Microwave Acid Digestion Method Note...

MARS 6Microwave Acid Digestion

Method Note Compendium

Updated January 31, 2018

Contents

Agriculture

Boric Acid HF Neutralization 2

Coffee Beans 3

Cotton 4

Feed Grain 5

Fertilizer AOAC Method 2006.03 6

Plant Tissue 7

Soybean 8

Spinach Leaves 9

Straw 10

Tobacco 11

Wheat 12

Yeast 13

Clinical and Biological

Animal Tissue (Dry) 15

Animal Tissue (Wet) 16

Blood (Human) 17

Bovine Liver (Wet) 18

Hair 19

Lobster Hepatopancreas (Tort2-CRM) 20

Urine (Human) 21

Consumer Products


Cosmetics (Liquid Foundation) 24

Cotton 25

Eye Shadow 26

Shampoo (Dandruff) 27

Suppository (Capsule) 28

Vaseline 29

Wax (Candle) 30

Environmental and Regulatory


Fertilizer - AOAC Method 2006.03 33

Limestone 34

NPDES (Wastewater) 35

Pine Needles 36

RoHS (For Pb, Hg, and Cd Analysis) 37

Sediment (BCCS-1 CRM) (Leach) 38

Sediment (Buffalo River) (Leach) 39

Sludge (Industrial) 40

Sludge (Waste Activated) 41

Soil (Montana-CRM) (Leach) 42

TCLP Extract 43

US EPA 3015 (Aqueous Samples) 44

US EPA 3015a (Aqueous Samples) 45

US EPA 3051 (Solid Samples) 46

US EPA 3051a (Solid Samples) 47

US EPA 3052 48

USP 232/233 (Pharmaceuticals) 49

Water (for analysis of Phosphorus) 50

Wood 51

Food Testing

Apple 53

Asparagus 54

Bacon (Cooked Pieces) 55

Beef (Ground) 56

Beer (Light) 57

Blueberry 58

Broccoli 59

Caramel Color 60

Carrot 61

Celery 62

Cheese Crackers 63

Cheese (Processed) 64

Cherry 65

Chewing Gum 66

Chicken (Boneless) 67

Chili Candy (Mexican) 68

Chips (Potato) 69

Coffee Beans 70

Cucumber 71

Dog Food (Dry) 72

Dog Food (Wet) 73

Flour 74

Food Coloring (Liquid) 75

Food 76

Fruit Juice 77

Granola Bar 78

Grape 79

Grapefruit 80

Ham 81

Infant Cereal (Rice Grain) 82

Infant Formula (Liquid) 83

Infant Formula (Liquid) in iPrep Vessels 84

Infant Formula (Powder) 85

Infant Formula (Powder) in iPrep Vessels 86

Kidney Bean 87

Maple Syrup 88

Mayonnaise 89

Milk (Liquid, Whole) 90

Milk (Powder) 91

Nutritional Drink (Adult) 92

Olive Oil 93

Orange 94

Orange Juice 95

Peanut Butter 96

Pear 97

Pepper (Bell, Chili, etc.) 98

Pizza (Frozen, Pepperoni) 99

Plum 100

Pork Gelatin 101

Pork (Ground) 102

Potato 103

Pretzel (Salted) 104

Protein Bar 105

Raspberry 106

Rice 107

Safflower Oil 108

Salami 109

Sausage 110

Soda (Diet) 111

Soybean 112

Spinach 113

Spinach Leaves 114

Strawberry 115

Sugar (Granulated) 116

Tea Leaves 117

Tomato Leaves 118

Tomato Soup 119

Walnut (Ground) 120

Watermelon 121

Whey Powder 122

Wine 123

Yogurt (Plain) 124

Geoscience and Mining

Alpha - Alumina in iPrep Vessels 126

Aluminum Oxide 127

Automotive Catalyst 128

Bauxite (Step 1 of 2) 129

Bauxite (Step 2 of 2) 130


Carbon 132

Carbon Nanotubes 133

Cement 134

Ceramic (Fused Silica) 135

Ceramics 136

Char (Sulfuric Acid) 137

Clay 138

Coal 139

Coal in iPrep Vessels 140

Coal Ash 141

Diesel Fuel 142

Iron Ore 143

Kerosene 144

Limestone 145

Mill Tailings (Step 1 of 2) 146

Mill Tailings (Step 2 of 2) 147

Motor Oil (Waste) 148

Petroleum Coke (Step 1 of 2) 149

Petroleum Coke (Step 2 of 2) 150

Rock (Pulverized) 151

Rutile Ore 152

Sand 153

Silica Sand 154

Silicon Dioxide 155

Silicon Wafer 156

Slag (Furnace) 157

Titanium Dioxide 158

Tungsten Carbide 159

Tungsten Oxide 160

Zeolite 161

Industrial Hygiene

Filter Paper (Cellulose) 163

Filter (37 mm Mixed Cellulose Ester) 164

Filter (47 mm Polycarbonate) 165

Ghost Wipe 166

Toray Filter in iPrep Vessels 167

Materials Science

Circuit Board (Cryo-ground) 169

Glass (Ground) 170

Graphite Fiber (Epoxy Resin, Fiber Content) 171

Metals and Alloys

Alluminum Alloy 173

Alpha - Alumina in iPrep Vessels 174

Aluminum Oxide 175

Aluminum (Metal) 176

Copper (Metal) 177

Copper (Ore) 178

Metal Alloy (CoCr) (Step 1 of 2) 179

Metal Alloy (CoCr) (Step 2 of 2) 180

Metal Alloy (FeCr) 181

Metal Alloy (NiCr) 182

Nickel (Metal) 183

Platinum (Metal) 184

Precious Metal (Ore) (Step 1 of 2) 185

Precious Metal (Ore) (Step 2 of 2) 186

Selenium Alloy 187

SnAg Solder 188

Stainless Steel 189

Steel (Stainless) 190

Titanium Alloy 191

Titanium Dioxide 192

Zinc Oxide 193

Nutraceuticals

Biotin 195

Ginko (Ground) 196

Ginko (Whole Pill) 197

Infant Formula (Liquid) 198

Infant Formula (Liquid) in iPrep Vessels 199

Infant Formula (Powder) 200

Infant Formula (Powder) in iPrep Vessels 201

Kelp 202

Milk (Liquid, Whole) 203

Milk (Powder) 204

Plant Tissue 205


Wheat 207

Whey Powder 208

Organic Chemicals

Photoresist 210

Paints and Coatings

Paint (Latex Based Liquid) 212

Paint Chips (For Pb Analysis) 213

Photoresist 214

Toner (Ink) in iPrep Vessels 215

Personal Care (Health and Beauty)


