CEM Corporation

P.O. Box 200

Matthews, NC 28106
United States

Tel: (800) 726-3331 [USA & Canada]

Tel: (704) 821-7015
Fax: (704) 821-7894
e-mail: info@cem.com
www.cem.com
UNITED KINGDOM
CEM Microwave Technology Ltd.
2 Middle Slade
Buckingham Industrial Park
Buckingham MK18 1WA
Tel: (44) 1280-822873

Our commitment to you does not end

Fax: (44) 1280-822873
e-mail: info.uk@cem.com
User Guidelines
when your system is shipped; it begins. GERMANY General Guidelines to Assist with Microwave Digestion Method Development
CEM GmbH
Carl-Friedrich-Gauss -Str. 9
47475 Kamp-Lintfort
Tel: (49) 2842-9644-0
Fax: (49) 2842-9644-11
e-mail: info@cem.de
www.cem.de

ITALY
CEM S.R.L.
Via Dell’ Artigianato, 6/8
24055 Cologno al Serio (Bg)
Tel: (39) 35-896224
Fax: (39) 35-891661
e-mail: info.srl@cem.com
www.cemmicroonde.it

FRANCE
Applications Support Team CEM μWave S.A.S.
Immeuble Ariane
Domaine Technologique de Saclay
4, rue Rene’ Razel
91892 ORSAY Cedex
Tel: (33-1) 69 35 57 80
e-mail: info.fr@cem.com
www.cemfrance.fr

JAPAN
CEM Japan K.K.
5-8-8 Shinjuku
Shinjuku-Ku, Tokyo
160-0022
Tel: +03-5368-2507
Fax: +03-5368-2508
e-mail: info@cemjapan.jp
www.cemjapan.jp

IRELAND
CEM Technology (Ireland) Ltd
Sky Business Centre
9a Plato Business Park
Damastown
Dublin 15
Tel +353 (0)1 885 1752
Fax +353 (0)1 885 1601 600288
Email: info.ireland@cem.com Rev. 1

