HYDROCARBONS, HALGENATED 1003

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1 HYDRORBONS, HLGENTED 0 Table 1 MW: Table 1 S: Table 1 RTES: Table 1 METHOD:0, Issue 2 EVLUTION: PRTIL Issue 1: 15 February 1984 Issue 2: 15 ugust 1994 OSH : See TBLE 1 NIOSH: See TBLE 1 GIH: See TBLE 1 PROPERTIES: See TBLE 2 OMPOUNDS: benzyl chloride chlorobromomethane 1,1-dichloroethane 1,1,1-trichloroethane (synonyms bromoform chlorform 1,2-dichloroethylene tetrachloroethlene in Table 1 carbon tetrachloride o-dichlorobenzene ethylene dichloride 1,1,2-trichloroethane chlorobenzene p-dichlorobenzene hexachloroethane 1,2,-trichloropropane SMPLER: FLOW RTE: VOL-MIN: Table -MX: Table SMPLING SOLID SORBENT TUBE (coconut shell charcoal, 0 mg/50 mg 0.01 to 0.2 L/min TEHNIQUE: NLYTE: DESORPTION: INJETION VOLUME: MESUREMENT GS HROMTOGRPHY, FID compounds above 1 ml S 2, stand 0 min 5 L SHIPMENT: routine TEMPERTURE: Table 4 SMPLE STBILITY: BLNKS: not determined 2 to field blanks per set RRIER GS: OLUMN: N 2 or He, 0 ml/min Table 4; alternates are SP-20, Sp- 20 with 0.1% arbowax 1500 or DB-1 fused silica capillary column URY RNGE STUDIED: see EVLUTION OF METHOD [1] BIS: see EVLUTION OF METHOD [1] OVERLL PREISION ( rt : see EVLUTION OF METHOD [1] LIBRTION: standard solutions of analyte in S 2 RNGE: Table 4 ESTIMTED LOD: 0.1 mg per sample [2] PREISION ( r : see EVLUTION OF METHOD URY: see EVLUTION OF METHOD [1] PPLIBILITY: See Table for working ranges. This method can be used for simultaneous determination of two or more substances suspected to be present by changing gas chromatographic conditions (i.e., temperature program. High humidity during sampling will prevent organic vapors from being trapped efficiently on the sorbent and greatly decreases breakthrough volume. INTERFERENES: None identified. The chromatographic column or separation conditions may be changed to circumvent interferences. OTHER METHODS: This method combines and replaces P&M 127 [], S1 [4], S1 [5], S11 [6], S114 [7], S115 [8], S122 [9], S12 [], S126 [11], S1 [12], S14 [1], S15 [14], S281 [15], S14 [16], S28 [17], S5 [18], S51 [19], and Method 0 (dated 2/15/84. NIOSH Manual of nalytical Methods (NMM, Fourth Edition

2 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - 2 of 8 REGENTS: 1. arbon disulfide, chrom atographic quality.* 2. nalyte, reagent grade.. alibration stock solutions: a. benzyl chloride, mg/ml in n-heptane. b. bromoform, mg/ml in n-heptane. c. o-dichloro benzene, 00 m g/ml in acetone d. hexachloroethane, 25 mg/ml in toluene. 4. Decane, n-undecane, octane or other internal standards (see step Nitrogen or helium, purified. 6. Hydrogen, prepurified. 7. ir, filtered. * See SPEIL PREUTIONS EQUIPMENT: 1. Sampler: glass tube, 7 cm long, 6-mm OD, 4-mm ID, flame-sealed ends w ith plastic caps, containing two sections of 20/40 mesh activated (600 coconut shell charcoal (front = 0 mg; back = 50 mg separated by a 2-mm urethane foam plug. silylated glass wool plug precedes the front section and a -mm urethane foam plug follows the back section. Pressure drop across the tube at 1 L/min airflow must be less than.4 kpa. Tubes are com mercially available (e.g., SK # Personal sampling pump, 0.01 to 0.2 L min, with flexible connecting tubing.. Gas chromatograph, FID, integrator and column (see Table. 4. Vials, 2-mL, glass, PTFE-lined septum crimp caps. 5. Volumetric flasks, -ml. 6. Syringes, - L, readable to 0.1 L. 7. Pipet, TD, 1-mL, with pipet bulb. SPEIL PREUTIONS: arbon disulfide is toxic and a serious fire and explosion hazard (flash point = -0. Work with it only in a hood. Several of the analytes are suspect carcinogens (Table 1. n-heptane, n-hexane, and acetone are fire hazards. SMPLING: 1. alibrate each personal sampling pump with a representative sampler in line. 2. Break the ends of the sampler immediately before sampling. ttach sampler to personal sampling pump with flexible tubing.. Sample at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample size between the limits shown in Table ap the samplers. Pa ck securely for shipment. SMPLE PREPRTION: 5. Place the front and back sorbent sections of the sampler tube in separate vials. Discard the glass wool and foam plugs. 6. dd 1.0 ml S 2 to ea ch v ial. ap e ach vial. NOTE: suitable internal standard, such as decane [16], n-undecane [6,19], or octane [9,1,17] at 0.1% (v/v may be added at this step and step llow to stand 0 min with occasional agitation. NIOSH Manual of nalytical Methods (NMM, Fourth Edition