Cosmetics (Liquid, Foundation) 218

Eye Shadow 219

Shampoo (Dandruff) 220

Pharmaceutical and Biotech

Allergy Pill (Ground) 222

Allergy Pill (Whole Pill) 223

Antioxidant (Ground) 224

Antioxidant (Whole Pill) 225

APIs with Aromatic Ring Structures in iPrep Vessels 226

Ascorbic Acid 227

Aspirin (Ground) 228

Aspirin (Whole) 229

Beta Carotene 230

Biotin 231

Calcium Carbonate 232

Calpan Pantothenic Acid 233

Cephalexin 234

Chromium Chelate 235

Cold and Flu Medicine (Liquid) 236

Cupric Sulfate 237

Diclofenac K 238

Empty Capsule (Gel) 239

Fish Oil (No Capsule) 240

Folic Acid 241

Ginko (Ground) 242

Ginko (Whole Pill) 243

Kelp 244

Losataran K 245

Magnesium Carbonate 246

Magnesium Oxide 247

Manganese Carbonate 248

Metaformin (Ground) 249

Multivitamin (Ground) 250

Multivitamin (Whole) 251

Niacinamide 252

Pantothenic Acid 253

Potassium Chelate 254

Pyridoxine 255

Riboflavin 256

Selenium Chelate 257

Stearic Acid 258

Thiamine 259


Vitamin B-12 261

Vitamin C (Ground) 262

Vitamin C (Whole) 263

Vitamin D 264

Vitamin D3 265

Vitamin E 266

Vitamins 267

Zinc Sulfate 268

Plastics, Polymers, and Oils

Acrylamide 270

Bunker Oil 271

Bunker Oil in iPrep Vessels 272

Char (Sulfuric Acid) 273

Crude Oil 274

Diesel Fuel 275

Epoxy Hardener 276

Fatty Alcohol 277

Gasoline 278

HDPE (High Density Polyethylene) 279

Kerosene 280

Kevlar in iPrep Vessels 281

Lube Oil 282

Mineral Oil 283

Motor Oil (Waste) 284

Motor Oil (Waste) in iPrep Vessels 285

Nylon 286

PET (Polyethylene Terephthalate) 287

PET (Polyethylene Terephthalate) in iPrep Vessels 288

Polycarbonate Resin (Step 1 of 2) 289

Polycarbonate Resin (Step 2 of 2) 290

Polyethersulfone (Filter Paper) 291

Polypropylene 292

Polyurethane 293

PVC (Polyvinyl Chloride, Resin) 294

Rubber 295

Terephthalic Acid 296

Pulp and Paper

Filter Paper (Cellulose) 298

Filter (37 mm Mixed Cellulose Ester) 299

Filter (47 mm Polycarbonate) 300

Paper Pulp 301

Water and Wastewater Treatment

NPDES (Wastewater) 303

Sludge (Industrial) 304

Sludge (Waste Activated) 305

TCLP Extract 306

US EPA 3015 (Aqueous Samples) 307

US EPA 3015a (Aqueous Samples) 308

Water (for Analysis of Phosphorus) 309

Agriculture

2

Procedure

Notes

Recommended Equipment Recommended Vessels

Microwave Digestion of

Heating Program

1

Ramp (mm:ss) Hold (mm:ss) Pressure (psi) Power (W) StirringStage Temp (°C)

Control Type Method Type

Reagents

Max Sample Weight Sample Type

www.cem.com Form prepared by:

MARS 6TM

Method Note

Results

General Precautions

* Ramp times and power may vary depending on type and number of vessels.

Boric Acid HF Neutralization

Allow vessel to cool. Add 30 ml H3BO3 (4%) into the vessel that contains the sample and acid.

This procedure can be used if it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed by reaction ofcertain analytes with hydrofluoric acid.

Alternatively, 1-4g of solid H3BO3 + 25mL deionized H2O can be used in place of the 4% w/v solution.

MARS 6MARS 6 iWave

EasyPrepEasyPrep Plus

H3BO3 (4%)

Varies by Sample Organic Ramp to Temperature One Touch

170 15:00 15:00 800 900-1050 Off

See sample specific method notes.

a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results onyour sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Microwave Digestion ofBoric Acid HF Neutralization

3

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Coffee Beans

Weigh 0.5 g of ground sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.

The addition of Conc. HCl (0-4mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. Theamount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit thetechniques or increase the difficulties of analysis.

MARS 6MARS 6 iWave

EasyPrepEasyPrep PlusXpressXpress Plus

HNO3

0.5 g Organic Ramp to Temperature One Touch

200 20:00 15:00 800 900-1050 Off

Sample was clear, colorless, and particle free upon dilution to 50 ml.


Microwave Digestion ofCoffee Beans

4

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cotton

Weigh 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave

XpressXpressPlusEasyPrepEasyPrep Plus

HNO3


200 15:00 15:00 800 900-1050 Off

Sample was clear, colorless, and particle free upon dilution to 50 mL.


Microwave Digestion ofCotton

5

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Feed Grain

Weigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3, and 2 ml of HCl. Gently swirl the mixtureand wait approximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave

XpressXpress PlusEasyPrepEasyPrep Plus

HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFeed Grain

6

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Fertilizer-AOAC Method 2006.03

Weigh 1 g (0.5 g for organic matrices) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


This method may not provide a total digest of all fertilizer samples. Hydrofluoric acid will be required to provide complete digestion of somesample matrixes.

MARS 6MARS 6 iWave


HNO3HCl

1 g Organic Ramp to Temperature One Touch

200 15:00 20:00 800 900-1050 Off



Microwave Digestion ofFertilizer AOAC Method 2006.03

7

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Plant Tissue

Weigh 0.5 g of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


Some plant tissues contain silicates which would require HF for total dissolution.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPlant Tissue

8

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Soybean



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSoybean

9

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Spinach Leaves




MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSpinach Leaves

10

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Straw

Weigh 0.5 g of the sample into the digestion vessel. Add 10 ml of HNO3, and 1 ml of HF. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluoridesformed, an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled“Boric HF Neutralization”


MARS 6MARS 6 iWave


HNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofStraw

11

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Tobacco


The use of HF may be required to digest any silicates found in the sample.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofTobacco

12

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Wheat



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWheat

13

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Yeast

Weigh 1.0 g of dry weight (0.5 g w/Xpress vessels) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofYeast

Clinical and Biological

15

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Animal Tissue (Dry)

Weigh 0.5 g (0.25 g w/Xpress Vessels) into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

The addition of Conc. HCl (0-4 ml) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. Theamount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit thetechniques or increase the difficulties of analysis.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAnimal Tissue (Dry)

16

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Animal Tissue (Wet)

Weigh 1 g wet weight (0.5 g w Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAnimal Tissue (Wet)

17

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Blood (Human)

Weigh 2 ml of the sample into the digestion vessel. Add 5 ml of HNO3 and 2 ml of H2O2. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

Take caution when mixing the acids and the sample. The sample may foam slightly.

MARS 6MARS 6 iWave


HNO3H2O2

2 ml Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBlood (Human)

18

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Bovine Liver (Wet)

Weigh 1.0 g wet weight (0.5 g w/Xpress Vessels) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBovine Liver (Wet)

19

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Hair

Weigh 0.25 g of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture before closing the vessel.

MARS 6MARS 6 iWave


HNO3


180 15:00 15:00 800 900-1050 Off

Sample was clear, colorless and particle free upon dilution to 50 ml.


Microwave Digestion ofHair

20

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Lobster Hepatopancreas (Tort-2 CRM)

Weigh 1.0 g dry weight (0.5 g w/Xpress Vessels) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofLobster Hepatopancreas (Tort2-CRM)

21

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Urine (Human)

Transfer 4 ml of the sample into the digestion vessel. Add 4 ml of HNO3, and 2 ml of H2O2. Gently swirl the mixture and wait approximately15 minutes before closing the vessel.

Take caution when mixing the acids and the sample. The sample may foam slightly.

MARS 6MARS 6 iWave


HNO3H2O2

4 mL Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofUrine (Human)

Consumer Products

23

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions






MARS 6MARS 6 iWave


H3BO3 (4%)


170 15:00 15:00 800 900-1050 Off




24

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cosmetics (Liquid Foundation)

Weigh 1 g of the sample into the digestion vessel. Add 8 ml of HNO3 and 2 ml of HF. Gently swirl the mixture before closing the vessel.

This procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed, anadditional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “Boric AcidHF Neutralization”.

MARS 6MARS 6 iWave


HNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCosmetics (Liquid Foundation)

25

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cotton


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCotton

26

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Eye Shadow

Weigh 0.25 g of the sample into the digestion vessel. Add 7 mL of HNO3 and 3 mL of HF. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.


MARS 6MARS 6 iWave


HFHNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofEye Shadow

27

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Shampoo (Dandruff)

Add 1 mL of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofShampoo (Dandruff)

28

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Suppository (Capsule)

Weigh 1 Capsule (approx. 1.0 g) into the digestion vessel. Add 12 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.

Ensure that the capsule is completely covered with reagent before sealing the vessel.

MARS 6MARS 6 iWave


HNO3

1 Capsule (approx 1 g) Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSuppository (Capsule)

29

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vaseline



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofVaseline

30

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Wax (Candle)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWax (Candle)

Environmental and Regulatory

32

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions






MARS 6MARS 6 iWave


H3BO3 (4%)


170 15:00 15:00 800 900-1050 Off




33

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Fertilizer - AOAC Method 2006.03

Weigh 1 g (0.5 g for organic matrices) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


This method may not provide a total digest of all fertilizer samples. Hydrofluoric acid will be required to provide complete digestion of somesample matrixes.

MARS 6MARS 6 iWave


HNO3HCl


200 15:00 20:00 800 Off



Microwave Digestion ofFertilizer - AOAC Method 2006.03

34

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Limestone

Weigh 0.5 g of the sample into the digestion vessel. Add 7.5 ml of HNO3 and 2.5 ml of HF. Gently swirl the mixture before closing the vessel.

Allow any initial reaction to subside before sealing the vessel.


MARS 6MARS 6 iWave


HNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofLimestone

35

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


NPDES (Waste Water)

Transfer 50 ml of the sample into the digestion vessel. Add 3 ml of HNO3, and 2 ml HCl. Gently swirl the mixture before closing the vessel.