Rev. 1
Safety Concerns with Microwave Digestion
The MARS 6 Operation Manual includes sections “Compounds
Unsuitable for Closed Vessel Microwave Digestion” and “Chemical
Safety Concerns at High Temperatures.” These sections should be
read prior to preparing samples for digestion.
Sample Preparation Guidelines
If available, please follow the methods and guidelines that have
been developed for your samples. If a method has not been
developed, the recommendations offered in this document are
only guidelines to assist with method development. They may not
pertain to your exact sample, your metal analyte of interest in the
sample, or your specific microwave digestion vessel. If you have
additional questions after reading these guidelines, please contact
CEM for applications support.
Organic Materials
Organic Material Examples: Plant and Animal Tissues, Foods, Oils
and Oily Waste, Paint Chips, Polymers
Important Note: Digestion of organic materials results in an
exothermic reaction that produces heat and increases pressure in
the microwave digestion vessel.
Recommended Sample Mass: For all vessels, start with 0.1 gram
sample size. When using an XP-1500, EasyPrep, or EasyPrep Plus
vessel, watch that the pressure does not exceed 800 psi and the
vessel does not vent excessively. When using a MARSXpress or
MARSXpress Plus vessel, watch that the vessels do not vent exces-
sively. If the acid volume loss during the digestion is less than 2 mL
in each vessel and/or analyte recovery is acceptable, then the sample
mass can be increased and tested again at 0.25 grams. This test can
be repeated with 0.5, 0.75, and 1.0 grams.
Recommended Acid: 10 mL of Nitric Acid (70%)
Recommended Digestion Temperatures: 180 – 210 oC
Minimum Number of Vessels: For the EasyPrep and EasyPrep Plus,
the minimum number of vessels is one. For the MARSXpress and
MARSXpress Plus, the minimum number of vessels is eight.
Sample Predigestion: The addition of acid to some organic samples
can cause a reaction that will result in an increase of temperature
and escape of gases, which is known as predigestion. We recom-
mend that you to allow organic samples to predigest for 30 minutes
in uncovered microwave vessels in the fume hood.
MARS 6 Software Method Selection: Select a MARS 6 One Touch
Method similar to your sample type. If there is not a One Touch
Method for your sample, create a new Classic Method. When creat-
ing a new Classic Method, select Ramp-to-Temperature as the Control
Type, a ramp time of 20 – 25 minutes, and a hold time of 15 minutes.
Finishing the Sample Preparation: Prior to metals analysis, the
digested sample will require dilution. Digested samples are usually
diluted to 25 or 50 mL in a volumetric flask. A diluted sample solution
that is completely digested will be clear (not cloudy) and free of
particles. It may or may not be colorless. A solution that contains
particles can be centrifuged or filtered prior to analysis, but analyte
recovery should be measured.
Inorganic Materials Notes
Inorganic Material Examples: Soils, Ores, Ceramics, Catalysts, Metal
Alloys, Ash, Water
Important Notes: Digestion of inorganic materials usually produces
less heat and pressure than organic digestions. Inorganic materials
cover a large range of sample types. Each of these sample types
requires different acid mixtures and digestion temperatures. For
these reasons, it is very difficult to specify exact conditions.
Recommended Sample Mass: For all vessels, start with a sample
size of 0.1 grams. A sample that has more surface area will digest
quicker than samples with less surface area. Therefore, try to use
several smaller pieces of sample instead of one large piece. Watch
the digestion and make sure the vessels do not vent excessively. If
the acid volume loss during the digestion is less than 2 mL in each
vessel and/or analyte recovery is acceptable, then the sample mass
can be increased and tested again at 0.25 grams. This test can be
repeated with 0.5, 0.75, and 1.0 grams.
Recommended Acid and Digestion Temperature:
Alloys – HNO3, HCl, HF. In general, an acid mixture is required to
digest most samples with digestion temperatures of 200 – 210 oC.
For example:
l NiCr, Steel, Cobalt Alloy, Tungsten Alloy – HNO3, HF
l Aluminum and Iron Alloys – HCl, HF
l Aluminum – HCl, HNO3 (3:1)
l Precious Metals – HCl, HNO3 (3:1) at 180 – 210 oC
Ceramics and Catalysts – In general, an acid mixture is required to
digest most samples with digestion temperatures of 180 – 210 oC.
For example:
l Aluminum Oxide – H3PO4, H2SO4 at 270 oC
l Silicon Dioxide – HF, HNO3 at 180 oC
l Ores, Silicates, Ash – HNO3, HCl, HF at 180 – 210 oC
Recommended Acid Volume: 10 mL
Minimum Number of Vessels: For the EasyPrep and EasyPrep Plus,
the minimum number of vessels is one. For the MARSXpress and
MARSXpress Plus, the minimum number of vessels is eight.
Sample predigestion is not usually needed.
MARS 6 Software Method Selection: Select a MARS 6 One Touch
Method similar to your sample type. If there is not a One Touch
Method for your sample, create a new Classic Method. When creating
a new Classic Method, select Ramp-to-Temperature as the Control
Type. Select a ramp time of 20 – 25 minutes and a hold time of 20
minutes; this will work for most samples that digest at 180 – 210 oC.
Samples that digest at 230 – 270 oC will require a ramp time of 30 –
45 minutes and a hold time of 20 – 40 minutes.
Finishing the Sample Preparation: Prior to metals analysis, the
digested sample will require dilution. Digested samples are usually
diluted to 25 or 50 mL in a volumetric flask. A diluted sample solution
that is completely digested will be clear (not cloudy) and free of
particles. It may or may not be colorless. A solution that contains
particles can be centrifuged or filtered prior to analysis, but analyte
recovery should be measured.
 Recommended distribution of EasyPrep, EasyPrep Plus One Touch Method General Guidelines Icon Reference Guide
and XP-1500 vessels in the turntable General Precautions
l The One Touch Methods and sample preparation procedures are
System Setting
1 2 3 a reference point for sample digestion using a CEM system and
may need to be modified or changed to obtain the required
results for your sample. Screen Context Menu
l The control (reference) vessel should contain the largest and
most reactive sample. Classic Menu
l Sample digestion requires concentrated acids.
l To avoid the potential for chemical burns, manual venting
of CEM vessels should only be performed when the vessel One Touch Method
contents are at room temperature and hand, eye, and body
protection should be worn. Always open vessels in a fume
Back
hood and point the vent hole away from the operator.
4 5 6
Home
Samples that Quickly Produce Heat and Gas
l Allow samples to predigest by standing open for a minimum of
30 minutes in a fume hood before sealing vessels and proceeding Done
to heating program.
Info
Samples that Require Hydrofluoric Acid (HF)
l If insoluble fluoride compounds are formed when using HF, Run
a boric acid solution should be used to complex and dissolve
these compounds. Edit
l Use 10 mL of 4% w/v boric acid solution per 1 mL of HF Delete
7 8 9
l Alternatively, 1 – 4 grams of solid boric acid and 25 mL of
deionized water can be used in place of the 4% w/v solution. New
l After the digestion is complete, add the boric acid to the
vessel and reseal. Run the “Boric Acid HF Neutralization” Save
One Touch Method.
Add Stage
Samples with Large Pieces
l Reducing the particle size increases the efficiency of digestion Remove Stage
and may decrease the digestion time. Make sure the particles
are well suspended in the acid mixture prior to heating. Fiberoptic
10 11 12
Stabilization of Ag, Ba, Sb, Fe, and Al Infrared
l The addition of HCl is appropriate for the stabilization of Ag,
Ba, and Sb, and high concentrations of Fe and Al in solution. DuoTemp
The amount of HCl will vary depending on the matrix and the
concentration of the analytes. The addition of HCl acid may,
however, limit the techniques or increase the difficulties of Turntable
analysis.
Blower
Samples Resistant to Oxidation
l The “Char-Sulfuric Acid” One Touch Method is for the pretreat- Print
ment of large organic sample sizes or difficult organic samples
that are resistant to oxidation. After the char is complete, the Temperature
= control vessel vessel is opened and a normal oxidation with nitric acid can
be run, usually at around 200 oC. Pressure

