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VVC 000008972
NIOSH Manual of Analytical Methods
Second Edition
U. S. DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE Public Health Service Center for Disease Control National Institute for Occupational Safety anb Health
VVC 000008973
CONTENTS OF VOLUME 1
Foreword ............................................................................................................... *`i Preface ................................................................................................................... v Abstract ........................--.................................................................................. v Acknowledgments .................................................................................................. xm
PART I NIOSH Monitoring Methods
P&CAM No. Lead in Blood and Urine ................................................................................... 102 Colorimetric Method for Free Silica .................................................................. 106 Antimony in Urine .............................................................................................. 107 Nitrogen Dioxide in Air ..................................................................................... 108 Free Silica (Quartz, Cristobalite, Tridymite) in Atmospheric Dust ................ 109 Quartz in Coal Dust by Infrared Spectroscopy ................................................ 110
Carbon Monoxide in Air ..................................................................................... 112
Carbon Monoxide in Blood ................................................................................. 113
Fluoride in Urine ................................................................................................ 114
Chloride in Air .................................................................................................... 115
Cyanide in Air .................................................................................................... 116
Fluoride and Hydrogen Fluoride in Air ............................................................ 117
Acrolein in Air .................................................................................................... 118
Beryllium in Air ................................................................................................- 121
Selenium in Urine .....................
124
Formaldehyde in Air ............................................................................................ 125
Hydrogen Sulfide in Air ..................................................................................... 126
Organic Solvents in Air ..................................................................................... 127
Arsenic in Urine and Air ................................................................................... 139
Arsenic in Urine and Air..................................................................................... 140
2,4-Toluenediisocyanate (TDI) in Air .............................................................. 141
p.p-Diphenylmethanediisocyanate (MDI) in Air ................................................ 142
Mercury in Urine .................................................................................................. 145
Sulfur Dioxide in Air............................................................................................ 146
Total Particulate Chromium in Air.................................................................... 152
Ozone in Air ........................................................................................................ 153
Ozone in Air ........................................................................................................ 154
Parathion in Air .................................................................................................... 158
Oil Mist in Air...................................................................................................... 159
Sulfur Dioxide in Air .......................................................................................... 160
Sulfur Dioxide in Air .......................................................................................... 163
Mercury in Urine ..............................................
165
Mercury in Blood .................................................................................................. 167
Aromatic Amines in Air ..................................................................................... 168
Chromic Acid Mist in Air ................................................................................. 169
General Procedure for Metals ......................
173
Mercury in Air .................................................................................................... 175
Tin in Atmospheric Particulate Matter and Biologic Materials ...................... 176
Gallium in Air ......................
177
Vinyl Chloride in Air............................................................................................ 178
Carbon Disulfide in Air....................................................................................... 179
Arsenic in Air .................................................................................................... 180
ix VVC 000008974
Selenium in Air .................................................................................................... 181
Chromium in Air .................................................................................................. 182
Polynuclear Aromatic Compounds in Air .......................................................... 183
Polynuclear Aromatic Hydrocarbons in Air ...................................................... 184
Benzo(a)pyrene in Air.......................................................................................... 186
Sulfuric Acid Mist in Air ................................................................................... 187
Arsenic in Air ...................................................................................................... 188
Antimony in Air .................................................................................................. 189
Indium in Air ........................................................................................................ 190
Lead and Cadmium in Air ................................................................................. 191
Arsenic in Blood .................................................................................................. 192
Antimony in Blood .............................................................................................. 193
Indium in Blood .................................................................................................. 194
Lead in Blood .................................................................................................... 195
Arsenic in Urine .................................................................................................. 196
Antimony in Urine .............................................................................................. 197
Gallium in Urine .................................................................................................. 198
Indium in Urine .................................................................................................... 199
Lead in Urine ...................................................................................................... 200
Methyl Chloride in Air.......................................................................................... 201
Acrylonitrile in Air .............................................................................................. 202
Nitroglycerin and Ethylene Glycol Dinitrate (Nitroglycol) in Air .................... 203
Sulfur Dioxide in Air ........................................................................................... 204
Ammonia in Air.................................................................................................... 205
Total Particulate Aromatic Hydrocarbons (TPAH) in Air .............................. 206
Lead in Blood and Urine ................................................................................... 208
Free Chlorine in Air .......
209
Acrolein in Air...................................................................................................... 211
Gaseous and Particulate Fluorides in Air............................................................ 212
Bis(chloromethyl) Ether in Air ........................................................................... 213
Lead , in Air or Blood ......................................................................................... 214
Inorganic Phosphate in Urine............................................................................... 215
Phosphoric Acid in Air .............................................................................
216
Benzene-Soluble Compounds in Air .................................................................. 217
Phosgene in Air ...........................................................................................