MARS 6MARS 6 iWave

Xpress (75 ml)Xpress PlusEasyPrepEasyPrep Plus

HNO3HCl

50 ml Water Ramp to Temperature One Touch

165 30:00 0:00 800 900-1050 Off



Microwave Digestion ofNPDES (Wastewater)

36

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pine Needles

Weigh 0.5 g of the sample into the digestion vessel. Add 8 mL of HNO3 and 2 mL of H2O2 (30%). Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3H2O2 (30%)


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPine Needles

37

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


RoHS (For Pb, Hg, and Cd Analysis)

Weigh 0.2 g of the sample into the digestion vessel. Add 10 ml of HNO3, and 0.02 ml of H2SO4. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3H2SO4.


200 10:00 15:00 800 900-1050 Off



Microwave Digestion ofRoHS (For Pb, Hg, and Cd Analysis)

38

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sediment (BCCS-1 CRM) (Leach)


This method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide complete digestion of some samplematrixes.


MARS 6MARS 6 iWave


HNO3


180 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSediment (BCCS-1 CRM) (Leach)

39

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sediment (Buffalo River) (Leach)

Weigh 0.5 g into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing thevessel.

This method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide complete digestion of some samplematrixes.


MARS 6MARS 6 iWave


HNO3


175 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSediment (Buffalo River) (Leach)

40

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sludge (Industrial)

Weigh 0.5 g (dry weight) of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.



MARS 6MARS 6 iWave


HNO3

0.5 g (dry weight) Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSludge (Industrial)

41

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sludge (Waste Activated)

Weigh 0.5 g dry weight (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 5 ml of HNO3, and 5 ml of H2O2. Gently swirlthe mixture and wait approximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave

MARSXpressMARSXpress PlusEasyPrepEasyPrep Plus

HNO3H2O2


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSludge (Waste Activated)

42

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Soil (Montana-CRM) (Leach)


This method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide completedigestion of some sample matrixes.


MARS 6MARS 6 iWave


HNO3


175 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSoil (Montana-CRM) (Leach)

43

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


TCLP Extract

Transfer 25 ml of the sample into the digestion vessel. Add 5 ml of HNO3. Gently swirl the mixture before closing the vessel.

If a high organic content is suspected, a 10 ml sample volume is recommended.

MARS 6MARS 6 iWave

EasyPrep PlusXpress (75 ml)Xpress Plus

HNO3

25 mL EPA Digestion (Water) Standard Control One Touch

170 10:00 10:00 800 900-1050 Off



Microwave Digestion ofTCLP Extract

44

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3015 (Aqueous Samples)


MARS 6MARS 6 iWave

EasyPrep PlusXpress (75 ml)XpressPlus

HNO3

45 ml Environmental Digestion(Water)

Standard Control One Touch

170 10:00 10:00 800 900-1050 Off

This method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the samplematrix.


Microwave Digestion ofUS EPA 3015 (Aqueous Samples)

45

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3015a (Aqueous Samples)

Transfer 45 ml of the sample into the digestion vessel. Add 5 ml of HNO3, or alternatively 4 ml of HNO3 and 1 ml HCl. Gently swirl themixture before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl (Optional)



170 10:00 10:00 800 900-1050 Off



Microwave Digestion ofUS EPA 3015a (Aqueous Samples)

46

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3051 (Solid Samples)


MARS 6MARS 6 iWave

EasyPrep PlusXpressXpressPlus

HNO3HCl (Optional)

0.5 g Environmental Digestion(Solids)


175 5:30 4:30 800 900-1050 Off

This method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the samplematrix. (See method 3052 for total digestion).


Microwave Digestion ofUS EPA 3051 (Solid Samples)

47

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3051a (Solid Samples)

Weigh 0.5 g of the sample into the digestion vessel. Add 10 ml of HNO3, or alternatively 9 ml HNO3, and 1 ml HCl. Gently swirl the mixturebefore closing the vessel.


MARS 6MARS 6 iWave

EasyPrep PlusXpressXpressPlus

HNO3HCl (Optional)



175 5:30 4:30 800 900-1050 Off

This method is intended to be an acid leach, not a total digest. Hydrofluoric acid will be required to provide complete digestion of the samplematrix. (See method 3052 for total digestion)


Microwave Digestion ofUS EPA 3051a (Solid Samples)

48

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3052

Weigh 0.5 g of the sample into the digestion vessel. Add 9 ml of HNO3, and 3 ml HF. Gently swirl the mixture before closing the vessel.

MARS 6MARS 6 iWave

EasyPrep PlusXpressXpress Plus

HNO3HF



180 5:30 9:30 800 900-1050 Off



Microwave Digestion ofUS EPA 3052

49

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


USP 232/233 (Pharmaceuticals)

Weigh 0.2 g of the sample into the digestion vessel. Add 9 ml of HNO3, and 1 ml HCl. Gently swirl the mixture before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofUSP 232/233 (Pharmaceuticals)

50

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Water (for analysis of Phosphorus)

Weigh 50 mL of H2O into the digestion vessel. Add 0.5 g of K2S2O8 and 1 mL of H2SO4. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

MARS 6 XpressXpressPlusEasyPrepEasyPrep Plus

K2S2O8H2SO4


170 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWater (for analysis of Phosphorus)

51

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Wood



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWood

Food Testing

53

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Apple


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofApple

54

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Asparagus


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAsparagus

55

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Bacon (Cooked Pieces)

Weigh 1.0 g of the sample into the digestion vessel. Add 8 mL of HNO3 and 2 mL of DI H2O. Gently swirl the mixture and wait approximately15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3DI H2O


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBacon (Cooked Pieces)

56

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Beef (ground)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBeef (Ground)

57

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Beer (Light)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBeer (Light)

58

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Blueberry


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBlueberry

59

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Broccoli


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBroccoli

60

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Caramel Color

Weigh 2.0 mL of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.

MARS 6MARS 6 iWave


HNO3

2.0 mL Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCaramel Color

61

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Carrot


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCarrot

62

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Celery


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCelery

63

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cheese Crackers



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofCheese Crackers

64

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cheese (Processed)



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofCheese (Processed)

65

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cherry


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCherry

66

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Chewing Gum




MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofChewing Gum

67

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Chicken (Boneless)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofChicken (Boneless)

68

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Chili Candy (Mexican)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofChili Candy (Mexican)

69

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Chips (potato)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofChips (Potato)

70

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Coffee Beans



MARS 6MARS 6 iWave


HNO3


200 20:00 15:00 800 900-1050 Off



Microwave Digestion ofCoffee Beans

71

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cucumber


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCucumber

72

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Dog Food (Dry)

Weigh 0.5 g of sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofDog Food (Dry)

73

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Dog Food (Wet)

Weigh 1 g of wet sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofDog Food (Wet)

74

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Flour


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFlour

75

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Food Coloring (liquid)

Add 0.5 mL of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFood Coloring (Liquid)

76

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Food

Weigh 0.5 g dry weight (0.25 g w/Xpress vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture andwait approximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFood

77

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Fruit Juice


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFruit Juice

78

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Granola Bar



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofGranola Bar

79

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Grape


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGrape

80

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Grapefruit


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGrapefruit

81

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ham


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofHam

82

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Cereal (Rice Grain)



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofInfant Cereal (Rice Grain)

83

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Liquid)

Transfer 1 ml (0.5 ml w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the requiredresults on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or belowroom temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Microwave Digestion ofInfant Formula (Liquid)

84

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Liquid) in iPrep Vessels

Transfer 2 ml of of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.

This application can only be run in the iPrep vessel.


MARS 6 iWave iPrep HNO3


210 20:00 20:00 N/A 500-1800 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results onyour sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.d) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Microwave Digestion ofInfant Formula (Liquid) in iPrep Vessels

85

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Powder)

Weigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofInfant Formula (Powder)

86

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Powder) in iPrep Vessels

Weigh 1 g of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.





210 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofInfant Formula (Powder) in iPrep Vessels

87

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Kidney Bean

Weigh 0.5 g (dry weight) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofKidney Bean

88

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Maple Syrup



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofMaple Syrup

89

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Mayonnaise



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofMayonnaise

90

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Milk (Liquid, Whole)

Transfer 4 ml of the liquid sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMilk (Liquid, Whole)

91

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Milk (Powder)



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofMilk (Powder)

92

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Nutritional Drink (adult)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofNutritional Drink (Adult)

93

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Olive Oil


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofOlive Oil

94

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Orange


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofOrange

95

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Orange Juice


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofOrange Juice

96

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Peanut Butter



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofPeanut Butter

97

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pear


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPear

98

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pepper (Bell, Chili, etc.)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPepper (Bell, Chili, etc.)