l Inspect the vessel at the end of the char step to ensure the Power
= standard vessel sample has the appearance of a homogenous black liquor. It
may be necessary to repeat the char step for some especially
resistant samples.
 Recommended distribution of MARSXpress vessels when turntable is less than capacity Recommended distribution of MARSXpress Plus vessels in the turntable

8 10 12 14
2 4 6 8

16 18 20 22
10 12 14 16

24 26 28 30
18 20 22 24

32 34 36 38

7 15

Incorrect distribution: What not to do

XXX = control vessel

= standard vessel
 Recommended distribution of EasyPrep, EasyPrep Plus One Touch Method General Guidelines Icon Reference Guide
and XP-1500 vessels in the turntable General Precautions
l The One Touch Methods and sample preparation procedures are
System Setting
1 2 3 a reference point for sample digestion using a CEM system and
may need to be modified or changed to obtain the required
results for your sample. Screen Context Menu
l The control (reference) vessel should contain the largest and
most reactive sample. Classic Menu
l Sample digestion requires concentrated acids.
l To avoid the potential for chemical burns, manual venting
of CEM vessels should only be performed when the vessel One Touch Method
contents are at room temperature and hand, eye, and body
protection should be worn. Always open vessels in a fume
Back
hood and point the vent hole away from the operator.
4 5 6
Home
Samples that Quickly Produce Heat and Gas
l Allow samples to predigest by standing open for a minimum of
30 minutes in a fume hood before sealing vessels and proceeding Done
to heating program.
Info
Samples that Require Hydrofluoric Acid (HF)
l If insoluble fluoride compounds are formed when using HF, Run
a boric acid solution should be used to complex and dissolve
these compounds. Edit
l Use 10 mL of 4% w/v boric acid solution per 1 mL of HF Delete
7 8 9
l Alternatively, 1 – 4 grams of solid boric acid and 25 mL of
deionized water can be used in place of the 4% w/v solution. New
l After the digestion is complete, add the boric acid to the
vessel and reseal. Run the “Boric Acid HF Neutralization” Save
One Touch Method.
Add Stage
Samples with Large Pieces
l Reducing the particle size increases the efficiency of digestion Remove Stage
and may decrease the digestion time. Make sure the particles
are well suspended in the acid mixture prior to heating. Fiberoptic
10 11 12
Stabilization of Ag, Ba, Sb, Fe, and Al Infrared
l The addition of HCl is appropriate for the stabilization of Ag,
Ba, and Sb, and high concentrations of Fe and Al in solution. DuoTemp
The amount of HCl will vary depending on the matrix and the
concentration of the analytes. The addition of HCl acid may,
however, limit the techniques or increase the difficulties of Turntable
analysis.
Blower
Samples Resistant to Oxidation
l The “Char-Sulfuric Acid” One Touch Method is for the pretreat- Print
ment of large organic sample sizes or difficult organic samples
that are resistant to oxidation. After the char is complete, the Temperature
= control vessel vessel is opened and a normal oxidation with nitric acid can
be run, usually at around 200 oC. Pressure

