HYDROCARBONS, AROMATIC 1501
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1 HYDROCARBONS, AROMATIC 50 FORMULA: Tble MW: Tble CAS: Tble RTECS: Tble METHOD: 50, Issue EVALUATION: PARTIAL Issue : 5 Februry 984 Issue 2: 5 August 994 OSHA : Tble 2 NIOSH: Tble 2 ACGIH: Tble 2 PROPERTIES: Tble COMPOUNDS: benzene cumene -methylstyrene styrene vinyltoluene (Synonyms p-tert-butyltoluene ethylbenzene nphthlene toluene xylene in Tble ) SAMPLING MEASUREM ENT SAMPLER: FLOW RATE, VOLUME: Tble 3 SHIPMENT: SAMPLE STABILITY: BLANKS: BULK SAMPLE: SOLID SORBENT TUBE (coconut shell chrcol, 00 mg/50 mg) routine not determined 2 to 0 field blnks per set desirble, to 0 ml; ship in seprte continers from smples ACCURACY RANGE STUDIED: Tble 3 BIAS: Tble 3 OVERALL PRECISION ( rt ): Tble 3 TECHNIQUE: ANALYTE: DESORPTION: INJECTION VOLUME: GAS CH RO MATOGRA PH Y, FID hydrocrbons listed bove ml CS 2 ; stnd 30 min 5 L TEM PERATURE-INJECTION: 225 C -DETECTOR: 225 C -COLUMN: see step CARRIER GAS: COLUMN: CALIBRATION: N2 or H e, 25 ml/min glss, 3.0 m x 2-mm, 0% OV-275 on 00/20 mesh Chromosorb W -AW or equivlent (Tble 4) nlytes in CS2 RANGE AND PRECISION ( r ): Tble 4 ESTIMATED LOD: 0.00 to 0.0 mg per smple with cpillry colomn [] ACCURACY: Tble 3 APPLICABILITY: This m ethod is for pek, ceiling nd TW A determintions of romtic hydrocrbons. It my be used for simultnious mesurements, though there is the possibiltity tht interctions between nlytes my reduce the brekthrough volumes INTERFERENCES: Use of the recommended column will prevent interference by lknes ( C 0 ). U nder conditions of high humidity, the brekthrough volumes my be reduced by s much s 50%. Other voltile orgnic solvents, e.g., lcohols, ketones, ethers, nd hlogented hydrocrbons, re possible interferences. If interference is suspected, use less polr column or chnge column temperture. OTHER METHODS: This m ethod is bsed on nd supercedes Methods P&CA M 27, benzene, styrene, toluene nd xylene [2]; S3, benzene [4]; S22, p-tert-butyltoluene [3]; S23, cumene [3]; S29, ethylbenzene [3]; S26, -methylstyrene [3]; S292, nphthlene [4]; S30, styrene [3]; S343, toluene [4]; S25, vinyltoluene [3]; S38, xylene [4]
2 HYDROCARBONS, AROMATIC: METHOD 50, Issue 2, dted 5 August Pge of 2 of 7 REAGENTS:. Eluent: Crbon disulfide*, chromtogrphic qulity contining (optionl) suitble internl stndrd. 2. Anlytes, regent grde.* 3. Nitrogen or helium, purified. 4. Hydrogen, prepurified. 5. Air, filtered. 6. Nphthlene colibrtion stock solution, 0.40 g/ml in CS 2. * See SPECIAL PRECAUTIONS EQUIPMENT:. Smpler: glss tube, 7 cm long, 6-mm OD, 4-mm ID, flme-seled ends, contining two sections of ctivted (600 C) coconut shell chrcol (front = 00 mg, bck = 50 mg) seprted by 2- mm urethne fom plug. A silylted glss wool plug precedes the front section nd 3-mm urethne fom plug follows the section. Pressure drop cross the tube L/ min irflow must be less thn 3.4 kp. Tubes re commercilly vilble. 2. Personl smpling pumps, 0.0 to L/min (Tble 3), with flexible connection tubing. 3. Gs chromtogrph, FID, integrtor, nd column (pge 50-). 4. Vils, glss, -ml, with PTFE-lined cps. 5. Pipet, -ml, nd pipet bulb. 6. Syringes, 5-, 0-, 25- nd 00 L. 7. Volumetric flsks, 0-mL SPECIAL PRECAUTIONS: Crbon disulfide is toxic nd extremely flmmble (flsh point = -30 C); benzene is suspect crcinogen. Prepre smples nd stndrds in well-ventilted hood. SAMPLING:. Clibrte ech personl smpling pump with representtive smpler in line. 2. Brek the ends of the smpler immeditely before smpling. Attch smpler to personl smpling pump with flexible tubing. 3. Smple t n ccurtely known flow rte between 0.0 nd 0.2 L/min (to L/min for nphthlene or styrene) for totl smple size s shown in Tble Cp the smplers with plstic (not rubber) cps nd pck securely for shipment. SAMPLE PREPARATION: 5. Plce the front nd bck sorbent sections of the smpler tube in seprte vils. Discrd the glss wool nd fom plugs. 6. Add.0 ml eluent to ech vil. Attch crimp cp to ech vil immeditely. 7. Allow to stnd t lest 30 min with occsionl gittion. CALIBRATION AND QUALITY CONTROL: 8. Clibrte dily with t lest six working stndrds over the pproprite rnge (c. 0.0 to 0 mg nlyte per smple; see Tble 4).. Add known mounts of nlyte (clibrtion stock solution for nphthlene) to eluent in 0-mL volumetric flsks nd dilute to the mrk. b. Anlyze together with smples nd blnks (steps through 3). c. Prepre clibrtion grph (pek re of nlyte vs. mg nlyte per smple).