99

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pizza (Frozen, Pepperoni)

Weigh 1.0 g (homogenized) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPizza (Frozen, Pepperoni)

100

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Plum


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPlum

101

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pork Gelatin


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPork Gelatin

102

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pork (ground)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPork (Ground)

103

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Potato


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPotato

104

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pretzel (salted)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPretzel (Salted)

105

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Protein Bar

Weigh 0.5 g ground sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofProtein Bar

106

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Raspberry


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofRaspberry

107

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Rice



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofRice

108

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Safflower Oil


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSafflower Oil

109

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Salami



MARS 6MARS 6 iWave

EasyPrepEasyPrep PlusXpress (75 ml)Xpress Plus

HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSalami

110

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sausage



MARS 6MARS 6 iWave

EasyPrepEasyPrep PlusXpress (75 ml)Xpress Plus

HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSausage

111

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Soda (Diet)

Add1 mL of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSoda (Diet)

112

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Soybean



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSoybean

113

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Spinach


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSpinach

114

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Spinach Leaves




MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSpinach Leaves

115

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Strawberry


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofStrawberry

116

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sugar (granulated)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSugar (Granulated)

117

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Tea Leaves


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofTea Leaves

118

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Tomato Leaves



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off

Sample was clear, colorless, with white silica particles upon dilution to 50 mL.


Microwave Digestion ofTomato Leaves

119

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Tomato Soup


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofTomato Soup

120

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Walnut (ground)

Weigh 0.5 g (dry weight) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWalnut (Ground)

121

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Watermelon


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWatermelon

122

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Whey Powder



MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results onyour sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

Microwave Digestion ofWhey Powder

a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on your sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

123

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Wine

Transfer 1 ml of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofWine

124

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Yogurt (Plain)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofYogurt (Plain)

Geoscience and Mining

126

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Alpha - Alumina in iPrep Vessels

Weigh 0.5 g of sample into the digestion vessel. Add 10 ml HCl. Gently swirl the vessel to thoroughly mix the sample and acid.


Ensure that particles are well suspended in acid mixture prior to sealing vessel.

Stirring may be helpful to keep particles suspended in solution during digestion.

MARS 6 iWave iPrep HCl


240 30:00 60:00 N/A 1800 N/A



Microwave Digestion ofAlpha - Alumina in iPrep Vessels

127

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Aluminum Oxide

Weigh 0.25 g of sample into the digestion vessel. Add 6.5 ml H3PO4 and 3.5 ml H2SO4. Gently swirl the vessel to thoroughly mix thesample and acid.

EasyPrep Plus requires a high temperature probe for this method.



MARS 6MARS 6 iWave

Easy PrepEasy Prep Plus

H3PO4H2SO4


270 30:00 20:00 N/A 1800 N/A



Microwave Digestion ofAluminum Oxide

128

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Automotive Catalyst

Weigh 0.4 g of the sample into the digestion vessel. Add 10 ml of HCl and 0.5 ml of HF. Gently swirl the mixture before closing the vessel.


Reducing the particle size increases the efficiency of digestion and may decrease the digestion time.

MARS 6MARS 6 iWave


HClHF


210 15:00 30:00 800 900-1050 Off



Microwave Digestion ofAutomotive Catalyst

129

Step 1 of 2

www.cem.com

Procedure

Notes


Heating Program

1


Reagents

Microwave Digestion ofMARS 6TM

Method Note

Control Type Method TypeMax Sample Weight Sample Type


Bauxite

Weigh 0.25 g of the sample into the digestion vessel. Add 6.5 mL of H3PO4 and 3.5 mL of H2SO4. Gently swirl the mixture before closingthe vessel.

MARS 6MARS iWave


H3PO4H2SO4


240 15:00 15:00 800 900-1050 Off

Microwave Digestion ofBauxite (Step 1 of 2)

130

Procedure

Step 2 of 2

Notes

Heating Program

1


Reagents


MARS 6TM

Method NoteMicrowave Digestion of


Results

General Precautions

a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on yoursample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Bauxite

Proceeding step 1 add 1 mL of HNO3, 1 mL of HCl, and 1 mL of HF. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


HNO3HClHF

200 15:00 15:00 800 900-1050 Off

Sample was clear, colorless, and particle free upon dilution to 50 mL

Microwave Digestion ofBauxite (Step 2 of 2)

131

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions






MARS 6MARS 6 iWave


H3BO3 (4%)


170 15:00 15:00 800 900-1050 Off




132

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Carbon

Weigh 0.1 g of the sample into the digestion vessel. Add 10 ml of HNO3 . Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

The structure, form and surface area of carbon samples varies widely. Higher temperatures and use of other reagents may be necessary inorder to digest certain samples.

MARS 6MARS 6 iWave


HNO3


215 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCarbon

133

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Carbon Nanotubes


MARS 6MARS 6 iWave


HNO3


220 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCarbon Nanotubes

134

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cement

Weigh 0.3 g of the sample into the digestion vessel. Add 3 ml of HNO3 , 6 ml of HCL, and 3 ml of HF. Gently swirl the mixture before closingthe vessel.



MARS 6MARS 6 iWave


HNO3HClHF


175 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCement

135

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ceramic (Fused Silica)

Weigh 0.5 g of the sample into the digestion vessel. Slowly add 2 ml of HNO3 , and 8 ml of HF. Gently swirl the mixture before closing thevessel.

HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing the vessel.


MARS 6MARS 6 iWave


HNO3HF


190 10:00 20:00 800 900-1050 Off



Microwave Digestion ofCeramic (Fused Silica)

136

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ceramics

Weigh 0.2 g of the sample into the digestion vessel. Add 5 ml of HNO3, and 5 ml of HF. Gently swirl the mixture before closing the vessel.



MARS 6MARS 6 iWave


HNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCeramics

137

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Char (Sulfuric Acid)

Add 5 ml H2SO4 into the vessel that contains the sample and acid.


This method is for the pretreatment of large sample sizes or difficult organic samples that are resistant to oxidation. After the char iscomplete, the vessel is opened and a normal oxidation with HNO3 can be run, usually at around 200C.

MARS 6MARS 6 iWave


H2SO4


260 15:00 15:00 800 900-1050 Off



Microwave Digestion ofChar (Sulfuric Acid)

138

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Clay

Weigh 0.2 g of the sample into the digestion vessel. Add 3 ml of HNO3, 1 ml of HCl, and 5 ml of HF. Gently swirl the mixture before closingthe vessel.



MARS 6MARS 6 iWave


HFHNO3HCl


200 15:00 10:00 800 900-1050 Off



Microwave Digestion ofClay

139

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Coal (Anthracite)


After heating program in step1, allow vessel to cool before proceeding with step 2.

MARS 6MARS 6 iWave

EasyPrepEasy Prep Plus

HNO3


200 15:00 20:00 800 900-1050 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results onyour sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the the number and type of vessels detected.

Microwave Digestion ofCoal

140

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Coal in iPrep Vessels







250 20:00 20:00 N/A 500-1800 Off

Sample was clear, colorless with some particles remaining upon dilution to 50 ml.


Microwave Digestion ofCoal in iPrep Vessels

141

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Coal Ash

Weigh 0.3 g of the sample into the digestion vessel. Add 3 ml of HNO3, 3 ml of HCl and 3 ml of HF. Gently swirl the mixture before closingthe vessel.



MARS 6MARS 6 iWave


HNO3HClHF


15:00 15:00 800 900-1050 Off



Microwave Digestion ofCoal Ash

142

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Diesel Fuel

Weigh 0.25 g of the sample into the digestion vessel. Add 10 ml of HNO3 . Gently swirl the mixture and wait approximately 15 minutes topre-digest before closing the vessel.

The pre-digestion step will allow the lighter fuel fractions to react before sealing the vessels.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofDiesel Fuel

143

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Iron Ore

Weigh 1 g of the sample into the digestion vessel. Add 4 ml of H2O, 8 ml of HCl, 4 ml of HNO3, and 4 ml of HF. Gently swirl the mixture andwait approximately 15 minute before closing the vessel.


The addition of Conc. HCl (0-8 mL) is appropriate for the stabilization of Ag, Ba and Sb, and high concentrations of Fe and Al in solution. Theamount of HCl will vary depending on the matrix and the concentration of the analytes. The addition of HCl may, however, limit thetechniques or increase the difficulties of analysis.

