Alcohols Combined 1405

<ul style="display: flex;"><li style="flex:1">ALCOHOLS COMBINED </li><li style="flex:1">1405 </li></ul><ul style="display: flex;"><li style="flex:1">Formulas: Table 1 </li><li style="flex:1">MW: Table 1 </li><li style="flex:1">CAS: Table 2 </li><li style="flex:1">RTECS: Table 2 </li></ul><ul style="display: flex;"><li style="flex:1">METHOD: 1405, Issue 1 </li><li style="flex:1">EVALUATION: PARTIAL </li><li style="flex:1">Issue 1: 15 March 2003 </li></ul>OSHA : Table 2 NIOSH: Table 2 ACGIH: Table 2 PROPERTIES: Table 1 COMPOUNDS: (1) n-butyl alcohol (2) sec-butyl alcohol (3) isobutyl alcohol (4) n-propyl alcohol (5) allyl alcohol (6) diacetone alcohol (7) cyclohexanol (8) isoamyl alcohol (9) methyl isobutyl carbinol SYNONYMS: See Table 3. <ul style="display: flex;"><li style="flex:1">SAMPLING </li><li style="flex:1">MEASUREMENT </li></ul>SAMPLER: SOLID SORBENT TUBE (Coconut shell charcoal, 100 mg/50 mg) TECHNIQUE: ANALYTE: GAS CHROMATOGRAPHY, FID Compounds above FLOW RATE: 0.01 to 0.2 L/min DESORPTION: 1 mL 5% 2-propanol in CS2 Compounds: (1-3 ) (4-9) 1 L INJECTION VOLUME: VOL-MIN: -MAX: 2 L <ul style="display: flex;"><li style="flex:1">1 µL </li><li style="flex:1">10 L </li><li style="flex:1">10 L </li></ul>SHIPMENT: Routine TEMPERATURE -INJECTION: 220 °C -DETECTOR: 250 - 300 °C SAMPLE STABILITY: See Evaluation of Method. -COLUMN: 35 °C (7 minutes), to 60 °C at 5 °C/minute, hold 5 minutes, up to 120 °C at 10 °C /minute, hold 3 minutes. BLANKS: 2 to 10 field blanks per set CARRIER GAS: COLUMN: He, 4 mL/min ACCURACY Capillary, fused silica, 30 m x 0.32-mm ID; 0.5 µm film polyethylene glycol, DB- wax or equivalent RANGE STUDIED: Not studied [1, 2]. BIAS: Not determined CALIBRATION: RANGE: Solutions of analyte in eluent (internal standard optional) OVERALL PRECISION (ÖrT): Not determined See EVALUATION OF METHOD. ACCURACY: Not determined ESTIMATED LOD: 1 µg each analyte per sample PRECISION: See EVALUATION OF METHOD. APPLICABILITY: This method may be used to determine two or more of the specified analytes simultaneously. INTERFERENCES: High humidity reduces sampling capacity. Less volatile compounds may displace more volatile compounds on the charcoal. OTHER METHODS: This method combines and updates Methods 1401 and 1402, NMAM, Fourth Edition, Issue 2. Estimated LOD for each analyte is approximately ten times lower than that of the old methods. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 2 o f 6 <ul style="display: flex;"><li style="flex:1">EQUIPMENT: </li><li style="flex:1">REAGENTS: </li></ul>1. S a m ple r: Gla s s tube , 7-cm long, 6-mm OD, 4- mm ID, fla me -s e a le d e nds, containing two se ctio ns of a ctivate d (6 00 °C) coc on ut s he ll cha rcoa l (front - 100 mg; ba ck - 50 mg) s e pa ra te d by a 2-mm ure tha ne foa m plug follows the ba ck s e ction. P re s s ure drop a cros s the tube at 1 L/min a irflow mus t be le s s tha n 3.4 kPa . Tub es are com m ercia lly a va ila ble . 