WST 243-2004 职业接触正己烷生物限值.pdf

WS/T243-2004附.录A(规范性附录)尿2,5-己二酮的测定A.1原理尿中的2,5-己二酮在酸性条件下水解后，用乙醚萃取、FAP柱分离，气相色谱氢火焰离子化检测器测定，以保留时间定性，峰面积（或峰高）定量。A.2仪器A.2.1气相色谱仪：氢火焰离子化检测器。A.2.2具塞比色管：10mL,5mL。A.2.3水浴箱。A.3试剂乙醚、盐酸（分析纯），FFAP固定液：Chromosorbw AW DMCS(80100目)，2,5-己二酮标准贮备液：于10.0mL容量瓶中，加入5mL蒸馏水，然后准确加入0.0160mL2,5-己二酮(20时，1mL2,5-己二酮质量0.974g),用蒸馏水稀释至刻度，此贮备液每毫升含2,5-己二酮1.56mg。临用前准确吸取贮备液0.64mL到10mL的容量瓶中，加蒸馏水至刻度，摇匀（此液1mL含1004g的2,5己二酮），作为应用液。A.4采样、运输和保存用干净的玻璃瓶采集班后尿50mL,测其比重后，加盐酸0.25mL,尽快送回实验室分析。此尿样于4可保存5d,一8可保存1个月。A.5分析步骤A.5.1色谱条件：色谱柱为长1.6m、内径4mm的玻璃柱，内装FFAP:Chromosorbw AW DMCS=15：100,柱温165，检测室温度230，汽化室温度230，载气(N2)50mL/min。A.5.2样品处理：准确吸取2.0mL尿样于具塞比色管中，加人2滴盐酸，摇匀，于90100水浴中恒温40mi,取出放至室温后，加2mL乙醚萃取，静置分层。若乙醚损失应补加至原体积2mL。A.5.3工作曲线的制备：采集未接触正己烷者的尿，用2,5-己二酮贮备液分别配成5.0、10.0、15.0、20.0、30.0ug/mL的标准系列，然后各取2.0mL,同样品处理。取各种浓度的萃取液分别进样1L,作气相色谱分析。以2,5-己二酮的含量对峰面积作图，绘制工作曲线。A.5.4样品测定：取已处理的样品乙醚液1L进样分析。A6计算根据测得的峰面积从工作曲线中查出含量(g/mL),按式(A.1)计算尿中2,5-己二酮的浓度：1.020-1.000c=m尿样比重-1.000式中：c一尿中2,5-己二酮的浓度，单位为毫克每升(mg/L)；m一由工作曲线上查出的2,5-己二酮的含量，单位为徽克每升(4g/mL):1.020标准比重。2,5-己二酮换算系数为1mg/L=8.764mol/L。2WS/T243-2004n-hexane.Int Arch Occup Environ Health,1982,50(3):219-22324Raitta C Seppalainen AN,Huuskonen MS.N-hexane maculopathy in industrial workers.Albrecht Von Graefes Arch Klin Exp Opthalmol,1978,209(2):99-10125Sanagi S,Seki Y,Sugimoto K,et al.Peripheral nervous system functions of workers ex-posed to n-hexane at a low level.Int Arch Occup Environ Health,1980,47(1):69-7026Sax N1,Lewis RJ.Hawleys Condensed Chemical Dictionary.7th ed.New York:Van Nos-trand Company,NY,1987:600.27Scelsi R,Poggi P,Fera L,et al.Industrial neuropathy due to n-hexane.Clinical and mor-phological findings in three cases.Clin Toxicol,1981,18(12):138728Schaumburg HH,Spencer P S.Degeneration in xentral and peripheral nervous systemspriduced by pure n-hexane:an experimental study.Brain,1975,99:18329Sobue I,Yamamura Y.N-Hexane polyneuropathy.Outbreak among vinyl sandal manufac-turers.Rinsho Shinkei,1968,8:39330Spencer P.Neuropathic potential of n-hexane in the presence of other hexane isomers,Washington,DC,American Petroleum Institute(API Medical Research Publication No.30-30226).198231Takeuchi Y.N-hexane polyneuropathy in Japan:a review of n-hexane poisoning and itspreventive measures.Environ Res,1993,62(1):76-7832Takeuchi Y,Ono Y,Hisanagn N et al.A comparative study on the neurotoxicity of n-pen-tane,n-hexane and n-heptane in the rat.Br J Ind Med,1980,37(3):241-24433Van Engelen JG,Rebel de Haan W,Opdam JJ,et al.Effects of co-exposure to methylethylketong(MEK)on n-hexane toxicokinetics in human vlunteers.Toxicol Appl Pharmacol.1997,144(2):385-38734WHO.n-Hexane,Environmental Health Criteria 122,Geneva:WHO,199135Yokoyama K,Feldman RG,Sax DS.Relatioa of distribution of conduction velocities tonerve biopsy findings in n-hexane poisoning.Mucle Nerve,1990,13(4):314-31536Yuasa J,Kishi R,Eguchi T,et al.Investigaticn on neurotoxicity of occupational exposureto cyclohexane:a neurophysiological study.Occup nviron Med,1996,53(3):174-176行业标准信总服务平5