l Inspect the vessel at the end of the char step to ensure the Power
= standard vessel sample has the appearance of a homogenous black liquor. It
may be necessary to repeat the char step for some especially
resistant samples.
 Recommended distribution of MARSXpress vessels when turntable is less than capacity Recommended distribution of MARSXpress Plus vessels in the turntable

8 10 12 14
2 4 6 8

16 18 20 22
10 12 14 16

24 26 28 30
18 20 22 24

32 34 36 38

7 15

Incorrect distribution: What not to do

XXX = control vessel

= standard vessel
Safety Concerns with Microwave Digestion
The MARS 6 Operation Manual includes sections “Compounds
Unsuitable for Closed Vessel Microwave Digestion” and “Chemical
Safety Concerns at High Temperatures.” These sections should be
read prior to preparing samples for digestion.
Sample Preparation Guidelines
If available, please follow the methods and guidelines that have
been developed for your samples. If a method has not been
developed, the recommendations offered in this document are
only guidelines to assist with method development. They may not
pertain to your exact sample, your metal analyte of interest in the
sample, or your specific microwave digestion vessel. If you have
additional questions after reading these guidelines, please contact
CEM for applications support.
Organic Materials
Organic Material Examples: Plant and Animal Tissues, Foods, Oils
and Oily Waste, Paint Chips, Polymers
Important Note: Digestion of organic materials results in an
exothermic reaction that produces heat and increases pressure in
the microwave digestion vessel.
Recommended Sample Mass: For all vessels, start with 0.1 gram
sample size. When using an XP-1500, EasyPrep, or EasyPrep Plus
vessel, watch that the pressure does not exceed 800 psi and the
vessel does not vent excessively. When using a MARSXpress or
MARSXpress Plus vessel, watch that the vessels do not vent exces-
sively. If the acid volume loss during the digestion is less than 2 mL
in each vessel and/or analyte recovery is acceptable, then the sample
mass can be increased and tested again at 0.25 grams. This test can
be repeated with 0.5, 0.75, and 1.0 grams.
Recommended Acid: 10 mL of Nitric Acid (70%)
Recommended Digestion Temperatures: 180 – 210 oC
Minimum Number of Vessels: For the EasyPrep and EasyPrep Plus,
the minimum number of vessels is one. For the MARSXpress and
MARSXpress Plus, the minimum number of vessels is eight.
Sample Predigestion: The addition of acid to some organic samples
can cause a reaction that will result in an increase of temperature
and escape of gases, which is known as predigestion. We recom-
mend that you to allow organic samples to predigest for 30 minutes
in uncovered microwave vessels in the fume hood.
MARS 6 Software Method Selection: Select a MARS 6 One Touch
Method similar to your sample type. If there is not a One Touch
Method for your sample, create a new Classic Method. When creat-
ing a new Classic Method, select Ramp-to-Temperature as the Control
Type, a ramp time of 20 – 25 minutes, and a hold time of 15 minutes.
Finishing the Sample Preparation: Prior to metals analysis, the
digested sample will require dilution. Digested samples are usually
diluted to 25 or 50 mL in a volumetric flask. A diluted sample solution
that is completely digested will be clear (not cloudy) and free of
particles. It may or may not be colorless. A solution that contains
particles can be centrifuged or filtered prior to analysis, but analyte
recovery should be measured.
Inorganic Materials Notes
Inorganic Material Examples: Soils, Ores, Ceramics, Catalysts, Metal
Alloys, Ash, Water
Important Notes: Digestion of inorganic materials usually produces
less heat and pressure than organic digestions. Inorganic materials
cover a large range of sample types. Each of these sample types
requires different acid mixtures and digestion temperatures. For
these reasons, it is very difficult to specify exact conditions.
Recommended Sample Mass: For all vessels, start with a sample
size of 0.1 grams. A sample that has more surface area will digest
quicker than samples with less surface area. Therefore, try to use
several smaller pieces of sample instead of one large piece. Watch
the digestion and make sure the vessels do not vent excessively. If
the acid volume loss during the digestion is less than 2 mL in each
vessel and/or analyte recovery is acceptable, then the sample mass
can be increased and tested again at 0.25 grams. This test can be
repeated with 0.5, 0.75, and 1.0 grams.
Recommended Acid and Digestion Temperature:
Alloys – HNO3, HCl, HF. In general, an acid mixture is required to
digest most samples with digestion temperatures of 200 – 210 oC.
For example:
l NiCr, Steel, Cobalt Alloy, Tungsten Alloy – HNO3, HF
l Aluminum and Iron Alloys – HCl, HF
l Aluminum – HCl, HNO3 (3:1)
l Precious Metals – HCl, HNO3 (3:1) at 180 – 210 oC
Ceramics and Catalysts – In general, an acid mixture is required to
digest most samples with digestion temperatures of 180 – 210 oC.
For example:
l Aluminum Oxide – H3PO4, H2SO4 at 270 oC
l Silicon Dioxide – HF, HNO3 at 180 oC
l Ores, Silicates, Ash – HNO3, HCl, HF at 180 – 210 oC
Recommended Acid Volume: 10 mL
Minimum Number of Vessels: For the EasyPrep and EasyPrep Plus,
the minimum number of vessels is one. For the MARSXpress and
MARSXpress Plus, the minimum number of vessels is eight.
Sample predigestion is not usually needed.
MARS 6 Software Method Selection: Select a MARS 6 One Touch
Method similar to your sample type. If there is not a One Touch
Method for your sample, create a new Classic Method. When creating
a new Classic Method, select Ramp-to-Temperature as the Control
Type. Select a ramp time of 20 – 25 minutes and a hold time of 20
minutes; this will work for most samples that digest at 180 – 210 oC.
Samples that digest at 230 – 270 oC will require a ramp time of 30 –
45 minutes and a hold time of 20 – 40 minutes.
Finishing the Sample Preparation: Prior to metals analysis, the
digested sample will require dilution. Digested samples are usually
diluted to 25 or 50 mL in a volumetric flask. A diluted sample solution
that is completely digested will be clear (not cloudy) and free of
particles. It may or may not be colorless. A solution that contains
particles can be centrifuged or filtered prior to analysis, but analyte
recovery should be measured.
 CEM Corporation
P.O. Box 200
Matthews, NC 28106
United States