219
Chloromethyl Methyl Ether and Bis(chloromethyl) Ether in Air .................. 220
Aliphatic Amines in Air ..........
221
Zinc Oxide in Air .......................................
222
Cadmium in Blood .............................................................................................. 223
Cadmium in Urine ................................................................................................ 224
Kepone in Air........................................................................................................ 225
-2,6-Di-t-Butyl-p-Cresol (DBPC) in Air ................
226
Polymethylsiloxane Mist in Air ......................................................................... 227
Thiram in Air ...................................................................................................... 228
Pentachlorophenol in Urine ............................................................................... 230
Nitrogen Dioxide and Nitric Oxide in Air ........................................................ 231
Formic Acid in Air ............................................................................................ 232
Diazonium Salts and Azo Dyes in Air ....................... .................................... 234
Formaldehyde in Air ....................
235
4,4'-Methylenebi$(2-chloroaniline) in Air .......................................................... 236
Procedure for the Preparation of Tissue for Analysis ..................................... 237
x VVC 000008975
Asbestos Fiber in Air ......................................................................................... 239 Sodium Hydroxide in Air..................................................................................... 241 Phosphorous in Air .............................................................................................. 242 Benzidine in Air.................................................................................................... 243 Polychlorinated Biphenyls (PCB) in Air............................................................ 244 Chrysotile Asbestos in Bulk Samples .............................................................. 245 3,3'-Dichlorobenzidine in Air.................................................................... -........ 246 Methyl Alcohol in Air.......................................................................................... 247 Hydrazine Compounds in Air ............................................................................. 248 Benzo(a)Pyrene in Particulates ........................................................................... 251 N-Nitrosodimethylamine in Air........................................................................... 252 Polychlorinated Biphenyls (PCB) in Air ............................................................ 253 Thiophene in Air .................................................................................................. 255 Azelaic Acid in Air ............................................................................................ 256 Phosphorous (white) in Air ................................................................................. 257 Free Silica (Quartz, Crystobalite, Tridymite) in Airborne Dust...................... 259 Lead in Blood and Urine...................................................................................... 262 Index
xi vvc 000008976
CONTENTS OF VOLUME 2
PART II Standards Completion Program Validated Methods
Acetone ................................................................................................................ Antimony and compounds (as Sb).........................................................................
2-Butanone ........................................................................................................... Hydrogen sulfide................................................................................................... Manganese and compounds (as Mn) ............................................................... Ozone .................................................................................................................... Camphor................................................................................................................ Mesityl oxide ................................................. 5-Methyl-3-heptanone ........................................................................................ Methyl (n-amyl) ketone ...................................................................................... Ethyl butyl ketone .............................................................................................. Hexone ..................................-..............................................................................
Cyclohexanone ....................................................................................... ............. 2-Pentanone ......................................................................................................... p-tert-Butylcoluene ............................................................................................... Cumene ................................................................................................................ Vinyl toluene ....................................................................................................... alpha-Methyl styrene .......................................................................................... Terphenyls ........................................................................................................... Cyclohexane .........................................................................................................
Ethyl benzene............................................................................................. Styrene .................................................................................................................. sec-Amyl acetate.............................................................. :................................... tert-Butyl acetate ................................................................................................. Dibutyl phthalate ................................................................................................. Ethyl acrylate ....................................................................................................... Ethyl formate ....................................................................................................... Methyl isoamyl acetate..........................................................................................
Methyl acrylate .................................................................................................. Methyl cellosolve acetate ..................................................................................
Di-2-Ethylhexyl phthalate.................................................................................... 2-Ethoxyethyl acetate ........................................................................................ Methyl acetate ..................................................................................................... Isobutyl acetate .................................................................................................. Isoamyl acetate .................................................................................................. sec-Butyl acetate ................................................................................................ Butyl acetate .................................................................................. n-Propyl acetate ......................................... Ethyl acetate......................................................................................................... Isopropyl acetate ................................................................................................
n-Amyl acetate..................................................................................................... Allyl alcohol ......................................................................................................... sec-Butyl alcohol ................................................................................................
Cyclohexanol .....................................................................;................................ Diacetone alcohol ........... Ethyl alcohol .......................................................................................................
Hydroquinone ......................................................................................................
SI S2
S3 S4 S5 S8 S10 S12 SI3 S15 SI6 SIS
S19 S20 S22 S23 S25 S26 S27 S28
S29 S30 S31 S32 S33 S35 S3 6 S37
S38 S39
S40 S41 S42 S44 S45 S46 S47 S48 S49 S50
S51 S52 S53
S54 S55 S56
S57
' iii
VVC 000008977
Isoamyl alcohol .................................................................................................. *S5.8 Methyl alcohol .................................................................................................... S59 Methyl isobutyl carbinol .................................................................................... S60
Propyl alcohol .................................................................................................... S62 tert-Butyl alcohol.......................................................................................................S63
Isobutyl alcohol ........