MARS 6MARS 6 iWave


H2OHClHNO3HF


200 15:00 10:00 800 900-1050 Off



Microwave Digestion ofIron Ore

144

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Kerosene

Weigh 0.25 g of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes topre-digest before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofKerosene

145

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Limestone

Weigh 0.5 g of the sample into the digestion vessel. Add 7.5 ml of HNO3 and 2.5 ml of HF. Gently swirl the mixture before closing the vessel.



MARS 6MARS 6 iWave


HNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofLimestone

146

Step 1 of 2

www.cem.com

Procedure

Notes


Heating Program

1


Reagents


Method Note



Mill Tailings

Weigh 0.25 g of the sample into the digestion vessel. Add 3 ml of H3PO4, and 2 ml of H2SO4. Gently swirl the mixture before closing thevessel.

After heating program in step 1, allow vessel to cool before proceeding with step 2.

EasyPrep Plus vessels require a high temperature probe for this method.

MARS 6MARS 6 iWave


H3PO4H2SO4


270 15:00 30:00 800 900-1050 Off

Microwave Digestion ofMill Tailings (Step 1 of 2)

147

Procedure

Step 2 of 2

Notes

Heating Program

1


Reagents


MARS 6TM



Results

General Precautions

Mill Tailings

Cool, vent and open vessel after step 1. Add 2.5 ml HNO3, 2.5 ml HCl, 2.5 ml HF, and 2.5 ml H2O.

HF should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing the vessel.

The above procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluoridesformed, an additional complexation step with boric acid should be used. This procedure can be found in method note entitled “Boric HFNeutralization”


HNO3HClHFH2O

200 15:00 20:00 800 900-1050 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on yoursample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Microwave Digestion ofMill Tailings (Step 2 of 2)

148

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Motor Oil (Waste)

Weigh 0.25 g (0.1 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes to pre-digest before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMotor Oil (Waste)

149

Step 1 of 2

www.cem.com

Procedure

Notes


Heating Program

1


Reagents


Method Note



Petroleum Coke

Weigh 0.1 g of the sample into the digestion vessel. Add 10 mL of H2SO4. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

Mars iWaveMars 6


H2SO4

0.1 g Inorganic Ramp to Temperature One Touch

260 15:00 15:00 800 900-1050 Off

Microwave Digestion ofPetroleum Coke (Step 1 of 2)

150

Procedure

Step 2 of 2

Notes

Heating Program

1


Reagents


MARS 6TM



Results

General Precautions


Petroleum Coke

Proceeding step 1 add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

HNO3

200 15:00 15:00 800 900-1050 Off


Microwave Digestion ofPetroleum Coke (Step 2 of 2)

151

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Rock (pulverized)

Weigh 0.5 g of the sample into the digestion vessel. Add 5 mL of HNO3, 3 mL of HCl, and 3 mL of HF. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HClHFHNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofRock (Pulverized)

152

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Rutile Ore

Weigh 0.25 g of the sample into the digestion vessel. Add 4 ml of HNO3, 3 ml of H3PO4, and 8 ml of HF. Gently swirl the mixture beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3HFH3PO4


240 15:00 20:00 800 900-1050 Off



Microwave Digestion ofRutile Ore

153

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sand

Weigh 0.5 g of the sample into the digestion vessel. Add 3 ml of HNO3, 2 ml of HCl, and 5 ml of HF. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.



MARS 6MARS 6 iWave


HNO3HFHCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSand

154

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Silica Sand

Weigh 0.5 g of the sample into the digestion vessel. Add 5 ml of H2O, 3 ml of HNO3, and 8 ml of HF. Gently swirl the mixture before closingthe vessel.

Add HF slowly, and allow vessels to stand in the fume hood until the initial reaction subsides.


Reducing the particle size increase the efficiency of digestion and may decrease the digestion time.

MARS 6MARS 6 iWave


H2OHNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSilica Sand

155

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Silicon Dioxide





MARS 6MARS 6 iWave


HNO3HF


180 10:00 15:00 800 900-1050 Off



Microwave Digestion ofSilicon Dioxide

156

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Silicon Wafer

Weigh 0.5 g of the sample into the digestion vessel. Slowly add 3 ml of HNO3, and 6 ml of HF. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.



MARS 6MARS 6 iWave


HNO3HF


180 10:00 15:00 800 900-1050 Off



Microwave Digestion ofSilicon Wafer

157

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Slag (Furnace)




MARS 6MARS 6 iWave


HNO3HClHF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSlag (Furnace)

158

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Titanium Dioxide



MARS 6MARS 6 iWave


HNO3HF


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofTitanium Dioxide

159

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Tungsten Carbide

Weigh 0.25 g of the sample into the digestion vessel. Slowly add 5 ml of HNO3, and 10 ml of HF. Gently swirl the mixture before closing thevessel.




MARS 6MARS 6 iWave


HNO3HF


220 20:00 20:00 800 900-1050 Off



Microwave Digestion ofTungsten Carbide

160

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Tungsten Oxide

Weigh 0.5 g of the sample into the digestion vessel. Slowly add 2 ml of HNO3, and 7 ml of HF. Gently swirl the mixture before closing thevessel.




MARS 6MARS 6 iWave


HNO3HF


220 20:00 20:00 800 900-1050 Off



Microwave Digestion ofTungsten Oxide

161

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Zeolite




MARS 6MARS 6 iWave


HNO3HF


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofZeolite

Industrial Hygiene

163

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Filter Paper (Cellulose)

Weigh 1 filter (approximately 0.9 g) of the sample into the digestion vessel. Add 5 ml of H2O, and 5 ml of HNO3. Gently swirl the mixture andwait approximately 15 minutes before closing the vessel.

Add H2O before HNO3.


MARS 6MARS 6 iWave


H2OHNO3

1 filter (approximately 0.9 g) Organic Ramp to Temperature One Touch

180 15:00 10:00 800 900-1050 Off



Microwave Digestion ofFilter Paper (Cellulose)

164

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Filter (37 mm Mixed Cellulose Ester)

Weigh 1 filter (approximately 0.3 g) into the digestion vessel. Add 10 ml HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.


MARS 6MARS 6 iWave

XpressXpressPlusEasyPrepEasyPrep pLus

HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFilter (37 mm Mixed Cellulose Ester)

165

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Filter (47 mm Polycarbonate)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFilter (47 mm Polycarbonate)

166

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ghost Wipe

Weigh 1 wipe (approx 2.5 g) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.

Ensure that the entire wipe is covered with reagent.

MARS 6MARS 6 iWave


HNO3

1 wipe (approx 2.5 g) Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGhost Wipe

167

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Toray Filter in iPrep Vessels

Weigh 1 filter (approximately 0.3-0.5 g) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture before closingthe vessel.



1 filter(approximately 0.3-0.5 g)

Organic Ramp to Temperature One Touch

260 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofToray Filter in iPrep Vessels

Materials Science

169

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Circuit Board (cryo-ground)

Weigh 0.5 g of the sample into the digestion vessel. Add 3 mL of HNO3 and 9 mL of HCl. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

HCl should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

This method is considered a leach and may not provide a total digestion.

MARS 6MARS 6 iWave


HClHNO3


200 15:00 15:00 800 900-1050 Off

Sample was clear, with particles upon dilution to 50 mL.


Microwave Digestion ofCircuit Board (Cryo-ground)

170

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Glass (ground)

Weigh 0.1 g of the sample into the digestion vessel. Add 2 mL of HNO3, 4 mL of HCl, and 3 mL of HF. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HClHFHNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGlass (Ground)

171

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Graphite Fiber (Epoxy Resin, Fiber Content)

Weigh 1 g of the sample into the digestion vessel. Add 30 ml of HNO3. Gently swirl the mixture before closing the vessel.

Sample must be completely covered with acid prior to digestion.

After digestion the samples are filtered and the graphite fibers are rinsed with deionized water.

This method is for the gravimetric (weight) determination of fiber content.

MARS 6MARS 6 iWave


HNO3


150 10:00 10:00 800 900-1050 Off

Sample was digested, but the fiber filler material is left undigested for subsequent gravimetric analysis.


Microwave Digestion ofGraphite Fiber (Epoxy Resin, Fiber Content)

Metals and Alloys

173

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Aluminum Alloy

Weigh 0.25 g of the sample into the digestion vessel. Add 5 ml of H2O and 5 ml of HCl .Gently swirl the mixture before closing the vessel.

