CEM EasyPrep Vessel Owner's manual

Brand: CEM

Model: EasyPrep Vessel

Type: Owner's manual

EasyPrep Series

High Performance Vessels

Manual

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Contents

Safety Notations

Safety Notations 1

Introduction

About the EasyPrep™ Vessel Series 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

EasyPrep iWave Vessel Components 7

EasyPrep Plus Vessel Components 8

EasyPrep Vessel Components 10

Accessories 12

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

Classic Method Creation 30

Fiber Optic Temperature Control

Fiber Optic Installation 31

Fiber Optic Temperature Verication 32

Fiber Optic Care 32

Routine Maintenance

After Every Use 33

Daily 33

Weekly 33

Annually 33

As Needed 33

Troubleshooting

Problems and Possible Solutions 34

Contact Information 35

Glossary

Glossary 36

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1Safety 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.

2 Introduction

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 difcult 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 conguration, 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 Teon Insert Manual (P/N 600769) or contact CEM Corporation.

3Important Safeguards

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 specic 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

Hydrouoric 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% hydrouoric acid. Acid blanks must be

run separately.

4 Important Safeguards

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 ngers 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 congurations, 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 ber 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.

5Important 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.)

6 Vessel and Accessories Overview

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)

7Vessel 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

liner, cover and screw

Supports vessel liner Evenly distributes load from cover

Vessel Liner Standard Cover Premium Cover

P/N 432175 P/N 131125 P/N 131126

Contains acid and sample. 110 mL

Liner (5 -30 mL working volume)

Seals liner to contain acid and

sample

Seals liner to contain acid and

sample. Recommended for use with

HCl.

Frame Screw EasyPrep iWave Turntable

P/N 144996 P/N 404305

Uniformly provides pressure seal

among vessels when torqued

Holds assembled vessels inside

MARS iWave cavity and provides

rotation

8 Vessel and Accessories Overview

EasyPrep Plus Vessel Components

Frame Control Frame Sleeve

P/N 514050 P/N 514060 P/N 431740

Supports sleeve, load disc, vessel

liner, cover and screw

Fiber Optic Temperature and Pressure

Control: Supports sleeve, load disc,

vessel liner, cover and screw

Supports vessel liner

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:

Evenly distributes load from cover

Contains acid and sample. 110 mL

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

sample

Seals liner to contain acid and

sample. Recommended for use with

HCl.

Fiber Optic Temperature control: Seals

liner to contain acid and sample

9Vessel 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

control: Seals liner to contain acid

and sample

Fiber Optic Teperature control: Seals

liner to contain acid and sample.

Recommended for use with HCl

Fiber Optic Temperature and pressure

control: Seals liner to contain acid

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

among vessels when torqued

Fiber Optic Temperature Control:

Uniformly provides pressure seal

among vessels when torqued

Seals Pressure connector when ESP-

1500+ not in use

Sapphire Thermowell Thermowell Nut EasyPrep and EasyPrep Plus

Turntable

P/N 131173 P/N 325029 P/N 432100

Protects ber optic temperature probe Secures sapphire thermowell to

Control Cover

Holds assembled vessels inside

MARS 6 cavity and provides rotation

10 Vessel and Accessories Overview

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

liner, cover and screw

Fiber Optic Temperature Control:

Supports sleeve, load disc, vessel

liner, cover and screw

Fiber Optic Temperature and Pressure

Control: Supports sleeve, load disc,

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

Liner (6 -30 mL) working volume)

Seals liner to contain acid and

sample

Seals liner to contain acid and

sample. Recommended for use with

HCl

11Vessel 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:

Seals liner to contain acid and

sample

Fiber Optic Temperature and pressure

control: Seals liner to contain acid

and sample

Fiber Optic Temperature control:

Seals liner to contain acid and

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

control: Seals liner to contain acid

and sample. Recommended for use

with HCl.

Uniformly provides pressure seal

among vessels when torqued

Fiber Optic Temperature Control:

Uniformly provides pressure seal

among vessels when torqued

Pressure Nut EasyPrep and EasyPrep Plus

Turntable

P/N 431311 P/N 432100

Seals Pressure connector when ESP-

1500+ not in use

Holds assembled vessels inside

MARS 6 cavity and provides rotation

12 New Liner and Cover Conditioning

Accessories

Torque Tool Vessel Loosening Wrench Torque Stand

P/N 514140 P/N 430660 P/N 144925

Provides appropriate vessel seal (84

inches per pound (7 ft-lbs))

Removes frame screw. Holds Vessels in place while torquing

Vessel Liner Holder

P/N 166222

Holds up to a set of 16 vessel liners

13New 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 Teon® 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 Teon. 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 Teon 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.

14 New Liner and Cover Conditioning

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 Teon. 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 Teon 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.

15Perform a Digestion

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 congurations 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

congurations.

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 specic 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.

16 Perform a Digestion

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 nger 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.

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CEM EasyPrep Vessel Owner's manual

CEM EasyPrep Vessel Owner's manual

CEM EasyPrep Vessel Owner's manual

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