3 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - of 8 LIBRTION ND QULITY ONTROL: 8. alibrate daily with at least six working standards over the approp riate range (Ta ble. a. dd known amounts of neat analyte or calibration stock solution to S 2 in -ml volumetric flasks and dilute to the mark. b. nalyze w ith samples a nd blanks (steps 11 an d 12. c. Prepare calibration graph (peak area vs. mg an alyte. 9. Determine desorption efficiency (DE at least once for each lot of charcoal used for sampling in the range o f interest. Pre pare thr ee tu bes at ea ch o f five c onc entr ation s plu s three m edia blanks. a. Rem ove and discard back sorbent section of a media blank sa mpler. b. Inject a known amount (2 to 20 µl of pure analyte, or calibration stock solution (see REGENTS,., directly onto front sorbent section with a microliter syringe. c. ap the tub e. llow to stand ove rnight. d. Desorb (steps 5 through 7 and analyze together with working standards (steps 11 and 12. e. Prepare a graph of DE vs. mg analyte recovered.. nalyze three quality control blind spikes and three analyst spikes to insure that the calibration graph a nd D E gr aph are in co ntro l. MESUREMENT: 11. Set gas chromatograph according to manufacturer's recommendations and to conditions given on page 0-1 and in Table. Inject sample aliquot either manually using solvent flush technique o r with autosam pler. NOTE: If peak area is above the linear range of the working standards, dilute with S 2, reanalyze and apply the appropriate dilution factor in calculations. 12. Measure peak area. LULTIONS: 1. Determine the mass, mg (corrected for DE, of analyte found in the sample front (W f and back (W b sorbent sections and in the average media blank front (B f and back (B b sorbent sections. NOTE: If W b > W f /, report breakthrough and possible sample loss. 14. alculate concentration,, of analyte in the air volume sampled, V (L: NIOSH Manual of nalytical Methods (NMM, Fourth Edition

4 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - 4 of 8 EVLUTION OF METHOD: Laboratory testing was performed with spiked samples and generated atmospheres using SK Lot 5 coconut shell charcoal [1]. Results were: ompound Range mg/m Sample Size Bias % Precision Overall Measurement ccuracy ±% Desorption Efficiency Ref. Benzyl chloride arbon tetrachloride hlorobenzene hlorobromomethane hloroform o-dichlorobenzene p-dichlorobenzene 1,2-Dichloroethylene* Ethylene dichloride Hexachloroethane 1,1,1-Trichloroethane Tetrachloroethylene 1,1,2-Trichloroethane 1,2,-Trichloropropan e L L 15 L L 5 L 15 L L L L L L L L L L L mg mg mg mg mg mg mg mg mg mg mg mg mg mg mg mg [8] [7] [16] [12] [6] [19] [14] [15] [] [5] [9] [4] [17] [18] [1] [11] *isomer used (i.e., cis- or trans- in evaluation unknown. REFERENES: [1] Documentation of the NIOSH Validation Tests, S1, S1, S11, S114, S115, S122, S12, S126, S1, S14, S15, S281, S14, S28, S5, S51, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH (1977, available as Stock No. PB from NTIS, Springfield, V [2] User check, UBTL, NIOSH Sequences #990-T, 990-U and 990-W (NIOSH, unpublished, Novem ber, 198 and 40 4-J (NIOS H, unpublished, pril, [] NIOSH Manual of nalytical Methods, 2nd ed., V. 1., P&M 127, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H (1977. [4] Ibid., V. 2., S1, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH B (1977. [5] Ibid., S1. [6] Ibid., S11. [7] Ibid., S114. [8] Ibid., S115. [9] Ibid., S122. [] Ibid., S12. [11] Ibid., S126. [12] Ibid., S1. [1] Ibid., S14. [14] Ibid., V., S15, U.S. Departm ent of Health, Education, and Welfare, Publ. (NIOSH (1977. [15] Ibid., S281. [16] Ibid., S14. [17] Ibid., S28. [18] Ibid., S5. [19] Ibid., S51. [20] NIOSH/OSH Occupational Health Guidelines for hemical Hazards, U.S. Department of Health and Human Services, Publ. (NIOSH (1981, available as Stock #PB from NTIS, Springfield, V [21] NIOSH urrent Intelligence Bulletin 27, hloroethanes: Review of Toxicity, U.S. Department of Health, Edu cation, and W elfare, Publ. (NIOS H (1978. NIOSH Manual of nalytical Methods (NMM, Fourth Edition