Add H2O before HCl.

Add HCl slowly, and allow vessels to stand in the fume hood until initial reaction subsides.

MARS 6MARS 6 iWave


HClH2O

0.25g Organic Ramp to Temperature One Touch

190 10:00 15:00 800 900-1050 Off



Microwave Digestion ofAlluminum Alloy

174

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Alpha - Alumina in iPrep Vessels

Weigh 0.5 g of sample into the digestion vessel. Add 10 ml HCl. Gently swirl the vessel to thoroughly mix the sample and acid.




MARS 6 iWave iPrep HCl


240 30:00 60:00 N/A 1800 N/A



Microwave Digestion ofAlpha - Alumina in iPrep Vessels

175

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Aluminum Oxide

Weigh 0.25 g of sample into the digestion vessel. Add 6.5 ml H3PO4 and 3.5 ml H2SO4. Gently swirl the vessel to thoroughly mix thesample and acid.




MARS 6MARS 6 iWave

Easy PrepEasy Prep Plus

H3PO4H2SO4


270 30:00 20:00 N/A 1800 N/A



Microwave Digestion ofAluminum Oxide

176

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Aluminum (metal)

Weigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HCl and 3 mL of DI H2O. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

HCl should be added slowly and carefully to the sample. Allow any initial reaction to subside before sealing vessel.

MARS 6MARS 6 iWave


HClDI H2O


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAluminum (Metal)

177

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Copper (metal)


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on yoursample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below room temperature toavoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as One Touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Microwave Digestion ofCopper (Metal)

178

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Copper (Ore)

Weigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add10 ml of Aqua Regia (3:1 HCl:HNO3 ,). Gently swirl themixture before closing the vessel.



MARS 6MARS 6 iWave


HNO3HCl


180 15:00 10:00 800 900-1050 Off

Sample was clear, and colorless with some remaining particles upon dilution to 50 ml.


Microwave Digestion ofCopper (Ore)

179

Step 1 of 2

www.cem.com

Procedure

Notes


Heating Program

1


Reagents


Method Note



Metal Alloy (CoCr)

Weigh 0.5 g of the sample into the digestion vessel. Add 5 ml of HNO3, 5 ml of HF, and 5 of ml H2O. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


The addition of Deionized Water may improve solubility of metal alloys.


MARS 6MARS 6 iWave

EasyPrepEasyPrepPlus

HNO3HFH2O


200 15:00 15:00 800 900-1050 Off

Microwave Digestion ofMetal Alloy (CoCr) (Step 1 of 2)

180

Procedure

Step 2 of 2

Notes

Heating Program

1


Reagents


MARS 6TM



Results

General Precautions

Metal Alloy (CoCr)

Cool, vent and open vessel after step 1. Add 4 ml of H2O2, (30%)

H2O2

200 10:00 10:00 800 900-1050 Off



Microwave Digestion ofMetal Alloy (CoCr) (Step 2 of 2)

181

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Metal Alloy (FeCr)

Weigh 0.25 g of the sample into the digestion vessel. Add 5 ml of HCl, 5 ml of HNO3, and 5 ml of HF. Gently swirl the mixture before closingthe vessel.


MARS 6MARS 6 iWave


HClHFHNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMetal Alloy (FeCr)

182

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Metal Alloy (NiCr)

Weigh 0.5 g of the sample into the digestion vessel. Add 5 ml of H2O, 5 ml of HNO3, and 5 ml of HF. Gently swirl the mixture before closingthe vessel.


MARS 6MARS 6 iWave


H2OHNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMetal Alloy (NiCr)

183

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Nickel (metal)

Weigh 0.5 g of sample into the digestion vessel. Add 5 mL of HNO3 and 5 mL of DI H2O. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3DI H2O


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofNickel (Metal)

184

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Platinum (Metal)

Weigh 0.5 g of the sample into the digestion vessel. Add 10 ml of Aqua Regia (3:1 HCl:HNO3). Gently swirl the mixture before closing thevessel.

MARS 6MARS 6 iWave


HNO3HCl


180 15:00 20:00 800 900-1050 Off



Microwave Digestion ofPlatinum (Metal)

185

Step 1 of 2

www.cem.com

Procedure

Notes


Heating Program

1


Reagents


Method Note



Precious Metal (Ore)

Weigh 0.1 g of the sample into the digestion vessel. Add 10 ml of HNO3, and 0.5 ml of HF. Gently swirl the mixture before closing the vessel.



MARS 6MARS 6 iWave


HNO3HF


200 15:00 20:00 800 900-1050 Off

Microwave Digestion ofPrecious Metal (Ore) (Step 1 of 2)

186

Procedure

Step 2 of 2

Notes

Heating Program

1


Reagents


MARS 6TM



Results

General Precautions

a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results on yoursample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or belowroom temperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.e) If programming as one touch, the ramp time and power will be automatically determined based on the number and type of vessels detected.

Precious Metal (Ore)

Cool, vent and open vessel after step 1. Add 5 ml of HCl.


HCl

180 10:00 10:00 800 900-1050 Off


Microwave Digestion ofPrecious Metal (Ore) (Step 2 of 2)

187

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Selenium Alloy

Weigh 1 g (0.5 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture before closing thevessel.

MARS 6MARS 6 iWave


HNO3




Microwave Digestion ofSelenium Alloy

188

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


SnAg Solder

Weigh 0.5 g of the sample into the digestion vessel. Slowly add dropwise 10 ml of 1:1:1 H2O:HNO3:HF (premixed) to the sample. Gentlyswirl the mixture and wait approximately 15 minutes before closing the vessel.

Caution must be taken when adding the acid solution to the sample as the reaction is very vigorous and exothermic.


MARS 6MARS 6 iWave


H2OHNO3HF


180 15:00 10:00 800 900-1050 Off



Microwave Digestion ofSnAg Solder

189

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Stainless Steel

Weigh 0.5 g of the sample into the digestion vessel. Add 9 ml of HCl, 3 ml of HNO3, and 3 ml of HF. Gently swirl the mixture before closingthe vessel.


MARS 6MARS 6 iWave


HNO3HFHCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofStainless Steel

190

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Steel (Stainless)


This method may not provide a total digest of all samples. Hydrofluoric acid will be required to provide completedigestion of some sample matrixes.

MARS 6MARS 6 iWave


HClHNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSteel (Stainless)

191

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Titanium Alloy



MARS 6MARS 6 iWave


HNO3HFHCl


200 15:00 30:00 800 900-1050 Off



Microwave Digestion ofTitanium Alloy

192

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Titanium Dioxide



MARS 6MARS 6 iWave


HNO3HF


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofTitanium Dioxide

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Zinc Oxide


MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofZinc Oxide

Nutraceuticals

195

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Biotin

Weigh 0.5 g of the sample into the digestion vessel. Add 9 ml of HNO3, and 1 ml of HCl. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofBiotin

196

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ginko (Ground)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGinko (Ground)

197

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ginko (Whole Pill)

Weigh 1 pill (approx 1.0 g) into the digestion vessel. Add 10 mL of HNO3 and 2 mL of H2O2. Gently swirl the mixture and wait approximately15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3H2O2

1 pill (Approx 1.0 g) Organic Ramp to Temperature One Touch

210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGinko (Whole Pill)

198

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Liquid)

Transfer 1 ml (0.5 ml w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofInfant Formula (Liquid)

199

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Liquid) in iPrep Vessels

Transfer 2 ml of of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.





210 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofInfant Formula (Liquid) in iPrep Vessels

200

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Powder)

Weigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofInfant Formula (Powder)

201

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Infant Formula (Powder) in iPrep Vessels

Weigh 1 g of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.





210 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofInfant Formula (Powder) in iPrep Vessels

202

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Kelp



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofKelp

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Milk (Liquid, Whole)

Transfer 4 ml of the liquid sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMilk (Liquid, Whole)

204

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Milk (Powder)



MARS 6MARS 6 iWave


HNO3


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofMilk (Powder)

205

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Plant Tissue




MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPlant Tissue

206

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions





MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off




207

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Wheat



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWheat

208

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Whey Powder



MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off


a) This procedure is a reference point for sample digestion using a CEM system and may need to be modified or changed to obtain the required results onyour sample.b) If using a vessel other than the recommended choice, adjust sample size and pressure limit to values appropriate for the vessel chosen.c) The control / reference vessel must contain the largest and most reactive sample.d) Manual venting of CEM vessels should be performed when wearing hand/eye/body protection and when the vessel contents are at or below roomtemperature to avoid the potential for chemical burns. Always point the vent hole away from the operator.

