Document qkeNdz6RK01JM06nMq1X2pJq5

FORMULA: Table 1 AHIHOETHANOL COMPOUNDS METHOO: 2007 M.U.: Table 1 ISSUEO: VI5/85 REVISION #1: 8/15/87 COMPOUNDS 2-ami noethanol: ethanol amine; 2-hydroxyethy1 amine; CAS #141-43-5. and 2--dibutyl ami noethanol: CAS #102-81-8. SYNONYMS: 2-dlethylami noethanol: 2-hydroxytriethylamine; CAS #100-37-8. OSHA/NtOSH/ACGIH: Table 1 PROPERTIES: Table 1 _____________________ SAMPLING___________________ _____________________ MEASUREMENT___________________ SAMPLER: SOLID SORBENT TUBE {TECHNIQUE: GAS CHROMATOGRAPHY, FID (silica gel, 300 mg/150 mg) !ANALYTE: compounds above FLOW RATE: 0.01 to 0.2 LAain !DESORPTION: 2 mL 4:1 (v/v) methanol:water; stand VOL-HIN: 4 L ! 2 hrs with occasional shaking -MAX: 24 L 1 INJECTION VOLUME: 3 pL FIELD TREATMENT: add 20 pL cone. HC1 to ! silica gel iimediately TEMPERATURE-INJECTION: 150 *C after stapling -DETECTOR: 250 *C -COUfW: 90 *C, 3 min; 90 to SHIPMENT: routine 225 *C $ 16'/la1n, hold 6 min SAMPLE STABILITY: at least 4 weeks 25 *C [1] CARRIER GAS: or He, 30 mL/min FIELD BLANKS: 10X (>2) of safeties COUfW: 1.8 m X 2 me 10 silanized glass, 10X Carbowax 20 N 2% KOH on 80/100 mesh ACCURACY Chromosorb WAW RANGE STUOIED: see EVALUATION OF METHOO [1,2] BIAS: not significant [1,2] CALIBRATION: solutions of analyte in 4:1 methanol:water containing 0.12 N HC1 OVERALL PRECISION (sr): 0.056 [2] RANGE: 0.1 to 6 mg per sample [2] {ESTIMATED LOO: 0.005 wq per staple [2] ! '.PRECISION (sr): 0.026 f 0.6 to 2.7 mg per ! staple [2] APPLICABILITY: The working range Is 5 to 300 mg/ma for each ampound in a 20-L air sa^>1e. Water vapor does not significantly affect collection efficiency [3]. Sensitivity may be improved at least ten-fold by using a photoionization or nltrooen-selective detector. INTERFERENCES: None identified [3]. The chroamtographic column or separation conditions may be changed to circuevent interference problems. A 08-5 fused silica capillary coluan may be used._______________________________________________________________________________ _________________ OTHER METHOOS: This revises P6CJW 270 f31, SI40 f4l. and Method 2007 (dated S/15/851, 8/15/87 2007-1 N10SH Manual of Analytical fethods Oo 073840 Co/v/r JFNTTAt AHINOETHAMOL COMPOUNDS HETHOO: 2007 REAGENTS: 1. Eluent: Four parts methanol to one part distilled water (v/v). NOTE: Do not usa deionized water which may contain formaldehyde. 2. Analyte, reagent grade.* 3. Altai Inizing solution: 0.20 N NaOH (8.0 g NaOH/L) In eluent. 4. HC1, cone. (38%, 12 N) (needed for field use).* 5. HC1, 0.12 j(, In eluent. Dissolve 10.0 mL cone. HC1 In eluent to Make 1 L solution. 6. Benzaldehyde. 7. Calibration stock solutions, 10 Mg/M., in 0.12 N MCI in eluent for each analyte. 8. Nitrogen or hellue, purified. 9. Hydrogen, prepurified. 10. Air, filtered. 11. pH paper. 12. KOH, saturated solution. 13. Glass wool. See SPECIAL PRECAUTIONS. EQUIPMENT: 1. Sampler: glass tube, 7-cm long, 8-m 00, 6-bm ID, flame-sealed ends with plastic caps, containing two sections of 4S/60 Mesh chromatographic grade silica gel (front 300 Mg; back ISO Mg) separated by-a-plug of sllylated glass wool. A silylated plug of glass wool is at each end of the tube. Pressure drop across the tube at 0.2 L/min airflow oust be less than 3.2 kPa. Tubes are camaerelally available. Do not use sailing tubes constructed with Metal parts or urethane foa> plugs. Cone. HC1 will react with these Materials. 2. Personal sailing pwp. 0.01 to 0.2 LArin, with flexible connecting tubing. 3. Syringe for dispensing HC1, 50-pL with glass barrel, PTFE-tlpped plunger and inert (platinuM or PTFE) needle (for field use). 4. Gas chranatograph, FID, Integrator and coIimbi (page 2007-1). 5. Coated capillary injection port liner: Soak liner and small quantity of glass wool In saturated KOH. Air-dry liner and glass wool. Loosely pack glass wool in liner. 8. Vials, 2-mL, glass, PTFE-lined criM> caps. 7. VolUMetric flasks, 10-mL. 8. Syringe, 10-pL, readable to 0.1 tiL. 9. Micropipets, 10- to 100-pL. 10. Plpets, 0.5- and 2-mL, with pipet bulb. SPECIAL PRECAUTIONS: The analytes are eye irritants (5). Avoid skin contact or inhalation of cone. HC1. SAMPLING: 1. Calibrate each personal sampling pum with a representative saepler In line. 2. Break the ends of the sampler immediately before sampling. Attach sampler to personal sampling punp with flexible tubing. 