell.
• Do not force the fiber optic probe.
• If probe cannot be easily inserted, check vessel alignment. Loosen the screw and realign.

20 Perform a Digestion
 CAUTION
If resistance is felt when trying to insert probe, ensure that the thermowell is not broken inside the Teflon
cover. The sharp edges of any break can restrict the movement of the probe.

The "MTS-300 High Temp" (P/N 281461) Fiber Optic probe is required for applications running 250 ºC or
greater in temperature.

2. Load the remaining 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. See “Vessel Distribution” section of this manual
for optimal vessel distribution.

3. Ensure that the notch in the bottom of the frame engages the locking ring on the turntable.

Perform a Digestion 21
4. Verify the floor mat positioning, ensuring that the mat is not covering the temperature sensors.

5. Load the turntable into the instrument by aligning the Control Vessel or position “1” with the front of the instru-
ment. Ensure turntable is seated down on drive lug.

22 Perform a Digestion
 WARNING
The fully loaded turntable without vessels may be heavy (>20 pounds (9 kg)). Use caution when lifting and
loading into the cavity. Do not place fingers beneath the turntable when placing in the cavity.

6. If applicable, connect the pressure sensor to the right side wall of the MARS 6 cavity.
6.1. Press the turntable key to rotate the turntable until the control vessel is located in the back left corner
of the instrument.
6.2. Connect the ESP-1500 Plus pressure controller to the connector port on the right side of the instru-
ment cavity (facing instrument) by rotating the pressure sensor and gently pushing it into the connec-
tor port until it slips/locks into the correct position.
6.3. Secure the pressure line into the ceiling clip.

7. If applicable, connect the fiber optic probe to the port in the top center of the MARS 6 cavity by pushing in the
plug until it snaps into place.

8. With the door open, use the Turntable icon to rotate the turntable. Observe the positioning and balance of the
turntable. If applicable, permit the turntable to rotate 2 or 3 times to ensure that the pressure sensing line and
temperature probe do not become entangled and stay in position. Make adjustments by re-seating the turnta-
ble if necessary.

Perform a Digestion 23
Load and Perform a Method
1. Verify Max Power Monitor is enabled and the alarm time is programmed for 5 minutes (Settings > Run > Max
Power Monitor).
2. For EasyPrep and EasyPrep Plus vessels, verify fiber optic temperature.
2.1. Select the System Settings icon in the bottom right corner of the screen.
2.2. Select Tools.
2.3. Select the "System" tab. The "FISO Temperature (ºC)" will appear under "Status".

2.4. Verify the temperature reading at room temperature.

• If the fiber optic probe is new or the temperature is not reading correctly, enter the GF number. See
the "Fiber Optic" section of the manual for details.
• If “---” appears as the temperature, then the MARS 6 does not recognize the Fiber Optic Probe. The
probe is either not installed or is not working properly. See the "Fiber Optic" section of the manual
for details.
2.5. Press the Home icon in the lower left corner of the screen to return to the Home page.
3. 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.
4. Close the instrument door.
5. Select “Start” to run the method. The instrument will begin the method according to the selected parameters
– initializing, ramping, holding, cooling, etc.
5.1. Verify that vessel count, type and position are correct.

NOTE
If a run is stopped during the digestion, do not restart the method with hot vessels. Allow vessels to cool
for a minimum of 15 minutes, vent vessels and reseal, and restart method from the beginning.

CAUTION
Observe the entire digestion sequence when establishing a procedure for the first time. It is normal for
vessels to vent during digestion.

6. During the run, the user can select the applicable image on the left side of the screen. If the line graph is se-
lected, the user can select the icons on the right side of the screen to display the desired parameter(s).
7. After completion of the method, permit the vessels to cool in the microwave cavity for a minimum of 15 min-
utes.

24 Perform a Digestion
Vessel Removal
1. Allow the vessels to cool for a minimum of 15 minutes 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. If applicable, disconnect fiber optic probe.

3. If applicable, disconnect the pressure sensor from the connector port by pulling on the collar. Do not pull on
the pressure line.
4. Remove the turntable, keeping the vent holes pointed away from the user at all times, and place into a fume
hood.
5. If applicable, remove the fiber optic probe from the control vessel.
6. Remove the vessel assemblies from the turntable one by one, keeping the vent hole pointed away from the
user.
7. With the vent hole pointed away from the user, use the vessel loosening wrench to slowly and carefully loosen
the vessel screws, allowing them to vent. If the screw is difficult to loosen, position the vessel back in the
torque stand and use the wrench to loosen the screw, but not to the point that the vessel vents (unless the
torque stand is inside the fume hood.)

NOTE
A plastic vessel loosening wrench is required to loosen frame screws.

8. If applicable, disconnect the pressure sensor from the control cover.

9. Remove the load disc, cover, liner and sleeve from the frame.
10. Remove the sleeve from the liner and set aside.
11. Place the liner and cover into the liner holder rack.

Perform a Digestion 25
12. Remove the cover.
13. Transfer the sample from liner and proceed with work-up.

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

14. Inspect vessel components and replace worn or damged parts.

15. Clean vessels as outlined in “Vessel Cleaning ” section.

26 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.