Microwave Digestion ofWhey Powder

Organic Chemicals

210

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Photoresist

Add 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPhotoresist

Paints and Coatings

212

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Paint (Latex Based Liquid)

Weigh 1 g (0.5 g w/Xpress Vessels) of sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture before closing thevessel.

HF is required for a total dissolution of inorganic filler if present.

If this procedure uses hydrofluoric acid. If it is necessary to complex the residual hydrofluoric acid or redissolve insoluble fluorides formed,an additional complexation step with boric acid should be used. This procedure can be found in the One Touch Method note entitled “BoricAcid HF Neutralization”.

MARS 6MARS 6 iWave


HNO3


200 15:00 10:00 800 900-1050 Off



Microwave Digestion ofPaint (Latex Based Liquid)

213

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Paint Chips (For Pb Analysis)


HF may be required for a total dissolution.

MARS 6MARS 6 iWave


HNO3


200 15:00 10:00 800 900-1050 Off

Sample was clear, colorless, with some remaining inorganic particles upon dilution to 50 ml.


Microwave Digestion ofPaint Chips (For Pb Analysis)

214

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Photoresist

Add 0.5 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPhotoresist

215

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Toner (Ink) in iPrep Vessels






240 20:00 20:00 N/A 500-1800 Off

Sample was clear, colorless with some particles remaining upon dilution to 50 ml.


Microwave Digestion ofToner (Ink) in iPrep Vessels

Personal Care (Health and Beauty)

217

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions






MARS 6MARS 6 iWave


H3BO3 (4%)


170 15:00 15:00 800 900-1050 Off




218

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cosmetics (Liquid Foundation)

Weigh 1 g of the sample into the digestion vessel. Add 8 ml of HNO3 and 2 ml of HF. Gently swirl the mixture before closing the vessel.


MARS 6MARS 6 iWave


HNO3HF


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCosmetics (Liquid, Foundation)

219

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Eye Shadow

Weigh 0.25 g of the sample into the digestion vessel. Add 7 mL of HNO3 and 3 mL of HF. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.


MARS 6MARS 6 iWave


HFHNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofEye Shadow

220

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Shampoo (Dandruff)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofShampoo (Dandruff)

Pharmaceutical and Biotech

222

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Allergy Pill (Ground)



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAllergy Pill (Ground)

223

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Allergy Pill (Whole Pill)

Weigh 1 pill (Approx 1.0 g) into the digestion vessel. Add 10 mL of HNO3 and 2 mL of H2O2 (30%). Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3H2 O2 (30%)


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAllergy Pill (Whole Pill)

224

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Antioxidant (Ground)



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAntioxidant (Ground)

225

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Antioxidant (Whole Pill)

Weigh 1 pill (approx 1.4 g) into the digestion vessel. Add 10 mL of HNO3 and 2 mL of H2O2 (30%). Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3H2O2 (30%)


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAntioxidant (Whole Pill)

226

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


APIs with Aromatic Ring Structures in iPrep Vessels

Weigh 0.1 g - 0.5 g of the sample into the digestion vessel. Add 9 ml of HNO3 and 1 ml of HCl. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.



MARS 6 iWave iPrep HNO3HCl

0.1 g - 0.5 g Organic Ramp to Temperature One Touch

250 30:00 25:00 N/A 1800 N/A

Sample was clear, colorless, and particle free upon dilution to 50 ml. If the sample contains precious metals the diluted sample may be thecolor associated with the metals.


Microwave Digestion ofAPIs with Aromatic Ring Structures in iPrep Vessels

227

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ascorbic Acid



MARS 6MARS 6 iWave

EasyPrepEasyPrep PlusXpress PlusXpress

HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofAscorbic Acid

228

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Aspirin (Ground)

Weigh 0.25 g of the sample into the digestion vessel. Add 9 mL of HNO3 and 1 mL of HCl. Gently swirl the mixture and wait approximately15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAspirin (Ground)

229

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Aspirin (Whole)

Weigh 1 pill (Approx 1.0 g) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAspirin (Whole)

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Beta Carotene



MARS 6 iWaveMARS 6


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofBeta Carotene

231

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Biotin



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofBiotin

232

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Calcium Carbonate

Weigh 0.5 g of the sample into the digestion vessel. Slowly add 9 ml of HNO3, and 1 ml of HCl. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.


Allow initial reaction to subside before sealing vessel.

MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofCalcium Carbonate

233

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Calpan Pantothenic Acid



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCalpan Pantothenic Acid

234

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cephalexin



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCephalexin

235

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Chromium Chelate



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofChromium Chelate

236

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cold and Flu Medicine (Liquid)

Add 0.75 mL of the sample into the digestion vessel. Add 9 mL of HNO3 and 1 mL of HCl. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCold and Flu Medicine (Liquid)

237

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Cupric Sulfate



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off

Sample was clear, blue in color, and particle free upon dilution to 50 ml.


Microwave Digestion ofCupric Sulfate

238

Procedure

Notes



Heating Program

1



Reagents


www.cem.com Form preparedby:

MARS 6TM

Method Note

Results

General Precautions


Diclofenac K



MARS 6MARS 6 iWave


HNO3H2O2 (30%)


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofDiclofenac K

239

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Empty Capsule (gel)

Weigh 1 capsule (Approx 0.1 g) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.


MARS 6MARS 6 iWave


HNO3

1 capsule (Approx 0.1 g) Organic Ramp to Temperature One Touch

200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofEmpty Capsule (Gel)

240

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Fish Oil (No Capsule)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFish Oil (No Capsule)

241

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Folic Acid



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFolic Acid

242

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ginko (Ground)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGinko (Ground)

243

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Ginko (Whole Pill)

Weigh 1 pill (approx 1.0 g) into the digestion vessel. Add 10 mL of HNO3 and 2 mL of H2O2. Gently swirl the mixture and wait approximately15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3H2O2


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGinko (Whole Pill)

244

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Kelp



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofKelp

245

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Losataran K



MARS 6MARS 6 iWave


HNO3H2O2 (30%)


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofLosataran K

246

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Magnesium Carbonate


Allow any reaction to subside before sealing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofMagnesium Carbonate

247

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Magnesium Oxide



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMagnesium Oxide

248

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Manganese Carbonate



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofManganese Carbonate

249

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Metaformin (ground)



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMetaformin (Ground)

250

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Multivitamin (Ground)

Weigh 0.5 g of the sample into the digestion vessel. Add 9 mL of HNO3 and 1 mL HCl. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMultivitamin (Ground)

251

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Multivitamin (Whole)

Weigh 1 pill (Approx 2.5 g) into the digestion vessel. Add 10 mL of HNO3 and 2 mL of HCl. Gently swirl the mixture and wait approximately15 minutes before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMultivitamin (Whole)

252

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Niacinamide



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofNiacinamide

253

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pantothenic Acid



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofPantothenic Acid

254

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Potassium Chelate



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofPotassium Chelate

255

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Pyridoxine



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofPyridoxine

256

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Riboflavin



MARS 6MARS 6 iWave


HNO3HCl


230 20:00 30:00 800 900-1050 Off



Microwave Digestion ofRiboflavin

257

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Selenium Chelate



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofSelenium Chelate

258

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Stearic Acid



MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofStearic Acid

259

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Thiamine



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofThiamine

260

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions





MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off




261

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamin B-12



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofVitamin B-12

262

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamin C (ground)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofVitamin C (Ground)

263

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamin C (whole)

Weigh 1 pill (Approx 1.4 g) into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofVitamin C (Whole)

264

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamin D



MARS 6MARS 6 iWave


HNO3HCl


210 20:00 15:00 800 900-1050 Off



Microwave Digestion ofVitamin D

265

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamin D3



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofVitamin D3

266

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamin E



MARS 6MARS 6 iWave


HNO3HCl


230 20:00 30:00 800 900-1050 Off



Microwave Digestion ofVitamin E

267

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Vitamins

Weigh 0.5 g (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 9 ml of HNO3, 1 ml HCl, and 1 ml of HF. Gently swirl themixture and wait approximately 15 minutes before closing the vessel.