3. Sample at an accurately known flaw rate between 0.01 and 0.2 L/Mn for a total saple size of 4 to 24 L. NOTE: If sanples are to be eluted {mediately or will be stored in a freezer for less than 14 days, the following step may be eliminated. 4. Imediately after sampling, stabilize the samples by adding exactly 20 pL cone. NCI to each section of silica gel in each sampler using a syringe. NOTE 1: The amount of NCI added Must be measured carefully because the saeple will be neutralized and made alkaline (step 9) for proper chranatography. NOTE 2: Iron impurities in silica gel will turn yellow upon addition of acid. 5. Cap the samplers. Pack securely for shipment. SAMPLE PREPARATION: 6. Place the first glass wool plug and the front section of the sampler in a vial. second plug and backup section in a separate vial. Place the 8/15/87 2007-2 NI05H Manual of Analytical Methods DO CONF ?384 rOF NT 7 I Al HETHOO: 2007 AMIMOETHANOL COMPOUMS 7. Add 2.0 ii eluant to each vial. Attach cap to each vial. NOTE: If cone. HC1 was not added to the silica geV after sanpling, desorb the samples In 2.0 m 0.12 N HC1 in eluent. The acid increases desorption efficiency. 8. Allow to stand 2 hrs with occasional agitation. 9. Transfer a 0.5-mL aliquot of each sanple to another vial. Add O.S mL alkalinizing solution and attach cap. Nix thoroughly. Check the solution pH with pH paper. If the solution pH is <9 add alkalinizing solution until solution pH Is >9. 10. If 2-ami noethanol Is present, repeat step. 9 with another 0.5-mL aliquot. Add 10 pL benzaldehyde to the basic solution, mix thoroughly and let stand 20 min. NOTE: Benzaldehyde derivatizes 2-ami noethanol to 2-benzylideneaminoethanol which has a higher molecular weight, thereby decreasing the GC detection limit. (Jnderivatized 2-ami noethanol can be determined by this method if the saaple size Is large. CALIBRATION AND QUALITY CONTROL: 11. Calibrate daily with at least five working standards over the range 0.05 to 6 mg of each analyte. a. Add known amounts of analyte or calibration stock solution to 0.12 N HC1 In eluent in 10-mL volunetrlc flasks and dilute to the mark. b. Treat the working standards with base and benzaldehyde as needed (steps 9 and 10). c. Analyze together with sanples and blanks (steps 14 and 15). d. Prepare calibration graph (peak area vs. mg analyte). 12. Determine desorption efficiency (DE) at least once for each lot of silica gel used for sampling. Prepare three tubes at each of five levels plus three media blanks. a. Remove and discard back sorbent section of a media blank sanpler. b. Inject a known amount of analyte or calibration stock solution directly onto front sorbent section with a microliter syringe. c. Add 20.0 pL cone. HC1. d. Cap the tube. Allow to stand overnight. e. Desorb (steps 6 through 10) and analyze with working standards (steps 14 and 15). f. Prepare a graph of DE vs. mg analyte recovered. 13. Analyze three quality control blind spikes and three analyst spikes to ensure that the calibration graph and DE graph are in control. MEASUREMENT: 14. Set gas chromatograph according to manufacturer's recamaendations and to conditions given on page 2007-1. Inject sample aliquot manually using solvent flush technique or with autosampler. NOTE 1: The teeperature program separates all three conpounds. Isothermal colimm conditions are 225, 150, and 90 *C for 2-wlnoethanol, 2-dlbutylamlnoethanol and 2-diethyl ami noethanol, respectively. The colimm packing degrades rapidly at 225 *C; keep operating time at a minimus near this temperature. NOTE 2: If peak area is above the linear range of the working standards, dilute with eluent, reanalyze, and apply the appropriate dilution factor In calculations. NOTE 3: Wien using a capillary colimm system, use the split injection port liner coated with KOH to Improve amine peak shape. 