S64
Isopropyl alcohol ................................................................................................ S65 Butyl alcohol ....................................................................................................... S66
Chlorinated camphene ........................................................................................ S67 Dipropylene glycol methyl ether ....................................................................... S69
Glycidol ............................................................................................................... S70
Methylal ............................................................................................................... S71
Phenyl ether ......................................................................................................... S72
Phenyl ether-Biphenyl mixture (vapor) ..........................
S73
Phenyl glycidyl ether ................
S74
Propylene oxide .................................................................................................. S75
2-Butoxy ethanol ............................................................................................... S76 Isopropyl glycidyl ether ...................................................................................... S77
Tetrahydrofuran .................................................................................................. S78
Methyl cellosolve ................................................................................................ S79 Ethyl ether ........................................................................................................... S80
n-Butyl glycidyl ether ........................................................................................ S81
Cyclohexene .......
S82
Naphtha, coal tar ................................................................................................ S86
Propane ............................................................................................................... S87 Turpentine ........................................................................................................... S88
Heptane ............................................................................................................... S89
Hexane ................................................................................................................. S90
Butadiene ............................................................................................................. S91 Ketene ................................................................................................................. S92
LPG (Liquified petroleum gas) ......................................................................... S93 Methylcyclohexane .............................................................................................. S94
Propylene dichloride............................................................................................ S95 Pentachloronaphthalene ...................................................................................... S96
Octachloronaphthalene ........................................................................................ S97
Methyl iodide ....................................................................................................... S98 Hexachloronaphthalene ...................................................................................... SI00
Hexachloroethane ................................................................................................ S101 Fluorotrichloromethane ..................................................................................... SI02 Ethylene chlorohydrin ........................................................................................ Si03
Ethylene dibromide ............................................................................................ S104
Ethyl bromide .................................................................................................... SI06 Difluorodibromomethane .................................................................................... S107
Dichlorotetrafluoroethane .................................................................................... S108 Dichloromonofluoromethane............................................................................... S109 1,2-Dichloroethylene .......................................................................................... SI 10
Dichlorodifiuoromethane .................................................................................... Sill
Chloroprene .......................................
SI 12
Chlorobromomethane ................
Si 13
Bromoform ........................................................................................................... SI 14
Benzyl chloride..................................................................................................... SI 15
IV
VVC 000006978
Allyl chloride ...................................... Acetylene tetrabromide....................... Epichlorohydrin .................................. Chlorinated diphenyl oxide.... ............ Chlorodiphenyl, 54% chlorine ........ Ethylene dichloride ........................... 1,1-Dichloroethane ............................. 1.1.2.2- Tetrachloroethane................ Trifluoromonobromomethane ............. 1,2,3-Trichloropropane....................... Trichloronaphthalene ......................... 1.1.2- TrichIoro-lt2,2-trifluoroethane . Tetrachloronaphthalene ..................... 1.1.1.2- Tetrachloro-2,2-difluoroethane 1 tl,2,2-Tetrachloro-l ,2-difluoroethane Chlorobenzene .................................... 1.1.2- Trichloroethane ...................
Index
.. S116 - SI 17
.. SI 18 .. SI 19 .. S121 . S122 .. S123 .. S124
.. S125 .. S126 .. S128 .. S129 .. S130 .. S131 .. S132 .. SI33 .. S134
v
VVC 000008979
CONTENTS OF VOLUME 3
PART n Standards Completion Program Validated Methods
o-Dichlorobenzene .............................................................................................. SI35
Diazomethane .................
S137
Diethylamine .................................................................................. ................... SI39
Dimethylamine .................................................................................................... SI42
1.1- DimethyIhydrazine ................................... -............................................... S143
Ethylamine .......................................................................................................... SI44
N-Ethylmorpholine .............................................................................................. SI 46
Isopropylamine .................................................................................................... S147
Monomethyl hydrazine ....................................................................................... SI49
Morpholine .......................................................................................................... SI50
Triethylamine ...................................................................................................... S152
Monomethyl aniline ............................................................................................ SI53
Tetramethyl succinonitrile ................................................................................. SI55
Acrylonitrile ........................................................................................................ SI56 Phenylhydrazine .................................................................................................. SI60
Pyridine .............................................................................................................. SI61
Xylidine .............................. ............................................................................... SI62
Dimethylaniline.................................................................................................... SI 64
Acetonitrile .......................................................................................................... SI65
Cresol, all isomers .............................................................................................. S167
o-Toluidine .......................................................................................................... SI 68
Acetic anhydride ................................................................................................ SI70
Sulfuric acid ........................................................................................................ S174
Hydrogen bromide .............................................................................................. S175
Hydrogen fluoride ................................................................................................ S176
2-Hexanone ........................................................................................................ S178
Phthalic anhydride .............;............................................................................... SI79
Tin, inorganic compounds, except oxides.......................................................... SI 83
Zirconium compounds (as Zr) .................................