Tel: (800) 726-3331 [USA & Canada]

Tel: (704) 821-7015
Fax: (704) 821-7894
e-mail: info@cem.com
www.cem.com
UNITED KINGDOM
CEM Microwave Technology Ltd.
2 Middle Slade
Buckingham Industrial Park
Buckingham MK18 1WA
Tel: (44) 1280-822873

Our commitment to you does not end

Fax: (44) 1280-822873
e-mail: info.uk@cem.com
User Guidelines
when your system is shipped; it begins. GERMANY General Guidelines to Assist with Microwave Digestion Method Development
CEM GmbH
Carl-Friedrich-Gauss -Str. 9
47475 Kamp-Lintfort
Tel: (49) 2842-9644-0
Fax: (49) 2842-9644-11
e-mail: info@cem.de
www.cem.de

ITALY
CEM S.R.L.
Via Dell’ Artigianato, 6/8
24055 Cologno al Serio (Bg)
Tel: (39) 35-896224
Fax: (39) 35-891661
e-mail: info.srl@cem.com
www.cemmicroonde.it

FRANCE
Applications Support Team CEM μWave S.A.S.
Immeuble Ariane
Domaine Technologique de Saclay
4, rue Rene’ Razel
91892 ORSAY Cedex
Tel: (33-1) 69 35 57 80
e-mail: info.fr@cem.com
www.cemfrance.fr

JAPAN
CEM Japan K.K.
5-8-8 Shinjuku
Shinjuku-Ku, Tokyo
160-0022
Tel: +03-5368-2507
Fax: +03-5368-2508
e-mail: info@cemjapan.jp
www.cemjapan.jp

IRELAND
CEM Technology (Ireland) Ltd
Sky Business Centre
9a Plato Business Park
Damastown
Dublin 15
Tel +353 (0)1 885 1752
Fax +353 (0)1 885 1601 600288
Email: info.ireland@cem.com Rev. 1

Rev. 1