MARS 6MARS 6 iWave


HNO3HFHCl


210 15:00 30:00 800 900-1050 Off



Microwave Digestion ofVitamins

268

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Zinc Sulfate



MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofZinc Sulfate

Plastics, Polymers, and Oils

270

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Acrylamide


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofAcrylamide

271

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Bunker Oil


MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofBunker Oil

272

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Bunker Oil in iPrep Vessels






250 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofBunker Oil in iPrep Vessels

273

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Char (Sulfuric Acid)

Add 5 ml H2SO4 into the vessel that contains the sample and acid.


This method is for the pretreatment of large sample sizes or difficult organic samples that are resistant to oxidation. After the char iscomplete, the vessel is opened and a normal oxidation with HNO3 can be run, usually at around 200C.

MARS 6MARS 6 iWave


H2SO4


260 15:00 15:00 800 900-1050 Off



Microwave Digestion ofChar (Sulfuric Acid)

274

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Crude Oil


MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofCrude Oil

275

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Diesel Fuel

Weigh 0.25 g of the sample into the digestion vessel. Add 10 ml of HNO3 . Gently swirl the mixture and wait approximately 15 minutes topre-digest before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofDiesel Fuel

276

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Epoxy Hardener


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofEpoxy Hardener

277

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Fatty Alcohol


MARS 6MARS 6 iWave


HNO3HCl


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFatty Alcohol

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Gasoline

Add 0.1g of the sample into the digestion vessel. Slowly add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutesbefore closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofGasoline

279

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


HDPE (High Density Polyethylene)

Weigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture before closing the vessel.

MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofHDPE (High Density Polyethylene)

280

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Kerosene



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofKerosene

281

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Kevlar in iPrep Vessels



Ensure that all fibers are completely covered with acid and not adhered to the vessel liner wall.



250 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofKevlar in iPrep Vessels

282

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Lube Oil


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofLube Oil

283

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Mineral Oil


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMineral Oil

284

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Motor Oil (Waste)

Weigh 0.25 g (0.1 g w/Xpress Vessels) of the sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture and waitapproximately 15 minutes to pre-digest before closing the vessel.


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofMotor Oil (Waste)

285

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Motor Oil (Waste) in iPrep Vessels






240 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofMotor Oil (Waste) in iPrep Vessels

286

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Nylon

Weigh 0.25 g of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture before closing the vessel.

MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofNylon

287

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


PET

Weigh 0.2 g of the sample into the digestion vessel. Add 8 mL of HNO3 and 2 mL of H2SO4. Gently swirl the mixture before closing thevessel.

MARS 6MARS 6 iWave


HNO3H2SO4


230 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPET (Polyethylene Terephthalate)

288

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


PET (Polyethylene Terephthalate) in iPrep Vessels





250 20:00 20:00 N/A 500-1800 Off



Microwave Digestion ofPET (Polyethylene Terephthalate) in iPrep Vessels

289

Step 1 of 2

www.cem.com

Procedure

Notes


Heating Program

1


Reagents


Method Note



Polycarbonate Resin

Char Step

Weigh 1.0 g of the sample into the digestion vessel. Add 6 mL of H2SO4. Gently swirl the mixture and wait approximately 15 minutes beforeclosing the vessel.

MARS 6MARS iWave


H2SO4


260 15:00 15:00 800 900-1050 Off

Microwave Digestion ofPolycarbonate Resin (Step 1 of 2)

290

Procedure

Step 2 of 2

Notes

Heating Program

1


Reagents


MARS 6TM



Results

General Precautions


Polycarbonate Resin

Proceeding step one, add 10 mL of HNO3. Gently swirl the mixture and wait approximately 15 minutes before closing the vessel.

HNO3

210 15:00 15:00 800 900-1050 Off


Microwave Digestion ofPolycarbonate Resin (Step 2 of 2)

291

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Polyethersulfone (Filter Paper)

Weigh 1 filter paper (Approx 0.1 g) into the digestion vessel. Add 8 mL of HNO3 and 2 mL H2SO4. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3H2SO4

1 Filter (Approx 0.1 g) Organic Ramp to Temperature One Touch

230 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPolyethersulfone (Filter Paper)

292

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Polypropylene

Weigh 0.25 (0.1 g w/Xpress vessels) of the sample into the digestion vessel. Add 10 mL of HNO3. Gently swirl the mixture and waitapproximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3

0.25 g (0.1 g w/Xpress) Organic Ramp to Temperature One Touch

210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPolypropylene

293

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Polyurethane


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPolyurethane

294

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


PVC (Polyvinyl Chloride, Resin)

Weigh 0.25 g (0.1 g w/Xpress Vessels) of sample into the digestion vessel. Add 10 ml of HNO3. Gently swirl the mixture before closing thevessel.

MARS 6MARS 6 iWave


HNO3


210 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPVC (Polyvinyl Chloride, Resin)

295

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Rubber


MARS 6MARS 6 iWave


HNO3


220 15:00 15:00 800 900-1050 Off



Microwave Digestion ofRubber

296

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Terephthalic Acid


MARS 6MARS 6 iWave


HNO3


230 15:00 15:00 800 900-1050 Off



Microwave Digestion ofTerephthalic Acid

Pulp and Paper

298

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Filter Paper (Cellulose)

Weigh 1 filter (approximately 0.9 g) of the sample into the digestion vessel. Add 5 ml of H2O, and 5 ml of HNO3. Gently swirl the mixture andwait approximately 15 minutes before closing the vessel.

Add H2O before HNO3.


MARS 6MARS 6 iWave


H2OHNO3


180 15:00 10:00 800 900-1050 Off



Microwave Digestion ofFilter Paper (Cellulose)

299

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Filter (37 mm Mixed Cellulose Ester)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFilter (37 mm Mixed Cellulose Ester)

300

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Filter (47 mm Polycarbonate)



MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofFilter (47 mm Polycarbonate)

301

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Paper Pulp


MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofPaper Pulp

Water and Wastewater Treatment

303

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


NPDES (Waste Water)

Transfer 50 ml of the sample into the digestion vessel. Add 3 ml of HNO3, and 2 ml HCl. Gently swirl the mixture before closing the vessel.


MARS 6MARS 6 iWave

Xpress (75 ml)Xpress PlusEasyPrepEasyPrep Plus

HNO3HCl

50 ml Water Ramp to Temperature One Touch

165 30:00 0:00 800 900-1050 Off



Microwave Digestion ofNPDES (Wastewater)

304

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sludge (Industrial)




MARS 6MARS 6 iWave


HNO3


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSludge (Industrial)

305

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Sludge (Waste Activated)

Weigh 0.5 g dry weight (0.25 g w/Xpress Vessels) of the sample into the digestion vessel. Add 5 ml of HNO3, and 5 ml of H2O2. Gently swirlthe mixture and wait approximately 15 minutes before closing the vessel.

MARS 6MARS 6 iWave


HNO3H2O2


200 15:00 15:00 800 900-1050 Off



Microwave Digestion ofSludge (Waste Activated)

306

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


TCLP Extract


If a high organic content is suspected, a 10 ml sample volume is recommended.

MARS 6MARS 6 iWave

EasyPrep PlusXpress (75 ml)Xpress Plus

HNO3

25 mL EPA Digestion (Water) Standard Control One Touch

170 10:00 10:00 800 900-1050 Off



Microwave Digestion ofTCLP Extract

307

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3015 (Aqueous Samples)


MARS 6MARS 6 iWave


HNO3



170 10:00 10:00 800 900-1050 Off



Microwave Digestion ofUS EPA 3015 (Aqueous Samples)

308

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


US EPA 3015a (Aqueous Samples)

Transfer 45 ml of the sample into the digestion vessel. Add 5 ml of HNO3, or alternatively 4 ml of HNO3 and 1 ml HCl. Gently swirl themixture before closing the vessel.


MARS 6MARS 6 iWave


HNO3HCl (Optional)



170 10:00 10:00 800 900-1050 Off



Microwave Digestion ofUS EPA 3015a (Aqueous Samples)

309

Procedure

Notes



Heating Program

1



Reagents



MARS 6TM

Method Note

Results

General Precautions


Water (for analysis of Phosphorus)

Weigh 50 mL of H2O into the digestion vessel. Add 0.5 g of K2S2O8 and 1 mL of H2SO4. Gently swirl the mixture and wait approximately 15minutes before closing the vessel.

MARS 6 XpressXpressPlusEasyPrepEasyPrep Plus

K2S2O8H2SO4


170 15:00 15:00 800 900-1050 Off



Microwave Digestion ofWater (for Analysis of Phosphorus)

Microwave Acid Digestion Method Note...

Documents

Transcript of Microwave Acid Digestion Method Note...