S185
Copper, dusts and mists..................................................................................... Si 86
Tellurium hexafluoride ....................................................................................... SI 87
Rhodium, metal fume and dust........................................................................... SI 88
Rhodium, soluble salts ....................................................................................... S189
Selenium compounds (as Se) ............................................................................. S190
Platinum, soluble salts (as Pt) ........................................................................... S191
Molybdenum, soluble compounds .................................................................... SI93
Barium, soluble compounds .............................
S198
Yttrium ................................................................................................................ S200
Tellurium ......................
S204
Calcium oxide...................................................................................................... S205
Nickel, metal and soluble compounds (as Ni).................................................... S206
Tributyl phosphate ............................................................................................. S208
Triorthocresyl phosphate ................................................................................... S209
Triphenyl phosphate ......... .;v............................................................................ S210
1.1- Dichloro-l-nitroethane ............................................................................... S213
Ethylene glycol dinitrate/'Nitroglycerin ................................
S216
Nitrobenzene ...................................................................................................... S217
iii
VVC 000008980
p-Nitrochlorobenzene .......................................................................................... S218
Nitrotoluene ......................................................................................................... S223
Tetranitromethane .............................................................................................. S224
Tetryl (2,4,6-Trinitrophenylmethylnitramine) .................................................. S225
n-Propylnitrate .............
S227
Arsine .................-....... ......................................................................................... S229
Hydrazine ........................................ -................................................................... S237
Hydrogen chloride .............................................................................................. S246
Carbon disulfide .................................................................. .....---....... --........ S248
Carbon dioxide .................................................................................................... S249
Cyanide (as CN) .................................................................................................. S250
Dimethyl acetamide ............................................................................................ S254
Dimethyl formamide............................................................................................ S255
Carbon black ...................................................................................................... S262
Ethyl silicate ................................................
S264
Oil mist, mineral.................................................................................................. S272
Carbaryl ......................
S273
DDT ................................................................................................................... S274
Aldrin ................................................................................................................. S275
p-Dichlorobenzene .............................................................................................. S281
Dieldrin ................................................
S283
EPN (O-Eihyl-O-p-nitrophcnyl phenylphosphonothiolaic) ............................ S285
Ethylene oxide .................................................................................................... S286
Lindane ............................................................................................................... S290
Naphthalene ........................................................................................................ S292
Nicotine ..........................................
S293
Parathion ............................................................................................................. S295
Thallium, soluble compounds (as Tl) ................................................................ S306
Arsenic and compounds (asAs) .......................................................................... S309
Aniline ................................................................................................................. S310
Benzene .............................................................................................................. S311
Cadmium dust ............................................................................................
S312
Cadmium fume .................................................................................................. S313
Carbon tetrachloride........................................................................................... S314
Silica, crystalline .................................................................................................. S315
Chromic acid and chromates ............................................................................. S317
Xylene ................................................................................................................ S318
Chromium, soluble chromicand chromous salts (as Cr) ................................. S323
Methyl chloroform ........
S328
Methylene chloride ........................................................................................... S329
Phenol -............................................................................................................... S330
Phosphoric acid .....................................................
S333
Tetrachloroelhylene ........................................................................................... S335
Trichloroethylene ................................................................................................ S336
Beryllium and berylliumcompounds (as Be) ................................................... S339
Lead and inorganic lead compounds .......................-....................................... S341
Toluene .............................................................................................................. S343
Boron oxide ........................................................................................................ S349
Chloroform ...............................v......................................................................... S351
Chromium, metal and insoluble compounds........................................................ S352
Dichloroethyl ether.............................................................................................. S357
iv VVC 00000B981
Diisobutyl ketone ................................................................................................ S358
Dioxane ..................................................................-............................................................... S3 60 Isophoione ............................................................................................................................. S367
Isopropyl ether .................................................................................................... S368
Magnesium oxide fume .................................................................................................... S3 69
Malathion ............................................................................................................ S370 Methyl bromide .................................................................................................. S372
Molybdenum, insoluble compounds .............................................................................. S376
Octane ................................................................................................................. S378 Pentane .......................................-....................................................................... S379 Petroleum distillates ........................................................................................... S380 Stoddard solvent.................................................................................................. S382 Titanium dioxide ............................................................................................... S385 Vanadium, V205 dust......................................................................................... S391 Index
v
VVC 000008902