Liner
1. Rinse the liners 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 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 using the microwave as outlined below. All vessel components must be dry before use.
4.1. Add 10 mL of acid type 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. Select and run the "Easy Prep Clean" method in the One Touch directory.
4.4. Wait for vessels to cool for a minimum of 15 minutes before opening microwave door.
4.5. Discard acid and rinse the liners and covers with deionized water.

Liner 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.

1. Place the liners on their side in an air oven at room temperature.

CAUTION
Only the liners should be placed in the air oven at 180 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 180 °C and let the liners warm slowly. Do not exceed an oven temperature of 190
°C.

Vessel Cleaning 27
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.
5. Remove the liners from the oven. The liners should be white in color, comparable to new liners with no acid
history.

Covers
1. Rinse the covers with deionized water and allow to dry completely before use. Shake covers to remove liquid
that might be trapped between the cover and ring.

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, & Screw

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

28 Vessel Cleaning
Vessel Distribution

Even Vessel Distribution

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 29
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.

One Touch Method Creation

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 230 °C. Higher temperatures will permanently damage
liner and sleeve.

5. Select “Sample Type” and choose the appropriate sample type from the list.
• “Organic” is the recommend sample type for most samples. Contact CEM before selecting any other sample
types.
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 1.48 or lower, enable “Temp-
Guard” as outlined below.
• Always use TempGuard
• Set the TempGuard limit at 30 °C > control temperature if control temperature is < 230 °C.
• Set the TempGuard limit at 20 °C > control temperature if control temperature is > 230 °C
• Limit TempGuard to 250 °C for digestion of organics with HNO3
• Limit TempGuard to 300 °C for H3PO4/H2SO4 applications
8. If applicable, select “Sample Prep Notes” and enter appropriate information.
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.

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

Classic Method Creation

Contact CEM Corporation before creating Classic Methods.

30 Methods
Fiber Optic Temperature Control

The Fiber Optic probe provides direct temperature measurement inside the control vessel. Fiber Optic is only
available for the EasyPrep and EasyPrep Plus vessels.

The "MTS-300 High Temp" (P/N 281461) Fiber Optic probe is required for applications running 250 ºC or greater
in temperature.

Fiber Optic Installation

If the vessel set requires fiber optic temperature control, install and enter the GF value as outlined below.
1. Connect the fiber optic probe to the port in the top center of the MARS 6 cavity by pushing in the plug until it
snaps into place
2. Select the System Settings icon in the bottom right corner of the screen.
3. Select Settings.
4. Select Sensors.

5. Select the current GF Number.

6. Using the Keyboard, enter the GF Number on the Fiber Optic Probe installed in the instrument. The GF number
can be found on the white connector on the probe. Each probe has a specific 7-digit GF number.

NOTE
Always ensure that the number on the probe and the number in the software are the same. If a new probe
is installed, then a new GF will need to be saved.

Fiber Optic Temperature Control 31

7. Once the number is properly entered, select “hide” to close the keyboard.
8. Save the GF number by selecting the Save icon located at the top right corner of the screen.
9. The current fiber optic temperature reading is located above the GF number. Verify the temperature reading at
room temperature.

NOTE
If “---” appears as the temperature, then the MARS 6 does not recognize the Fiber Optic Probe. The probe
is either not installed or is not working properly.

10. Press the Home icon in the lower left corner of the screen to return to the Home page.

Fiber Optic Temperature Verification

1. Select the System Settings icon in the bottom right corner of the screen.
2. Select Tools.
3. Select the "System" tab. The "FISO Temperature (ºC)" will appear under "Status".

4. Verify the temperature reading at room temperature.

• If the fiber optic probe is new or the temperature is not reading correctly, enter the GF number. See the
"Fiber Optic" section of the manual for details.
• If “---” appears as the temperature, then the MARS 6 does not recognize the Fiber Optic Probe. The probe is
either not installed or is not working properly. See the "Fiber Optic" section of the manual for details.
5. The probe can also be inserted into a beaker of warm water for temperature verification.
6. Press the Home icon in the lower left corner of the screen to return to the Home page.

Fiber Optic Care

Proper care and handling will insure the maximum lifetime from the fiber optic temperature probe.
• Store the fiber optic probe in a secure place when not in use.
• Do not leave the probe attached to the ceiling connector. If left inside the cavity, probes can be damaged or
broken by accidental contact.
• Remove any liquid or debris that gets on the probe with a wet paper towel. Start at the base of the connector
and gently pull toward the tip. Dry the probe before the next use.

32 Fiber Optic Temperature Control

Routine Maintenance

A routine maintenance protocol is vital for the long-term operation of the vessels. For maintenance instructions for
MARS 6 instrument, see the MARS 6 manual (P/N 600284) or 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 cavity, including the sensors, with a lint free damp cloth.

CAUTION
Only use water and a soft cloth to clean the system. Using other cleaning solutions, brushes, and
materials can cause damage to the device.

