ALCOHOLS I 1400

1 ALCOHOLS I 1400 Table 1 MW: Table 1 CAS: Table 2 RTECS: Table 2 METHOD: 1400, Issue 2 EVALUATION: PARTIALI ssue 1: 15 February 1984 Issue 2: 15 August 1994 OSHA :Table 2 NIOSH:Table 2 ACGIH:Table 2 PROPERTIES: Table 1 COMPOUNDS AND SYNONYMS:(1) ethanol: ethyl alcohol.(2) isopropyl alcohol: 2-propanol.(3) tert-butyl alcohol: :SOLID SORBENT TUBE(coconut shell charcoal, 100 mg/50 mg)FLOW to L/min( L/min for ethyl alcohol)(1)(2)(3)VOL- L -MAX:1 L3 L10 LSHIPMENT:cooledSAMPLE STABILITY:unknown, store in freezerBLANKS:2 to 10 field blanks per setMEASUREMENTTECHNIQUE:GAS CHROMATOGRAPHY, FIDANALYTE:compounds aboveDESORPTION:1 mL 1% 2-butanol in CS2 INJECTION VOLUME:5 LTEMPERATURE-INJECTION:200 C -DETECTOR:250-300 C -COLUMN: 65-70 CCARRIER GAS:N2 or He, 30 mL/minCOLUMN:glass, 2 m x 4-mm ID, Carbowax1500 on 60/80 Carbopack C or equivalentCALIBRATION:solutions of analyte in eluent (internalstandard optional)RANGE ANDPRECISION:see EVALUATION OF METHODESTIMATED mg per sample [2]ACCURACYRANGE STUDIED:see EVALUATION OF METHODBIAS:not significant [1]OVERALL PRECISION (S rT): see EVALUATION OFMETHODACCURACY: 14%APPLICABILITY.

2 The working ranges are 16 to 1000 ppm ethanol (30 to 1900 mg/m3) for a 1-L air sample; 4 to 400 ppmisopropyl alcohol (10 to 1000 mg/m3) for a 3-L air sample; and 1 to 100 ppm t-butyl alcohol (3 to 300 mg/m3) for a 10-L air method employs a simple desorption and may be used to determine two or more analytes simultaneously by varying GCconditions ( , temperature programming).INTERFERENCES: High humidity reduces sampling efficiency. The methods were validated using a 3 m x 3-mm stainless steelcolumn packed with 10% FFAP on Chromosorb W-AW; other columns with equal or better resolution ( , capillary) may be volatile compounds may displace more volatile compounds on the METHODS: This method combines and replaces Methods S56, S65 and S63 [3].NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94 ALCOHOLS I: METHOD 1400, Issue 2, dated 15 August 1994 - Page 2 of 4 : Carbon disulfide* (chromatographicgrade) with 1% (v/v) 2-butanol and v/vn-undecane, v/v ethyl benzene, or othersuitable internal , reagent , , , compressed, filtered.

3 *See SPECIAL : : glass tube, 7 cm long, 6-mm OD,4-mm ID, flame-sealed ends, containing twosections of activated (600 C) coconut shellcharcoal (front = 100 mg; back = 50 mg)separated by a 2-mm urethane foam plug. Asilylated glass wool plug precedes the frontsection and a 3-mm urethane foam plugfollows the back section. Pressure dropacross the tube at 1 L/min airflow must beless than kPa. Tubes are commerciallyavailable. sampling pump, to L/min,with flexible connecting tubing. , bagged (Blue Ice, or equivalent). chromatograph, FID, integrator andcolumn (page 1400-1). , glass, 2-mL, PTFE-lined crimp caps. , 10- L, readable to L. flasks, PRECAUTIONS: Carbon disulfide is toxic and an acute fire and explosion hazard (flash point= -30 C); all work with it must be done in a each personal sampling pump with a representative sampler in the ends of the sampler immediately before sampling.