3 HYDROCARBONS, AROMATIC: METHOD 50, Issue 2, dted 5 August Pge of 3 of 7 9. Determine desorption efficiency (DE) t lest once for ech btch of chrcol used for smpling in the clibrtion rnge (step 8). Prepre three tubes t ech of five levels plus three medi blnks.. Remove nd discrd bck sorbent section of medi blnk smpler. b. Inject known mount of nlyte (clibrtion stock solution for nphthlene) directly onto front sorbent section with microliter syringe. c. Cp the tube. Allow to stnd overnight. d. Desorb (steps 5 through 7) nd nlyze together with working stndrds (steps through 3). e. Prepre grph of DE vs. mg nlyte recovered. 0. Anlyze three qulity control blind spikes nd three nlyst spikes to insure tht the clibrtion grph nd DE grph re in control. MEASUREMENT:. Set gs chromtogrph ccording to mnufcturer's recommendtions nd to conditions given on pge 50-. Select pproprite column temperture: Approximte Retention Time (min), t Indicted Column Temperture Substnce 50 C 00 C 50 C Progrmmed b benzene toluene xylene (pr) ethylbenzene xylene (met) cumene xylene (ortho) styrene methylstyrene vinyltoluene (met) nphthlene Dt not vilble for p-tert-butyltoluene nd p-vinyltoluene. b Temperture progrm: 50 C for 3 min, then 5 C/min to 200 C. NOTE:Alterntively, column nd temperture my be tken from Tble Inject smple liquot mnully using solvent flush technique or with utosmpler. NOTE:If pek re is bove the liner rnge of the working stndrds, dilute with eluent, renlyze nd pply the pproprite dilution fctor in clcultions. 3. Mesure pek re. CALCULATIONS: 4. Determine the mss, mg (corrected for DE) of nlyte found in the smple front (W f )nd bck (W b ) sorbent sections, nd in the verge medi blnk front (B f ) nd bck (B b ) sorbent sections. NOTE: IF W b > W f / 0, report brekthrough nd possible smple loss. 5. Clculte concentrtion, C, of nlyte in the ir volume smpled, V (L):
4 HYDROCARBONS, AROMATIC: METHOD 50, Issue 2, dted 5 August Pge of 4 of 7 EVALUATION OF METHOD: Precisions nd bises listed in Tble 3 were determined by nlyzing generted tmospheres contining one-hlf, one, nd two times the OSHA stndrd. Generted concentrtions were independently verified. Brekthrough cpcities were determined in dry ir. Storge stbility ws not ssessed. Mesurement precisions given in Tble 4 were determined by spiking smpling medi with mounts corresponding to one-hlf, one, nd two times the OSHA stndrd for nominl ir volumes. Desorption efficiencies for spiked smplers contining only one compound exceeded 75%. Reference [9] provides more specific informtion. REFERENCES: [] User check, UBTL, NIOSH Sequence #42-S (unpublished, December 7, 983). [2] NIOSH Mnul of Anlyticl Methods, 2nd. ed., V., P&CAM 27, U.S. Deprtment of Helth, Eduction, nd Welfre, Publ. (NIOSH) A (977). [3] Ibid, V. 2, S22, S23, S25, S26, S29, S30, U.S. Deprtment of Helth, Eduction, nd Welfre, Publ. (NIOSH) B (977). [4] Ibid, V. 3, S292, S3, S38, S343, U.S. Deprtment of Helth, Eduction, nd Welfre, Publ. (NIOSH) C (977). [5] R. D. Dreisbch. "Physicl Properties of Chemicl Compounds"; Advnces in Chemistry Series, No. 5; Americn Chemicl Society, Wshington (955). [6] Code of Federl Regultions; Title 29 (Lbor), Prts 900 to 90; U.S. Government Printing Office, Wshington (989); 29 CFR [7] NIOSH Recommendtions for Occuptionl Sfety nd Helth. U.S. Deprtment of Helth nd Humn Services. DHHS (NIOSH) Publicvtion No (992). [8] Threshold Limit Vlues for Chemicl Substnces nd Physicl Agents nd Biologicl Exposure Indices, ACGIH, Cincinnti, OH (992). [9] Documenttion of the NIOSH Vlidtion Tests, S22, S23, S25, S26, S29, S30, S292, S3, S38, S343, U.S. Deprtment of Helth, Eduction, nd Welfre; Publ. (NIOSH) (977). METHOD WRITTEN (REVISED) BY: R. Aln Lunsford, Ph.D., bsed on results of NIOSH Contrct CDC