Daily
• If installed, remove the ESP-1500+ cable connection from the connector port and thoroughly clean the connector
with a paper towel or soft cloth. Thoroughly wipe and clean both the inside and outside surfaces of the
connector. If necessary, dampen the towel with isopropyl alcohol to assist in cleaning.

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 authorized dealer for information on CEM Service
contracts.

As Needed
• Bake-out Procedure: See "Liner Bake-out Procedure" for detailed instructions. The bake out procedure can be
used to remove residual acid vapors and other trapped gases from the Teflon® material.

Routine Maintenance 33
Troubleshooting

Problems and Possible Solutions

Problems Possible Cause Possible Solutions
TempGuard message appears during run Some vessels are hotter • See “Liner Bake-out Procedure” to reduce differences in
than others 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 < 230 °C.
(software version <1.49 • Set the TempGuard limit at 20 °C > control temperature if
control temperature is > 230 °C
• Limit TempGuard to 250 °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
sample type or sample vessels 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 Bake-out Procedure” to reduce differences in liners
than others
Some vessels contain acid See "Sample Preparation Safeguards" for specific details
blanks when running acid blanks.
Liner not getting as hot due Inspect vessel components and replace worn or damged
to leaking parts
Max Power Monitor message appears Vessels leaking Vessels possibly not assembled properly or not torqued using
during run torque tool
Turntable not aligned Perform turntable calibration as outlined in the MARS Manual
Corrosion on the cover ring Vessels are leaking • Select appropriate cover according to acid application.
Wrong cover (standard vs • Covers with delaminated rings and/or heavy corrosion
premium) used for acid should be replaced.
application. • Standard composite ring is recommended for applications
using primarily HNO3, HF, H2SO4, and H3PO4.
Cover soaked in acid bath
• Premium Cover (Titanium metal ring) is recommended for
non-HF applications where HCl and aqua regia are heavily
used
• Do not soak covers to clean. Rinse with water and allow to
dry before use.
• Covers with delaminated rings and/or heavy corrosion
should be replaced.
Corrosion on ESP-1500+ Pressure Exterior acid exposure • Do not leave pressure sensor in fume hood or other acidic
Sensor environment when not in use.
• Place the protective black rubber cap on the connector end
when not in use to minimize contact with acid fumes, dust,
and dirt.
• If pressure readings are erratic or sensor will not read
pressure, replace pressure sensor.

34 Troubleshooting
Problems Possible Cause Possible Solutions
Corrosion on torque wrench Exterior acid exposure • Do not leave torque wrench in fume hood or other acidic
environment
when not in use.
• Use the vessel loosening wrench to loosen screws (never for
torquing)
• If pressure readings are erratic or sensor will not read
pressure, replace pressure sensor.
Vessel Liner or sleeve appearance has Dark ring along bottom of Liner needs cleaning - See “Vessel Cleaning” section
changed liner
Liner not fitting into Sleeve Determine if liner or sleeve is problem. Invert sleeves after
every run to extend lifetime of liner and sleeve
Alligator skin on outside of Result of high heat/pressure. May be ok to run but will need
liner to be grouped with like vessels
Liner and/or Sleeve Discard - See “Vessel assembly” for preventative measures
distorted, flared or frayed
Sleeve has turned white (no Replace sleeve. To prevent sleeve damage, avoid high
longer golden brown) and/ temperatures for long periods of time. Wipe sleeves with
or stained on ends damp cloth and allow to dry if sleeve comes in contact with
acid.

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.

Troubleshooting 35
Glossary

Glossary

Classic Method Methods created by the user. Creation of a method requires training and knowledge.

DuoTemp Dynamically adjusts the “Control Vessel” to prevent excessive venting or exothermic
reactions when using infrared and fiber optic temperature control.

ESP-1500+ Provides pressure control for the MARS 6 system utilizing an internal Electronic Sensor
(Pressure) for Pressure (ESP).

Fiber Optic Probe Provides direct in situ temperature measurement of a reference vessel for rapid feedback
during both sealed and open vessel reactions.

Infrared (IR) Contactless, volume-independent sensors measure the temperature of all sealed vessels
during the run.

iWave Contactless, volume-independent sensors utilizing Light Emitting Technology™ (LET), that
accurately measures the temperature of the actual sample, not the outer surface of the
vessel.

One Touch Methods created by CEM Applications Specialists. Determines all of the parameters,
adjusts power output, and performs the digestion for all major sample types

MAXPower Aborts the run if full programmed power is applied continuously over a specified period of
time.

ReactiGuard Continuously monitors the cavity and disables the magnetron if disturbances occur inside
the cavity.

TempGuard Safety feature for measurement of temperature inside each vessel in the system. If the
temperature in any vessel surpasses the maximum allowable temperature programmed
during a method, the instrument software stops microwave production and indicates the
position of the vessel in which the temperature has exceeded the programmed limit. As
of software version 1.49, all TempGuard parameters are preset to CEM factory settings.

36 Glossary
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 is a registered trademark of CEM Part Number 600962
All Rights Reserved. This guide contains Corporation. MARS 6, TempGuard, EasyPrep, September 23, 2019
proprietary information which shall not and One Touch are trademarks of CEM Rev. 0
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.