4 Attach sampler to personalsampling pump with flexible at an accurately known flow rate between and L/min for a total sample size to 1 L (ethanol), to 3 L (isopropyl alcohol) or to 10 L (t-butyl alcohol). the samplers with plastic (not rubber) caps and pack securely with bagged refrigerant the front and back sorbent sections of the sampler tube in separate vials. Discard theglass wool and foam mL eluent to each vial. Attach crimp cap to each to stand 30 min with occasional AND QUALITY daily with at least six working standards covering the range of the known amounts of analyte to eluent in 10-mL volumetric flasks and dilute to the together with samples and blanks (steps 11 and 12). calibration graph (ratio of peak area of analyte to peak area of internal standard analyte). desorption efficiency (DE) at least once for each batch of charcoal used for samplingin the calibration range (step 8). Prepare three tubes at each of five levels plus three Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94 ALCOHOLS I: METHOD 1400, Issue 2, dated 15 August 1994 - Page 3 of and discard back sorbent section of a media blank a known amount of analyte directly onto front sorbent section with a microliter the tube.

5 Allow to stand (steps 5 through 7) and analyze together with working standards (steps 11 and 12). a graph of DE vs. mg analyte three quality control blind spikes and three analyst spikes to insure that the calibrationgraph and DE graph are in gas chromatograph according to manufacturer's recommendations and to conditions givenon page 1400-1. Inject sample aliquot manually using solvent flush technique or :If peak area is above the linear range of the working standards, dilute with eluent,reanalyze and apply the appropriate dilution factor in peak area. Divide the peak area of analyte by the peak area of internal standard onthe same the mass, mg (corrected for DE) of analyte found in the sample front (Wf) and back(Wb) sorbent sections, and in the average media blank front (Bf) and back (Bb) sorbent :If Wb > Wf/10, report breakthrough and possible sample concentration, C, of analyte in the air volume sampled, V (L):EVALUATION OF METHOD:Methods S56, S65 and S63 were issued on January 17, 1975 [3], and validated using 1-, 3- and 10-Lair samples, respectively, of atmospheres generated in dry air by calibrated syringe drive from absoluteethanol, 2-propanol and t-butyl alcohol [1].

6 No stability studies were done. Overall precision andrecovery were as shown below, representing non-significant bias in each method:OverallMeasurement PrecisionRecovery Range Studied BreakthroughAvg. PrecisionMethod (S rT) (%) mg/m3 mg per sample @ 2X OSHA DE (S r) to 33001 to 4 * to 18901 to 5 * to to * *Over the range studied. Each laboratory must do their own DE Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94 ALCOHOLS I: METHOD 1400, Issue 2, dated 15 August 1994 - Page 4 of 4 REFERENCES:[1]Documentation of the NIOSH Validation Tests, Department of Health, Education, andWelfare, (NIOSH) Publication No. 77-185 (1977).[2]User check, UBTL, NIOSH Sequence #3990-S (unpublished, November 3, 1983).[3]NIOSH Manual of Analytical Methods, 2nd ed., V. 2., S56, S65 and S63, Department ofHealth, Education, and Welfare, Publ. (NIOSH) 77-157-B (1977).METHOD REVISED BY:George Williamson, NIOSH/DPSE; methods originally validated under NIOSH Contract 1.

7 PROPERTIES VP @ mg/m3 Density 20 C,= 1 ppm@ 20 C BP kPa Compound Formula @ NTP (g/mL) ( C) (mm Hg)EthanolCH3CH2OH; (42)Isopropyl alcoholCH3CH(OH)CH3; (33)tert-Butyl alcohol (CH3)3 COH; ; C4H10 OMP = (31) CTABLE 2. GENERAL INFORMATION. EXPOSURE LIMITS (ppm) COMPOUND OSHA NIOSHACGIH CAS# RTECS# EthanolTWA 10001000100064-17-5KQ6300000 Isopropyl alcoholTWA 400 400 40067-63-0NT8050000 500 STEL 500 STEL tert-Butyl alcoholTWA 100 100 10075-65-0EO1925000 150 STELNIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94