5 HYDROCARBONS, AROMATIC: METHOD 50, Issue 2, dted 5 August Pge of 5 of 7 TABLE. SYNONYMS, FORMULA, MOLECULAR WEIGHT, PROPERTIES [5]. Molec- Boiling Vpor Pressure Density Empiricl ulr C Nme/Synonyms Formul W eight ( C) (mm Hg) (kp) (g/ml) benzene C 6 H CAS # RTECS CY p-tert-butyltoluene C H CAS # tert-butyl-4-methylbenzene RTECS XS cumene C 9 H CAS # isopropylbenzene RTECS GR ethylbenzene C 8 H CAS # RTECS DA methylstyrene C 9 H CAS # isopropenylbenzene (-methylethenyl)-benzene RTECS W L nphthlene C 0 H CAS # RTECS QJ styrene C 8 H CAS # vinylbenzene RTECS W L toluene C 7 H CAS # methylbenzene RTECS XS vinyltoluene b C 9 H CAS # (met) methylstyrene (p-vinyltoluene) (pr) methylvinylbenzene (ortho) RTECS W L xylene c C 8 H CAS # (ortho) dimethylbenzene (p-xylene) (met) RTECS ZE (pr) Melting point. b Commercil mixture of met nd pr isomers. c Mixture of isomers.
6 HYDROCARBONS, AROMATIC: METHOD 50, Issue 2, dted 5 August Pge of 6 of 7 TABLE 2. PERMISSIBLE EXPOSURE LIMITS, PPM [6-8]. OSHA NIOSH ACGIH mg/m 3 Substnce TWA TWA C STEL TLV STEL per ppm benzene 0. c 0 f 3.9 p-tert-butyltoluene cumene 50 (skin) 50 (skin) 50 (skin) 4.9 ethylbenzene methylstyrene nphthlene 0 0 d styrene ** 00 (skin) 4.26 toluene (skin) 3.77 vinyltoluene xylene e Mximum durtion 0 min in 8 h. b Mximum durtion 5 min in ny 3 h. c Potentil crcinogen d Group III Pesticide e Group I Pesticide f Suspect crcinogen TABLE 3. SAMPLING FLOWRATE, VOLUME, CAPACITY, RANGE, OVERALL BIAS AND PRECISION [3,4,9]. Substnce Smpling Flowrte Volume b (L) (L/min) MIN MAX Brekthrough Concentrtion (L) (mg/m 3 ) Rnge t VO L-MIN (mg/m 3 ) Overll Bis Precision (%) ( rt ) Accurcy (±%) benzene p-tert-butyltoluene cumene ethylbenzene -methylstyrene nphthlene e styrene toluene vinyltoluene xylene >45 44 >45 35 >45 > d d 0.06 d d d Minimum recommended flow is 0.0 L/min. b VMin = minimum smple OSHA TW A; V Mx = mximum smple OSHA TW A c 0-m in smple. d Corrected vlue, clculted from dt in Reference 9. e Nphthlene shows poor desorption efficiency t low loding; 00-L minimum volume is recommended. f 5-m in smple. g 5-min smple.
7 HYDROCARBONS, AROMATIC: METHOD 50, Issue 2, dted 5 August Pge of 7 of 7 TABLE 4. MEASUREM ENT RANGE, PRECISION AND CONDITIONS [3,4,9]. Desorption Mesurement Crrier Column Prmeters b Volume Rnge Precision Flow t Length Substnce (ml) (mg) ( r ) (ml/min) ( C) (m) Pcking c benzene A p-tert-butyltoluene d B cumene B ethylbenzene B -methylstyrene B nphthlene C styrene d B toluene D vinyltoluene B xylene D Injection volume, 5.0 µl; nitrogen crrier gs. b All columns stinless steel, 3.2-mm outside dimeter. c A, 50/80 mesh Porpk P; B, 0% FFAP on 80/00 mesh Chromosorb W AW -DMCS; C, 0% OV-0 on 00/20 mesh Supelcoport; D, 50/80 mesh Porpk Q. d Corrected vlue, clculted from dt in [9].
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