5 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - 5 of 8 [22] NIOSH urrent Intelligence Bulletin 20, Tetrachloroethylene (Perchloroethylene, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H (1978. [2] riteria for a Recommended Standard...Occupational Exposure to Benzyl hloride, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H (1978. [24] riteria for a Recommended Standard...Occupational Exposure to arbon Tetrachloride, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H 76-1 (1976. [25] riteria for a Recommended Standard...Occupational Exposure to hloroform, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H (1975. [26] riteria for a Recommended Standard...Occupational Exposure to Ethylene Dichloride, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H (1976. [27] riteria for a Recommended Standard...Occupational Exposure to 1,1,1-Trichloroethane, U.S. Department of Health, Education, and Welfare, Publ. (NIOS H (1976. [28] riteria for a Recommended Standard...Occupational Exposure to Tetrachloroethylene (Perchloroethylene, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH (1976. METHOD WRITTEN (REVISED BY: G. David Foley and Yvonne T. Gagnon, NIOSH/DPSE; methods originally validated under NIOSH ontract D NIOSH Manual of nalytical Methods (NMM, Fourth Edition

6 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - 6 of 8 TBLE 1. GENERL INFORMTION. ompound RTES Synonyms OSH/NIOSH/GIH (ppm Benzyl chloride a ( 6 H 5 H 2 l; XS (HBr ; PB arbon tetrachloride ab (l 4 ; FG hlorobenzene ( 6 H 5 l; Z hlorobromomethane (H 2 Brl; P hloroform ab (Hl ; FS90000 o-dichlorobenzene c (1,2-6 H 4 l 2 ; Z p-dichlorobenzene ac (1,4-6 H 4 l 2 ; Z (H Hl 2 ; KI ,2-Dichloroethylene (lh=hl; KV Ethylene dichloride ab (lh 2 H 2 l; KI Hexachloroethane ac (l l ; KI ,1,1-trichloroethane (H l ; KJ Tetrachloroethylene ab (l 2 =l 2 ; KX ,1,2-Trichloroethane ad (l 2 HH 2 l; KJ ,2,-Trichloropropane a (H 2 lhlh 2 l; TZ (chloromethyl benzene; -chlorotoluene; S # tribromomethane; S # tetrachloromethane; S # monochlorobenzene; phenyl chloride; S # bromochloromethane; Halon 11; S # trichloromethane; S # ,2-dichlorobenzene; S # ,4-dichlorobenzene; S # ethylidene chloride; S #75-4- acetylene dichloride; 1,2-dichloroethene; S # ,2-dichloroethane; S # perchloroethane; S # methyl chloroform; S # perchloroethylene; S # vinyl trichloride; S # allyl trichloride; glycerol trichlorohydrin; S # / 1.0/1 0.5 (skin/0.5 (skin/0.5 (skin, 25/STEL 2 (1 h/5 (skin 75/--/ 200/200/200 50/STEL 2/ 50/ 50/25 (skin; STEL 50 75/1.7 (LOQ/75, STEL 1 0/0/0 200/200/200 50, 0/1, STEL 2/ 1 (skin/1/1 (skin 50/ 50/50, STEL 450 0, 200, P 00/0.4 (LOQ/ 25, STEL 0 (skin/ (skin/ (skin 50/ (skin/ (skin a Suspect carcinogen [20,21,22]; b Group I Pesticide; c Group II Pesticide; d Group III Pesticide NIOSH Manual of nalytical Methods (NMM, Fourth Edition