2. P e rs ona l s a mpling pump, 0.01 to 0.2 L/min, with fle xible conne cting tubing. 3. Ga s chroma togra ph, FID, inte gra tor a nd colum n (pa ge 14 05-1). 1. Ca rbon disulfide, ch rom atog raph ic gra de.* 2. 2-P ropa nol, ch rom atog raph ic gra de.* 3. He xan e, ch rom atog raph ic gra de.* 4. He ptan e, ch rom atog raph ic gra de.* 5. De s orbing s olution: Ca rbon dis ulfide with 5% (v/v) 2-propa nol a nd 0.05% (v/v) he xa ne a s a n inte rna l s ta nda rd. NOTE: n-Unde ca ne , 0.1 (v/v) or othe r s uita ble s ta nda rd ca n be us e d. 6. Ana lyte (s ). 7. S tock s olution, 100 mg/mL. P re pa re s olutions of e a ch a na lyte in he pta ne . 8. Nitroge n, purifie d. 4. Via ls , gla s s , 2-mL, P TFE -line d crimp ca ps . 5. S yringe , 10-µL, rea da ble to 0.1 µL. 6. Volume tric fla s ks , 2 mL. 9. Hydroge n, pre purifie d. 10. Air, compre s s e d, filte re d. * Se e SP ECIAL P RECAUTIONS SPECIAL PRECAUTIONS: Ca rbon dis ulfide is toxic a nd a n a cute fire a nd e xplos ion ha za rd (fla s h point = -30 °C); a ll work with it mus t be done in a hood. P ropa nol, he xa ne , a nd he pta ne a re fla mm a ble . Ana lyte s s hould be ha n dle d in a fume hood. W e a r glove s , s a fe ty gla s s e s , a nd a pp ropria te prote ctive clothing. SAMPLING: 1. Ca libra te e a ch pe rs ona l s a mpling pump with a re pre s e nta tive s a mple r in line . 2. Bre a k the e nds of the s a mple r imm e dia te ly be fore s a mpling. Atta ch s a mple r to pe rs ona l s a mpling pump with fle xible tubing. 3. Sa m ple at a n ac curately kn own flow ra te be twee n 0.0 1 an d 0.2 L/m in for a total sa m ple size of 1 to 10 L (2 to 10 L for n-buta n ol, s e c-buta nol, a nd is obutyl a lcohol). 4. Ca p the sam plers with pla stic (not rub ber) cap s an d pa ck sec urely for shipm ent. SAMPLE PREPARATION: 5. P la ce the front a nd ba ck s orbe nt s e ctions of the s a mple r tube in s e pa ra te via ls . Dis ca rd the gla s s wool a nd foa m plugs . 6. Ad d 1.0 m L des orbing s olution (DS) to e ac h vial. Attac h crim p cap to e ac h vial. 7. Allow to s ta nd 30 min with occa s iona l agita tion. CALIBRATION AND QUALITY CONTROL: 8. Ca libra te da ily with a t le a s t s ix working s ta nda rds covering the ra nge of s a mple s . a . Add known am oun ts of a nalyte to DS in 2-m L volum etric flas ks and dilute to th e m ark. b. Ana lyze toge the r with s a mp le s a nd bla nks (s te ps 11 a nd 12). c. P re pa re ca libra tion graph (ra tio of pe a k a rea of ana lyte to pe a k a re a of inte rna l s tanda rd vs . µg a na lyte . 9. Dete rm ine de so rption efficie nc y (DE) at le as t on ce for ea ch ba tch of c ha rcoa l us ed for sa m pling in the ca libra tion ra nge (s te p 8). P repa re thre e tube s a t e ach of five le ve ls plus tre e me dia bla nks . a . Re m ove a nd dis ca rd ba ck s orbe nt s e c tion of a me d ia bla nk s a m ple r. b. Inje ct a known a mount of s tock s olution dire ctly onto front s orbe nt s e ction with a microlite r s yringe . NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 3 o f 6 c. Ca p the tube . Allow to stan d overnig ht. d. De s o rb (s te ps 5 through 7 ) a nd a na lyze toge the r with working s ta nda rds (s te ps 11 a nd 12). e . P re pa re a gra ph of DE vs . µg a na lyte re cove re d. 10. Ana lyze thre e qua lity control bind s pike s a nd thre e a na lys t s pike s to ins ure tha t the ca libra tion gra ph an d DE g ra ph are in con trol. MEASUREMENT: 11. S e t ga s chroma togra ph a ccording to ma nufa cture r’s re comm e nda tions a nd to conditions give n on pag e 14 05-1 . Inject s am ple aliqu ot m anu ally using solve nt flus h tec hnique o r with a utos am pler. NOTE: If pea k a rea is abo ve the linear ra nge of the working stan dard s, dilute with elue nt, re a na lyze , a nd a pply the a ppropria te dilution fa ctor in calcula tions . 12. Me a s ure pe a k a re a . Divide the pea k a re a of a na lyte by the pe a k a re a of inte rna l s ta nda rd on the s a me chrom a togra m. CALCULATIONS: 13. De te rm ine the ma s s , µg (corre c te d for DE) of a n a lyte found in the s a m ple front (Wf) a nd ba ck (W b) s orbe nt s e c tions a nd in the a ve ra ge m e dia bla nk front (Bf) a nd (Bb) sorben t sec tions. NO TE: If W b > Wf/10, re port bre a kthrough a nd pos s ible s a mple los s . 14. Ca lcula te conce ntra tion, C, of a na lyte in the a ir volume s a m ple d, V (L): NO TE : :g/L = m g/m 3 EVALUATION OF METHOD: P re vious Eva lua tions [2] This me thod, NIOS H 1405, combine s a nd upda te s NIOS H Me thods 1401 a nd 1402. Me thods 1401 a n 1402 we re ba s e d on the 2nd e dition NMAM Me thods S 66 (n-butyl a lcohol), S 53 (s e c-butyl a lcohol), S 64 (is obutyl a lcohol), S 62 (n-propyl a lcohol), S 52 (a llyl a lcohol), S 55 (dia ce tone a lcohol), S 54 (cyclohe xa n ol), S 58 (is oa myl a ocohol), a nd S 60 (me thyl is obutyl ca rbinol) which we re is s ue d on J a nua ry 17, 1975 [3] a nd va lida ted us ing 10-L air s am ple s of atm os ph eres ge ne ra ted by injec tion of the pure alcoh ol into d ry air us ing a ca libra te d s yringe drive [1]. No s tora ge s ta bility s tudie s we re pe rforme d. Ove ra ll pre cis ion a nd re cove rie s a re s hown Ta ble 4, re pre s e nting non-s ignifica nt bia s in e a ch me thod. <ul style="display: flex;"><li style="flex:1">Curre nt Eva lua tion </li><li style="flex:1">[4] </li></ul>Meth od s for alcoh ols (n-bu tyl alc oh ol, s ec -butyl a lco ho l, iso bu tyl alc oh ol, n -propyl a lco ho l, allyl a lco ho l, dia ce tone a lcohol, cyclohe xa nol, is oa myl a lcohol) we re e va lua te d us ing a na lyte s fortifie d on Ana s orb CS C s orbe nt tube s (Lot #2000). Ta ble 5 lis ts the de s orption e fficie ncy (DE) a nd pre cis ion for the compounds te s te d in the e va lua tion. S tora ge s ta bility s tudie s we re pe rforme d a t two differe nt conce ntra tion le ve ls : one a t a pproxima te ly 10 µg e a ch a na lyte /s a mple for the low le ve l, a nd the othe r a t a pproxima te ly 150 µg e a ch a na lyte /s a mple for the high le ve l. The sa m ple s were s tored for 7, 1 4, 2 1, a nd 30 da ys a t 5 °C. The res ults are sum m arized in Ta ble 5. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 4 o f 6 REFERENCES: [1] NIOS H [1977]. Docum e nta tion of the NIOS H Va lida tion Te s ts . Cincinna ti, OH: U.S . De pa rtme nt of He a lth, Educa tion, a nd We lfa re , P ubl. (NIOS H) 77-185. [2] NIOS H [1994]. Me thods 1401 a nd 1402. In: Elle r P M, Ca s s ine lli ME, e ds . NIOS H Ma nua l of Analytical Metho ds, 4 th e d. Cincinna ti, OH: Na tiona l Ins titute for Occupa tiona l S a fe ty a nd He a lth, DHHS (NIOS H) P ublica tion No. 94-113. [3] Ta ylor DG , eds [197 7]. NIO SH Ma nua l of An alytical Metho ds, 2 nd e d., V.2., Cincinna ti, OH: U.S . De pa rtme nt of He alth, Educa tion, and We lfa re . DHHS (NIOS H) P ublication No. 77-157-B. [4] Yoon YH, P e rkins J B, Re ynolds J M [2002]. Ba ck-up Da ta Re port for Alcohols Combine d. Da ta Che m La bora torie s , Inc. unde r NIO S H c ontra cts CDC-200 -95-2955 a nd CDC 200 -2001-080 00 (Augu s t). METHOD WRITTEN BY: Yound He e Yoon, P h.D. a nd J a me s B. P e rkins , Da ta Che m La bora torie s , Inc., S a lt La ke City, Uta h. TABLE 1. PROPERTIES VP @ 20°C, kPa mg/m3 = 1 ppm @ NTP Density (g/mL) BP <ul style="display: flex;"><li style="flex:1">(°C) </li><li style="flex:1">(mm Hg) </li></ul>Compound n-Butyl alcohol <ul style="display: flex;"><li style="flex:1">Formula </li><li style="flex:1">M.W. </li></ul>CH3 CH2 CH2 CH2 OH; C4 H1 0 O 3.03 3.03 3.03 2.46 2.37 4.75 4.09 3.60 4.18 <ul style="display: flex;"><li style="flex:1">74.12 </li><li style="flex:1">0.810 </li></ul>@ 20 °C 117 99.5 108 0.56 (4.2) 1.7 (13) 1.2 (9) sec-Butyl alcohol Isobutyl alcohol n-Propyl alcohol Allyl alcohol CH3 CH(OH)CH2 CH3 ; C4 H1 0 O 74.12 74.12 60.09 58.08 116.16 100.16 88.15 102.18 0.808 @ 20 °C (CH3 )2 CHCH2 OH; C4 H1 0 O 0.806 @ 15 °C CH3 CH2 CH2 OH; C3 H8 O 0.805 @ 20 °C <ul style="display: flex;"><li style="flex:1">97 </li><li style="flex:1">2.0 (15) </li></ul>2.3 (17) 0.1 (0.8) 0.13 (1.0) 3.7 (28) 0.4 (3) CH2 =CHCH2 OH; C3 H6 O2 <ul style="display: flex;"><li style="flex:1">0.854 </li><li style="flex:1">96-97 </li></ul><ul style="display: flex;"><li style="flex:1">167.9 </li><li style="flex:1">0.931 </li></ul>@ 25 °C Diacetone alcohol Cyclohexanol (CH3 )2 C(OH)CH2 COCH3 ; C6 H1 2 O2 C6 H1 2 O <ul style="display: flex;"><li style="flex:1">0.962 </li><li style="flex:1">161: </li></ul>MP=24 Isoamyl alcohol Methyl isobutyl carbinol (CH3 )2 CHCH2 CH2 OH; C5 H1 2 O 0.813 @ 15 °C 132 <ul style="display: flex;"><li style="flex:1">132 </li><li style="flex:1">(CH3 )2 CHCH2 CH(OH)CH3 ; </li></ul>C6 H1 4 O 0.802 NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 5 o f 6 TABLE 2. GENERAL INFORMATION Exposure Limits <ul style="display: flex;"><li style="flex:1">Compound </li><li style="flex:1">CAS # </li><li style="flex:1">RETECS # </li><li style="flex:1">OSHA </li></ul>(ppm) NIOSH (ppm) ACGIH (ppm) <ul style="display: flex;"><li style="flex:1">n-Butyl alcohol </li><li style="flex:1">71-36-3 </li></ul>78-92-2 EO1400000 EO1750000 100 TWA 150 TWA <ul style="display: flex;"><li style="flex:1">C 50 (skin) </li><li style="flex:1">C 50 (skin) </li></ul><ul style="display: flex;"><li style="flex:1">100 TWA </li><li style="flex:1">sec-Butyl alcohol </li><li style="flex:1">100 TWA; </li></ul>150 STEL Isobutyl alcohol n-Propyl alcohol 78-83-1 71-23-8 NP9625000 UH8225000 100 TWA 200 TWA <ul style="display: flex;"><li style="flex:1">50 TWA </li><li style="flex:1">50 TWA </li></ul><ul style="display: flex;"><li style="flex:1">200 TWA; </li><li style="flex:1">200 TWA; </li></ul><ul style="display: flex;"><li style="flex:1">250 STEL(skin) </li><li style="flex:1">250 STEL (skin) </li></ul><ul style="display: flex;"><li style="flex:1">Allyl alcohol </li><li style="flex:1">107-18-6 </li><li style="flex:1">BA5075000 </li><li style="flex:1">2 TWA; (skin) </li><li style="flex:1">2 TWA; </li><li style="flex:1">2 TWA; </li></ul><ul style="display: flex;"><li style="flex:1">4 STEL (skin) </li><li style="flex:1">4 STEL (skin) </li></ul>(Group 1 Pesticide) Diacetone alcohol Cyclohexanol 123-42-2 108-93-0 123-51-3 SA9100000 GV7875000 EL5425000 50 TWA 50 TWA 100 TWA <ul style="display: flex;"><li style="flex:1">50 TWA </li><li style="flex:1">50 TWA </li></ul><ul style="display: flex;"><li style="flex:1">50 TWA (skin) </li><li style="flex:1">50 TWA (skin) </li></ul><ul style="display: flex;"><li style="flex:1">Isoamyl alcohol </li><li style="flex:1">100 TWA; </li></ul>125 STEL(skin) 100 TWA; 125 STEL <ul style="display: flex;"><li style="flex:1">Methyl isobutyl carbinol </li><li style="flex:1">108-11-2 </li><li style="flex:1">SA7350000 </li><li style="flex:1">25 TWA; (skin) </li><li style="flex:1">25 TWA; </li><li style="flex:1">25 TWA; </li></ul><ul style="display: flex;"><li style="flex:1">40 STEL (skin) </li><li style="flex:1">40 STEL (skin) </li></ul>TABLE 3. SYNONYMS Compound (1) n-butyl a lcohol (2) s e c-Butyl a lcohol (3) is obutyl a lcohol (4) n-propyl a lcohol (5) a llyl a lcohol Synonyms 1-bu tan ol; n -buta no l; prop yl ca rbinol. 2-buta nol; me thyl e thyl ca rbinol; 2-hydroxybuta ne . 2-me thyl-1-propa nol; is opropyl ca rbinol; IBA. 1-prop an ol; e thyl c arbinol. 2-prop en -1-ol; 2-prop en ol; vinyl carbinol. (6) dia ce tone a lcohol (7) cyclohe xa nol 4-hydroxy-4-me thyl-2-pe nta none ; 2-me thyl-2-pe nta nol-4-one . he xa lin; h ydralin; hyd roxyc yclo he na ne ; an ol. <ul style="display: flex;"><li style="flex:1">(8) is oa myl a lcohol </li><li style="flex:1">3-m eth yl-1-buta no l; iso bu tylca rbinol; iso pe ntyl a lco ho l. </li></ul><ul style="display: flex;"><li style="flex:1">MIBC ; 4-m eth yl-2-pen tan ol; m eth yl am yl alcoh ol. </li><li style="flex:1">(9) me thyl is obutyl ca rbinol </li></ul>

Alcohols Combined 1405

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