15. Measure peak area. CALCULATIONS: 16. Determine the mass, mg (corrected for DE) of analyte found in the sample front (Wf) and back (%) sorbent sections, and in the average media blank front (Bf) and back (B^) sorbent sections. NOTE: If 1^ > Uf/10, report breakthrough and possible saeple loss. 8/15/87 2007-3 WI05H Manual of Analytical Mthods 00 073R4? CONFTDFNT1AI AHIMOETHANOL COMPOUNDS 17. Calculate concentration, C, of analyte In the air vol we saapled, V (l): (Hf C ** Ef - Bb)*10* mg/m9. V "HWO:,, fP07 EVALUATION OF NETHOO: All three compounds were evaluated under Method PAGAN 270 using a smaller bed of silica gel (front * 150 mg; back * 150 mg) than given above [3]. Desorption efficiencies for 0.1 mg analyte were found to be 0.97 for Z-amlnoethanol, 0.85 for 2-dlethylwlnoethanol, and 0.93 for 2-dlbutylamlnoethanol [3]. Only 2-dlethyl1 noethanol was evaluated under Method $140 using the suggested sorbent tube. In all cases, laboratory testing was performed with spiked samples and generated atmosphere [1,2,6]. All analytes were stable on silica gel up to four weeks when stabilized with acid. Results were: Caioound 2-ami noethanol 2-dibutyl ami noethanol 2-d1ethylami noethanol Method P6CAM 270 [3] P6CAH 270 [3] SI40 [4] Range Studied (mo/Hll.. 30.4 to 63.6 unknown 25 to 113 Sa^>1e size (L) 30 unknown 24 Precision (sr) Measurement Overall <0.070 unknown 0.026 0.057 unknown 0.056 Method $140 [4] was Issued on January 19, 1979, and validated over the range 25 to 113 mg/ta* at 23 *C and 762 sn Hg using 24-L swples [2,7]. Coast Engineering Laboratory 40/60 mesh silica gel was the collecting medtw. Average recovery was 97.11, representing a non-significant bias. The concentration of 2-dlethylanrinoethanol was Independently verified using midget bubblers con taining 15 mL 3 HC1. Desorption efficiency was 0.964 In the range 0.6 to 2.3 mg per sample. Breakthrough (5% on back section) was not achieved after 5,3 hrs when sampling an atmosphere containing 88 mg/m* 2-diethylami noethanol at 0.2 l/mln at 83 relative humidity. REFERENCES: [1] Ubod, G. 0. and J. W. Nlckols. Development of Air-Monitoring Techniques Using Solid Sorbents, October 1, 1976 - Oecesber 31, 1977, Progress Report LA-7295-PR, Los Alamos Scientific Laboratory, Los Alamos, NH, NI0SH IA-77-12 (1978). [2] Backup Data Report No. S140, prepared under NIOSH Contract 210-76-0123 (NIOSH, uigiubllshod, 1979); Report on NIOSH Sequence 45162 (unpublished, April 2, 1986). [3] NIOSH Manual of Analytical Methods, 2nd ed., Vol. 4, PfCAM 270, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 78-175 (1978). [4] Ibid., Vol. 5, $140, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 79-141 (1979). [5] NIOSH/OSHA Occupational Health Guidelines for Chemical Hazards, Dlethylmnlnoethanol and Ethanolwine, U.S. Department of Health and Hunan Services, Publ. (NIOSH) 81-123 (1981), available as GPO Stock 4017-033-00337-8 from Superintendent of Documents, Washington, DC 20402. [6] Wood, G. 0., R. G. Anderson and J. W. Nlckols. Sapling and Analysis of Amlnoethanols In Air, Report LA-UR-77-1398, Industrial Hygiene Group, Los Alamos Scientific Laboratory, Los Alamos, Ifl (1977) (presented at the 1977 American Industrial Hygiene Conference, May 1977, New Orleans, LA). 8/15/87 2007-4 NIOSH Manual of Analytical Methods HO 073843 CONFIDFNTIAi HETHOO: 2007 AHIMOETHANOL COMPOUNDS [7] NIOSH Research Report - Development and Validation of Methods f r Sampling and Analysis of Workplace Toxic Substances, U.S. Department of Health and Human Services, Publ. (NIOSH) 80-133 (1980). HETHOO REVISED BY: Karen J. Williams, NIOSH/DPSE. Table 1. Structural formulas, molecular weights, permissible exposure limits and properties. Compound Formula 2-meinoethanol HOCH2CH2NH2: C^NO m 61,08 2-dibutylamino (C^ytCH^OH; 173.30 ethanol C10H23" 2-diethylamino- (C^J^fCH^OH; 117.19 ethanol c6h,5no mg/ta* - 1 P* NIP OSHA NIOSH* ACGIH BP CC> VP $ 20 *C Density (g/M. 8 20 *C) 2.50 3 ppm 3 ppm (STEL 6 ppm) 171 48 Pa 1.0180 (470 ppm) 7.09 2 ppm 228 * 2 ppm (skin) (STEL 4 ppm) not 0.859 available 4.79 10 ppm 163 10 ppm (skin) 130 Pa 0.8921 (1300 ppm) *No recommended criteria for a standard have been established by NIOSH. 8/15/87 2007-5 NIOSH Manual of Analytical Methods 073844 OONFroeNTlftL