7 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - 7 of 8 TBLE 2. PHYSIL PROPERTIES ompound RTES M.W. mg/m = 1 NTP Synonyms Properties Benzyl chloride ( 6 H 5 H 2 l (chloromethyl benzene; -chlorotoluene liquid; BP 179 ; MP 48 to 4 ; d 20 ; flash pt. 67 (HBr tribromomethane liquid, d 2.887; BP 148 ; nonflammable arbon tetrachloride (l tetrachloromethane liquid; d 1.585; BP 76.7 ; FP 2.0 ; VP ; vapor density (air = 1 5. hlorobenzene ( 6 H 5 l monochlorobenzene; phenyl chloride liquid; d 25 ; BP 11.6 ; MP 45 ; flash pt ( hlorobromomethane (H 2 Brl bromochloromethane; Halon 11 liquid; d 20 ; BP 68 ; MP 88 ; nonflammable hloroform (Hl trichloromethane liquid, d 20 ; BP 61.2 ; FP -6.5 o-dichlorobenzene (1,2-6 H 4 l ,2-dichlorobenzene liquid; d 1.284; BP 172 to 179 ; FP 17 ; flash pt p-dichlorobenzene (1,4-6 H 4 l ,4-dichlorobenzene solid crystals; d 1.458; BP 17.7 ; MP 5 ; sublimes; flash pt (H Hl ethylidene chloride liquid, d 20 ; BP 57 to 59 ; FP 98 1,2-Dichloroethylene (lh=hl acetylene dichloride; 1,2-dichloroethene liquid; transisomer; d 1.257; BP 47 to 49 ; MP 57 ; cis-isomer; d 1.282; BP 58 to 60 ; flash pt..9 ; FP 80 Ethylene dichloride (lh 2 H 2 l ,2-dichloroethane liquid; d 20 ; BP 8.5 ; FP 5.5 ; flash pt. 1 ; explosive limits in air 6 to 16% Hexachloroethane (l l perchloroethane solid; d 2.091; MP 185 ; BP sublimes at 187 1,1,1-trichloroethane (H l methyl chloroform liquid; d 1.25; BP 75 ; FP 0.4 ; nonflammable Tetrachloroethylene (l 2 =l perchloroethylene liquid; d 20 ; BP 121 ; FP ,1,2-Trichloroethane (l 2 HH 2 l vinyl trichloride liquid; d 20 ; BP 11.7 ; FP 6.4 ; VP 19 mm 20 1,2,-Trichloropropane (H 2 lhlh 2 l allyl trichloride; glycerol trichlorohydrin liquid; d 20 ; BP ; FP 15 ; flash pt (O NIOSH Manual of nalytical Methods (NMM, Fourth Edition

8 HYDRORBONS, HLOGENTED: METHOD 0, Issue 2, dated 15 ugust Page - 8 of 8 TBLE. SMPLING LIMITS. ompound ir Sample Volume (L Min Max Target Working Range, ppm, at Max Sample Volume Benzyl chloride arbon tetrachloride hlorobenzene hlorobromomethane hloroform o-dichlorobenzene p-dichlorobenzene 1,2-Dichloroethylene Ethylene dichloride Hexachloroethane 1,1,1-Trichloroethane Tetrachloroethylene 1,1,2-Trichloroethane 1,2,-Trichloropropane 1 ppm 0.5 ppm 75 ppm 200 ppm 50 ppm 50 ppm 75 ppm 0 ppm 200 ppm 50 1 ppm 50 ppm 0 ppm ppm 50 ppm to to 4 2 to 5 to to to to to 0 4 to to to to to to to 64 to TBLE 4. MESUREMENT PRMETERS. ompound olumn* Temp. ( olumn/injector/detector Range (mg per sample Benzyl chloride arbon tetrachloride hlorobenzene hlorobromomethane hloroform o-dichlorobenzene p-dichlorobenzene 1,2-Dichloroethylene Ethylene dichloride Hexachloroethane 1,1,1-Trichloroethane Tetrachloroethylene 1,1,2-Trichloroethane 1,2,-Trichloropropane B B D E 160/170/2 10/170/2 60/155/200 5/190/250 80/170/2 75/155/ /225/ /225/275 50/0/175 60/170/2 70/225/250 1/170/2 70/225/250 90/225/250 70/250/ /180/ to to to to 0.5 to to to 0.2 to to to to to to to to 2 0. to 9 * = m x -mm OD stainless steel, % SP-00 on 80/0 mesh hromosorb WHP. B = 6 m x -mm OD, otherwise same as. = m x -mm OD stainless steel, % OV-1 on 0/120 mesh hromosorb WHP. D = m x 6-mm OD glass, % SP-2250 on 80/0 mesh hromosorb WHP. E = m x -mm OD stainless steel, % FFP on 80/0 mesh hromosorb WHP. NIOSH Manual of nalytical Methods (NMM, Fourth Edition

Formulas: See Table 1 MW: Table 1 CAS: Table 1 RTECS: Table 1. METHOD: 2555, Issue 1 EVALUATION: PARTIAL Issue 1: 15 March 2003

KETONES I 2555 Formulas: See Table 1 MW: Table 1 CAS: Table 1 RTECS: Table 1 METHOD: 2555, Issue 1 EVALUATION: PARTIAL Issue 1: 15 March 2003 OSHA : See Table 2 NIOSH: See Table 2 ACGIH: See Table 2 PROPERTIES: