土壤和沉积物挥发性有机物的测定吹扫捕集气相色谱

方法验证报告方法名称：土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法HJ605-2011方法编号： HJ605-2011 分析项目： 挥发性有机物编制人：日期：审核人：日期：批改人： 日期：《土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法

HJ605-201O方法验证一、 人员本实验分析人员为***，男，27岁，大学本科学历，高分子材料与工程专业，从事大型仪器分析3年，具有挥发性有机物分析项目上岗证。本实验采样人员为**，男，30岁，大学木科学历，应用化学专业，中级工程师，从事现场监测和采样工作6年，具有土壤采样等上岗证。本实验采样人员为***,男，31岁，大学本科学历，资源环境与城乡规划管理专业，从事现场监测和采样工作5年，具有土壤采样等上岗证。木实验室己于2020年5月对上述人员开展《土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法》的培训及理论考试，成绩合格，上述人员对标准中采样方法、实验室检测方法、质控要求均能熟练掌握，且在Fl常工作中熟悉危险化学品等安全防护知识。二、 仪器实验室具备开展《土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法》现场采样、样品保存运输和制备、实验室分析及数据处理等监测工作各环节所需的仪器设备。仪器名称检定有效期仪器状态TraCeI310-1SQLr气质联用仪（El源，TG-624MS色谱柱）2020年4月8S-2022年4月7日艮好AtOmXXYZ吹扫捕集/艮好三、试剂与材料［标准物质名称证书编号批号浓度(ugmi)有效期甲醇中59种VOC混标ST-019-11H-31H301973H6720002025.4.23氮乙烯CDAAS.620037-AE-ImlF30485020002023.12.23甲暮中氯甲烷ZD0A25V19000302002023.9.28甲暮中3种内标56H-31H301936H9310002024.7.28甲醇中甲苯Y8和4浜氛本ZH0A86V190011010002023.11.112.试剂2.1甲醇：优级纯，天津永晟精细化工有限公司，500m棚；2.2石英砂：分析纯，天津永晟精细化工有限公司，SOOg/瓶；上述试剂材料均为市售，标准溶液均有证书。四、 标准文本与原始记录标准文木实验室己发放受控版本《土壤和沉积物挥发性有机物的测定吹扫捕集/气相色谱-质谱法》标准文本至相关检测人员。原始记录实验室根据挥发性有机物的项目设计了原始记录，己纳入质量管理体制，原始记录表格己受控，受控号分别为*****监测报告监测报告有固定格式，也纳入质量管理体系。五、 环境测定挥发性有机物项目的实验室装有空调，环境温度25°C左右，湿度20%左右，能够满足挥发性有机物项目的测定。所需仪器设备条件合适，能够达到挥发性有机物项目的实验需求。挥发性有机物项目的测定在大型仪器室六进行，位于四楼，为了避免二氯甲烷、四氯化碳、三氯甲烷、四氯乙烯等易挥发有机物质干扰，特地将有机前处理室设在三楼。该项目的工作人员配备有活性炭口罩、橡胶手套、实验服等防护装备。六、实验部分1.样品的采集和保存用具有玻璃塞的棕色磨口瓶采集样品，样品采集后，4°C以下密封、避光冷藏保存，保存时间不超过7d。仪器条件2.1.1吹扫条件吹扫流量：40mPMin;吹扫温度：40"C；预热时间：2min;吹扫时间：2ImirI;干吹时间：2min;预脱附温度：180°C；脱附温度：190°C；脱附时间：2min;烘烤温度：200°C；烘烤时间：8min;传输线温度：200oCo2.1.2气相色谱仪条件进样口温度：200°C;载气：氧气；分流比：30：1;柱流量(恒流模式)：1.5ml/min;升温程序：38oC(1.8min)—10°Cmin—120°Ct15°Cmin—240°C(2min)o2.1.3质谱条件扫描方式：全扫描；扫描范围：35270amu;离子化能量：70eV;离子源温度：250°C;传输线温度260OCO校准曲线的绘制用微量注射器分别移取一定量的标准使用液(2.4)和替代物标准溶液(2.6)至空口试剂水(2.1)中，配制目标物和替代物浓度分别为5.00、10.0>20.0、50.0、100和200ugL的标准系列。用气密性注射器分别量取5.00ml上述标准系列至40ml样品瓶中，加入20.0ul内标标准溶液使每点的内标浓度均为50.0ug/L。按照仪器设定条件，从低浓度到高浓度依次测定。样品测定4.1测定前，先将样品瓶从冷藏设备中取出，使其恢复至室温。4.2低含量样品的测定若初步判定样品中挥发性有机物含量小于200pg/kg时，用5g样品直接测定；初步判定浓度在200pig^kg〜1000pgkg之间时，用Ig样品直接测定。轻轻摇动样品瓶，确认样品瓶中的样品能够自由移动，称量并记录样品瓶重量（精确到0.01g）。用气密性注射器量取5.0Rll空白试剂水、用微量注射器分别量取10.0U1内标使用液和10.0U1替代物标准使用液加入样品瓶中，按照仪器设定条件进行测定。4.3高含量样品的测定对于初步判定目标物含量大于1000pgkg的样品，从60ml样品瓶（或大于60ml其他规格的样品瓶）中取5g左右样品于预先称重的40ml无色样品瓶中，称重（精确到0.0Ig）o迅速加入10.0ml甲醇，盖好瓶盖并振摇2mine静置沉降后，用一次性巴斯德玻璃吸液管移取约Iml提取液至2ml棕色玻璃瓶中，必要时，提取液可进行离心分离。用微量注射器分别量取20.0Ul200Ul提取液、10.0Ul内标使用液和10.0Ul替代物使用液全样品瓶中，用气密性注射器量取的5.0ml空白试剂水中作为试料，放入40ml样品瓶中，按照仪器设定条件进行测定。结果计算及表示。5.2目标物的定性分析。目标物以相对保留时间和标准物质质谱图比较进行定性。5.2定量计算5.2.2对于对于高含量样品，样品中目标物的含量（ugkg）可按照以下公式进行计算。殆 mX（IOO-UZ）式中：3 样品中H标物的含量，iigkg5——试料体积，ml：PeX 试料中目标物的质量，ug/L：W样品的含水率，%:m 木样品量，g：5.1.2对于高含量样品，样品中目标物的含量(u^g)以下按照公式进行计算。f>exxVcx5xKXlOO

mx(IOO-W)xV5式中：—样品中目标物的含量，3—5—ug/kg；-试料体积，ml：—PeX--试料中目标物的质量，ug/L；VC-一提取液体积，ml：m一样品量,g：VS-—用于吹扫的提取液体积，ml：W——样品的含水率，%；K-提取液的稀释倍数。检出限和测定下限当样品量为5g,用标准四级杆质谱进行全扫描分析时，目标物的方法检出限为0.4ug/kg~2.9ugkg,测定下限为1.6ugkg~7.6ugkg°检出限的2~5倍法。(采用空白加标1.0ugL.空白加标5.0ugL分别测量7次得到方法检出限)。精密度实验室内相对标准偏差：标准曲线点测定法。(对3组浓度分别为5.0ugL(5.0ugkg)、20.0ugL(20.0ugkg)、IOOUg/L(lOOUgkg)的标准曲线点各测定6次，得到3组结果)。准确度样品加标法。(在土壤样品中分别加入IoIIg/L、IOOUg/L的标准溶液，做6个平行，得到两组结果。)

甲醇中59种VOC混标(ST-O19-11H-31H301973H67)浓度：2000ughl氯乙烯(CDAAS.620037-AE-IIDI3040050)浓度：2000U福1甲醇中氯甲烷(ZDOA25V1900030)浓度：200u/blg甲醇中3种内标(ST-(H8-56HTIHV1900196)浓度：IoOOUr/«1甲醇中甲苯-d8和4-滇氟苯(ZHOA86V1900U0)浓度：IOOOU«/®l项目标准系列曲线标准曲线方程相关系数kall*%<u三1>5.0010.0020.050.0100200相对峰面积=0.1448)农度 +0.44300.9974%t*%1.IGu1.6078S.37638.1416M.7186氯乙$a%<US1>5.0010.0020.050.0100200相对峰面积=0-4181浓®-1.60380.9974NK1tIiIIIi|%>1.73032.19195.734519.2659■10.40011-1■二51乙烯iitt<us1>5.0010.0020.050.0100200相对峰面积=0.2237*浓度•O.19580.9983NK1tIiIIIi|%>1.00331.92353.知610.616123.523744.0056—氛甲烷iitt<us1>5.0010.0020.050.0100200相对峰面积=0.3967*浓度+3.39200.9972NK1tIiIIIi|%>•1.23556.193011.106724.279145.737681.2247反式1—二氛乙iitt<us1>5.0010.0020.050.0100200相对峰面积=0.3279浓度-K).02930.9990|%>1.51212.88206.265516.5501SL328364.83421.一二M乙烷浓哎3匕1>5.0010.0020.050.0100200相对峰面积=0.6205*浓度一1.13950.9978|%>3.32696.<%0212.95S133.005167.2159123.1607%Ai-3-Xa<%浓哎3匕1>5.0010.0020.050.0100200相对烽面枳=0.5511*浓度*0.93700.9981|%>2.93935.425211.543523.911959.4695109.1393剥仿浓tt<u三1>5.0010.0020.050.0100200相对蜂血积=0.p412浓度+9.22330.998012.131314.645220.73S1•11.303577.3883135.50651.1.I-三氯乙烷浓％<us1>5.0010.0020.050.0100200相对峰面枳=0.4843浓度030130.99922.31754.23658.731S23.457150.096095.7702四氛化碳浓tt<u三1>5.0010.0020.050.0100200相对峰面枳=0.4217■浓度-0.44880.99811.95703.69657.250819.499144.294682.W67*浓％<us1>5.0010.0020.050.0100200柿对峰面税=03557浓度+0.34370.9989NrAIV%%i%>1.95003.33227.M1618.055437.23070.67531.2二SR乙烷%tt<U81>5.0010.0020.050.0100200相对峰面枳=0.4059•浓度T.16270.9972NrAIV%%i%>3.11264.87209.016922.431645.200481.2851三氛乙烯%tt<U81>5.0010.0020.050.0100200相对蜂而枳=0.2620浓度018880.9997NrAIV%%i%>1.37222.59765.131412.182126.142052.29771.2-二Mn三%tt<U81>5.0010.0020.050.0100200相对峰面SU0.3709*〉农度*0.29690.9993i%>2.01093.47627.602918.92353S.750373.8202甲苯浓a<us4>5.0010.0020.050.0100200相对峰面SU1.3173*〉农度*6.97160.9965l%>10.729516.305831.718376.4901148.9031264.SSSS1-1.2-三氛乙烷浓a<us4>5.0010.0020.050.0100200相对峰面枳=0.3985浓度+0.63950.9956l%>1.91173.11138.019121.291744.163378.4545四氛乙烯浓a<us4>5.0010.0020.050.0100200相对峰面#UO.258O・浓度039180.9995l%>1.21032.H874-491412.024426.103951.OllS

甲静中59种VOC混标(ST-OI9-11H-31H301973H67)浓度：2(XX>ugmi氯乙烯(CDAAS.620037-AE-InI3040050)浓度：2000u皿l甲醉中氯甲烷(ZDOA25V1900030)浓度：200ugtol甲醇中3种内标(ST-OI8-56H-31HV1900196)浓度：IOOOug/"甲醇中甲苯78和4■溟氛苯(ZHOA86V1900110)浓度：IOOOU凶l项目标准系列曲线标准曲线方程相关系数F乙苯A%<US1>5.OO10.OO20.050.0100200相对峰面积=2.4132浓度+6.11910.9974Nrj>*%i%>14.165524.557S51.0784132.5100263.4%5480.0319何.对-二甲苯5.0010.OO20.050.0IOO200相对峰面积=0.9870)农度 +4.41670.9981HM・h1|・i|%>11.824520.012541.1914107.31S3213.0124393.1177JPiitt<usl>5.0010.OO20.050.0IOO200相对峰面积=0.9613*浓度+1.45140.9990|%>5.11339.311719.617551.7311101.1361191.5972苯乙烯浓哎3匕1>5.0010.OO20.050.0IOO200相对峰面积=1.6434*〉农度-2.94770.9989l%>9.318816.002734.702288.9487173.56S5327.85991.,•2.2-wa乙烷浓哎3匕1>5.0010.OO20.050.0IOO200相对峰面积=0.1567)农度 046990.9996l%>0.50951.03922.51517.355415.24041.2•3-三氛内烷iitt<usl>5.0010.OO20.050.0IOO200相对峰面积=1.1383■浓度-2.02380.9995NKltIillIi|%>1.5558S.570919.817856.0991111.41861・4・二氯iitt<usl>5.0010.0020.050.0IOO200相对峰面积=2.4678浓度+7.76510.9961|%>14.228724.765253.3585144.7689286.5771506.5S%1.2二纵苯<UE1>5.0010.0020.050.0IOO200相对峰面积=2.2975*浓度+8.3271-0.9946|%>13.116522.956350.5053132.9920259.0362455.S555浓哎3匕1>5.0010.0020.050.0IOO200相对峰面积=4.6224*浓度-3.71620.9998|%>22.SG5740.804336.0595228.1523458.6803甲苯-(JS浓哎3匕1>5.0010.0020.050.0IOO200相对烽面枳=2.3377*浓度-5.76320.98559.719620.8413>15.082291.5539236.4563浓tt<u三1>5.0010.0020.050.0100200相对烽面枳=2.0094*浓度-5.64890.98578.764517.S91935.811578.28S9202.7443浓tt<u三1>5.0010.0020.050.0100200相对峰面积44672浓度+3.17760.99919.267015.071S31.786078.8864155.1147293.5235,,,浓tt<u三1>5.0010.0020.050.0IOO200相对峰面枳=0.5087*〉农度*0.17500.99802.4382•1.06169.725926.158651.1741100.3160平行样品编号蔡备注测定结果(ug/kg)12.0180空白+1.0ug/l22.421032.200442.053252.134962.048472.0845平均值儿(ug/kg)2.14标准偏差Si(ug/kg)0.14t值3.143检出限(ug/kg)0.4测定下限(ug/kg)1.6气体或固体样品检出限的计算方法检出限( )测定下限( )平行样品编号氯甲烷氯乙烯bb2、2-四氯乙烷备注测定结果(ug/kg)15.06197.70585.3953空白+5.0ug/l24.24778.45425.548935.02798.02015.666844.89288.1276.075254.92178.18295.56364.49727.77915.470474.83688.0735.3275平均值X(ug/kg)4.888.055.58标准偏差Si(ug/kg)0.300.250.25t值3.1433.1433.143检出限(ug/kg)0.90.80.8测定下限(ug/kg)3.63.23.2气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号1,2,3-三氯丙烷1,1-二氯乙烯二氯甲烷备注测定结果(ug/kg)14.24865.08591.7196空白+5.0ug/l25.39696.12271.794935.15615.72071.48744.97885.78481.410655.08395.81991.401665.04785.43051.095274.94885.811.3666平均值X(ug/kg)5.235.71.5标准偏差Si(ug/kg)0.350.330.23t值3 1433.1433.143检出限(ug/kg)1.11.00.7测定下限(ug/kg)4.44.02.8气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号反式1,2-二氯乙烯1,1-二氯乙烷加式T,2-.氯乙烯备注测定结果(ug/kg)14.37643.51833.0485空白+5.0ug/l24.46913.93823.851333.49253.50663.4344.29183.53.415354.01373.53553.477263 93363.20233.211674.12473.44113.3562平均值x(ug/kg)4.13.53.4标准偏差Si(ug/kg)0.330.220.25t值3.1433.1433.143检出限(ug/kg)1.00.70.8测定下限(ug/kg)4.02.83.2气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号氯仿It1»I-二氯乙烷四氯化碳备注测定结果(ug/kg)17.12844.60724.8448空白+5.0ug/l26.0615.65776.011836.66125.33225.660346.79685.25195.604156.40765.35135.621466.72324.99435.306276.41335.23285.4961平均值X(ug/kg)6.65.25.5标准偏差Si(ug/kg)0.340.330.36t值3 1433.1433.143检出限(ug/kg)1.11.01.1测定下限(ug/kg)4.44.04.4气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号苯1,2-二氯乙烷三氯乙烯备注测定结果(ug/kg)13.79523.224611.8006空白+5.0ug/l24.63763.94711.570734.34113.206211.95144.22683.153511.508554.24473.277711.209463.87882.911711.275774.10623.132411.7478平均值X(ug/kg)4.23.311.6标准偏差Si(ug/kg)0.280.320.27t值3.1433.1433.143检出限(ug/kg)0.91.00.9测定下限(ug/kg)3.64.03.6气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号1,2-二氯丙烷甲苯If2-二氯乙烷备注测定结果(ug/kg)14 90832.382.2858空白+5.0ug/l24.70082.52812.540534.38542.38262.202144.17972.36242.165754.3042.42322.23264.02972.09212.066274.15252.26972.1177平均值x(ug/kg)4.42.32.2标准偏差Si(ug/kg)0.320.140.15t值3.1433.1433.143检出限(ug/kg)1.00.40.5测定下限(ug/kg)4.01.62.0气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号四氯乙烯氯苯Itb1,2-四氯乙烷备注测定结果(ug/kg)15.13243.2963.1172空白+5.0ug/l26.18914.00293.892835.84833.76753.76845.87443.7283.694155.88333.70093.749265.59833.47873.497875.84623.71633.6314平均值X(ug/kg)5.83.73.6标准偏差Si(ug/kg)0.330.220.25t值3 1433.1433.143检出限(ug/kg)1.00.70.8测定下限(ug/kg)4.02.83.2气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号乙苯间,对-二甲苯邻・二甲苯备注测定结果(ug/kg)12.53216.53323.2082空白+5.0ug/l23・16437.31734.12332.89546.74363.820742.93636.90213.862453・00626.80123.828762.65866.39493.606572.81446.66483.7802平均值X(ug/kg)2.96.83.7标准偏差Si(ug/kg)0.210.300.28t值3.1433.1433.143检出限(ug/kg)0.70.90.9测定下限(ug/kg)2.83.63.6气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号苯乙烯E4-二氯苯If2-二氯苯备注测定结果(ug/kg)12.9032.33142.1956空白+5.0ug/l23.71912.76682.525433.33612.48032.31943.40212.40812.005253.37272.43412.166763.20172.25331.931573.33142.27792.0695平均值X(ug/kg)3.32.42.2标准偏差Si(ug/kg)0.240.170.20t值3 1433.1433.143检出限(ug/kg)0.80.50.6测定下限(ug/kg)3.22.02.4气体或固体样品检出限的计算方法检出限( )测定下限( )

平行样品编号氯甲烷氯乙烯1,b2、2-四氯乙烷备注测定结果(ug/kg)15.06198.11877.004526.12168.45427.814335.02798.02015.666844.89288.1276.075254.92178.18295.563064.49727.77915.4704平均值乞(ug/kg)5.098.116.27标准偏差Si(ug/kg)0.550.220.95相对标准偏差RSD%10.72.715.1表3方法精密度测试数据表平行样品编号 b2,3-三氯丙烷b1-二氯乙烯备注1 4.2486 4.918平行样品编号 b2,3-三氯丙烷b1-二氯乙烯备注1 4.2486 4.9185.7622 5.3969 5.03445.0859测定结果(ug/kg)3 5.1561 4.8615.72074 4.9788 4.66485.78485.0839 4 7166 5.81995.0478 4.6001 5.4305平均值x(ug/kg)4.平均值x(ug/kg)4.99 4.80 5.60相对标准偏差 RSDj%7.83.55.2平行样品编号二氯甲烷反式1,2-二氯乙烯b1-二氯乙烷备注测定结果(ug/kg)11.71964.37643.518321.29213.49253.127431.4874・28933.506641.41064.29183.551.40164.01373.535561.09523.93363.2023平均值x(ug/kg)1.404.073.40标准偏差Si(ug/kg)0.210.330.18相对标准偏差RSD%14.88.15.4表3方法精密度测试数据表平行样品编号 顺式T,2-二氯氯仿乙烯1,1,1-二氯乙

烷备注1 3.4510 7.12845.33002 3.0485 6.06104.6072平行样品编号 顺式T,2-二氯氯仿乙烯1,1,1-二氯乙

烷备注1 3.4510 7.12845.33002 3.0485 6.06104.6072测定结果(ug/kg)3 3.4300 6.66125.33224 3.4153 6.79685.25193.47726.40765.35133.21165.59374.9943平均值乞(ug/kg)3.346.445.14相对标准偏差 RSDj%5.18.55.7平行样品编号四氯化碳苯b2-二氯乙烷备注测定结果(ug/kg)15.68664.21853.224624.84483.79523.102835.66034.34113.206245.60414.22683.153555.62144.24473.277765.30623.87882.9117平均值x1(ug/kg)5.454.123.15标准偏差Si(ug/kg)0.330.220.13相对标准偏差RSD%6.05.44.1表3方法精密度测试数据表平行样品编号 三氯乙烯 b2-二氯丙烷甲苯备注1 11.8006 4.34472.38002 11.5707 4.90831.9883测定结果(ug/kg)3 11.951 4.38542.38264 12.4594 4.17972.平行样品编号 三氯乙烯 b2-二氯丙烷甲苯备注1 11.8006 4.34472.38002 11.5707 4.90831.9883测定结果(ug/kg)3 11.951 4.38542.38264 12.4594 4.17972.362411.20944.3042.423211.27574.02972.0921平均值乞(ug/kg)11.714.362.27标准偏差Si(ug/kg)0.470.300.18相对标准偏差 RSDj%4.06.9&1平行样品编号If2-三氯乙烷四氯乙烯氯苯备注测定结果(ug/kg)12.28585.89483.791222.24415.13243.29632.20215.84833.767542.16575.87443.72852.2325.88333 700962.06625.59833.4787平均值x(ug/kg)2.205.713.63标准偏差Si(ug/kg)0.080.300.20相对标准偏差RSD%3.55.35.4表3方法精密度测试数据表间，对-二甲苯备注平行样品编号1,1,1,2-四氯乙乙苯

烷间，对-二甲苯备注1 3.7253 2.88366.85872 3.1 3.7253 2.88366.85872 3.1172 2.53216.5332测定结果(ug/kg)3 3.768 2.89546.74364 3.6941 2.93636.90213.74923.3.74923.00626.80123.49782.3.49782.65866.3949平均值乞(ug/kg)3.592.平均值乞(ug/kg)3.592.826.71相对标准偏差 RSDj%7.0653.0平行样品编号邻・二甲苯苯乙烯b4-二氯苯备注测定结果(ug/kg)13.83823.34222.331423.20822.9032.146533.82073.33612.480343.86243.40212.408153.82873.37272.434163.60653.20172.2533平均值x(ug/kg)3.693.262.34标准偏差Si(ug/kg)0.260.190.13相对标准偏差RSD%6.95.85.3表3方法精密度测试数据表平行样品编号It2-二氯苯备注测定结果(ug/kg)12.195621.928732.31942.005252.166761.9315平均值x(ug/kg)2.09标准偏差Si(ug/kg)0.16相对标准偏差 RSDj%7.6平行样品编号氯甲烷氯乙烯1»b2,2-四氯乙烷备注测定结果(ug/kg)118.088719.633315.3015217.356619.341313.3759318.288420.094816.2038418.064820.804512.5896519.333622.094916.1182618.802321.318216.4118平均值x1(ug/kg)18.3220.5515.00标准偏差Si(ug/kg)0.681.051.63相对标准偏差RSD%3.75.110.8表3方法精密度测试数据表平行样品编号b2,3-二氯丙烷b1-:氯乙烯备注测定结果(ug/kg)114.766114.945217.8277215.96415.799217.8855314.353613.889419.2092417.165414.166620.0727521.646715.983518.1639622.431817.595718.8231平均值乞(ug/kg)17.7215.4018.66标准偏差Si(ug/kg)3.491.370.88相对标准偏差RSD%19.78.94.7

平行样品编号二氯中烷反式1,2-二氯乙烯bI-二氯乙烷备注测定结果(ug/kg)119.654116.329315.6738217.307216.581915.7665318.157818.091917.1541419.48318.656618.0196518.725815.973616.0295618.90317.088216.9202平均值x(ug/kg)18.7117.1216.59标准偏差Si(ug/kg)0.871.050.93相对标准偏差RSD%4.76.15.6表3方法精密度测试数据表平行样品编号顺式T,2-二氯氯仿乙烯1,1,I-二氯乙烷备注1 15.2823 15.9449平行样品编号顺式T,2-二氯氯仿乙烯1,1,I-二氯乙烷备注1 15.2823 15.944916.77612 15.846 14.822417.6888测定结果(ug/kg)3 17.5241 16.551419.3684 18.4814 18.710820.333458316.214717.6095458316.214717.60955799962826957999628269平均值x(ug/kg)16.5316.7118.43标准偏差平均值x(ug/kg)16.5316.7118.43标准偏差Si(ug/kg)1.261.421.31相对标准偏差 RSDj%7.68.57.1平行样品编号四氯化碳苯1,2-二氯乙烷备注测定结果(ug/kg)118.938215.425213.885218.669816.313215.2317320.398217.88217.3498421.372818.782118.4116517.797915.133115.8031620.193216.68116.7847平均值x(ug/kg)19.5616.7016.24标准偏差Si(ug/kg)1.321.411.61相对标准偏差RSD%6.78.59.9表3方法精密度测试数据表平行样品编号 三氯乙烯 1,2-二氯丙烷甲苯备注1 17.5964 14.846312.48062 24.平行样品编号 三氯乙烯 1,2-二氯丙烷甲苯备注1 17.5964 14.846312.48062 24.0138 16.378812.8946测定结果(ug/kg)3 21.934418.208614.30084 23.088819.258114.833420.991815.20.991815.872115.479324.004617.24.004617.092516.484平均值x(ug/kg)21.9416.9414.41标准偏差Si(ug/kg)平均值x(ug/kg)21.9416.9414.41标准偏差Si(ug/kg)2.441.601.53相对标准偏差 RSDj%11.19.510.6平行样品编号If2-三氯乙烷四氯乙烯氯苯备注测定结果(ug/kg)111.045118.488814.5375212.466617.083215.2138314.272318.468816.8083414.593218.996917.4532516.571617.046615.1466617.447520.046416.6427平均值x1(ug/kg)14.4018.3615.97标准偏差Si(ug/kg)2.411.151.15相对标准偏差RSD%16.76.37.2表3方法精密度测试数据表平行样品编号1,1,1,2-四氯乙烷乙苯间，对-二甲苯备注测定结果(ug/kg)112.873414.2929.4439214.159815.03931.36315.779816.591433.9482416.273117.099134.9092515.596114.148127.7408617.038515.590730.6901平均值乞(ug/kg)15.2915.4631.35标准偏差Si(ug/kg)1.511.202.70相对标准偏差RSD%9.97.8&6

平行样品编号邻・二甲苯苯乙烯b4-二氯苯备注测定结果(ug/kg)114.303114.500920.4687215.557615.539519.8605316.941716.95215.9517417.463317.596716.4964514.259813.983415.1452615.90615.425516.9294平均值x(ug/kg)15.7415.6717.48标准偏差Si(ug/kg)1.321.392.18相对标准偏差RSD%8.48.912.4表3方法精密度测试数据表平行样品编号It2-二氯苯备注测定结果(ug/kg)118.2285218.6706315.6776416.0617516.2465617.8789平均值x(ug/kg)17.13标准偏差Si(ug/kg)1.28相对标准偏差 RSDj%7.5平行样品编号氯甲烷氯乙烯1»b2,2-四氯乙烷备注测定结果(ug/kg)174.398980.301667.4506283.617188.717462.8997374.126278.290164.0259468.764174.669957.3259573.591778.06661.1045673.24476.907664.5709平均值x1(ug/kg)74.6279.4962.90标准偏差Si(ug/kg)4.874.883.44相对标准偏差RSD%6.56.15.5表3方法精密度测试数据表平行样品编号b2,3-二氯丙烷b1-:氯乙烯备注测定结果(ug/kg)165.642277.368376.5354264.946277.831486.9573367.056779.548379.0129461.411473.177477.5305561.028169.483582.8853666.022175.367381.4554平均值乞(ug/kg)64.3575.4680.73标准偏差Si(ug/kg)2.523.663.87相对标准偏差RSD%3.94.84.8

平行样品编号二氯中烷反式1,2-二氯乙烯bI-二氯乙烷备注测定结果(ug/kg)178.988978.075377.8014293.226388.099987.7322383.084779.601478.551480.88178.468876.0773586.9384.379482.1995686.819683.310181.4852平均值x(ug/kg)84.9981.9980.64标准偏差Si(ug/kg)5.133.964.16相对标准偏差RSD%6.04.85.2表3方法精密度测试数据表平行样品编号顺式T,2-二氯氯仿乙烯1,1,I-二氯乙烷备注1 80.5091 82.945983.平行样品编号顺式T,2-二氯氯仿乙烯1,1,I-二氯乙烷备注1 80.5091 82.945983.02022 89.7226 95.023390.7995测定结果(ug/kg)3 80.066783.489182.32934 77.872181.148579.824883.042787.83.042787.381685.723382.250287.82.250287.118184.5208平均值x(ug/kg)82.2486.1884.37平均值x(ug/kg)82.2486.1884.37标准偏差Si(ug/kg)4.084.973.74相对标准偏差 RSDj%5.05.84.4平行样品编号四氯化碳苯1,2-二氯乙烷备注测定结果(ug/kg)188.036383.8189.9079297.382992.0703101.2466386.913883.210289.4598485.381481.732986.9302592.217987.01992.2338691.650586.631992.9425平均值x(ug/kg)90.2685.7592.12标准偏差Si(ug/kg)4.393.714.96相对标准偏差RSD%4.94.35.4表3方法精密度测试数据表平行样品编号三氯乙烯1,2-二氯丙烷甲苯备注102.248383.899373.9492115.120993.392480.3874测定结果(ug/kg)98.847683.999174.952999.756980.792471.6434109.173887.047178.5109106.平行样品编号三氯乙烯1,2-二氯丙烷甲苯备注102.248383.899373.9492115.120993.392480.3874测定结果(ug/kg)98.847683.999174.952999.756980.792471.6434109.173887.047178.5109106.559986.733676.9007平均值x(ug/kg)105.2885.9876.06标准偏差Si(ug/kg)6.244.293.18相对标准偏差 RSDj%5.95.04.2平行样品编号If2-三氯乙烷四氯乙烯氯苯备注测定结果(ug/kg)170.752777.518779.5695278.903184.281287.2272373.603678.827481.1538470.333776.014178.2111576.286182.093383.8631676.061680.093183.6915平均值x1(ug/kg)74.3279.8082.29标准偏差Si(ug/kg)3.383.033.29相对标准偏差RSD%4.53.84.0表3方法精密度测试数据表平行样品编号1,1,1,2-四氯乙烷乙苯间，对-二甲苯备注测定结果(ug/kg)177.917782.4009169.4923286.662490.8196186.2235380.450783.4656173.064477.599680.9537165.4833584.294986.6358178.0302682.053185.6464176.Illl平均值乞(ug/kg)81.5084.99174.73标准偏差Si(ug/kg)3.583.537.22相对标准偏差RSD%4.44.24.1

平行样品编号邻・二甲苯苯乙烯b4-二氯苯备注测定结果(ug/kg)182.166886.1824101.6629291.645595.5938100.1052386.104287.6765103.1327482.393184.947394.3118588.326391.693190.409688.057790.40896.5701平均值x(ug/kg)86.4589.4297.70标准偏差Si(ug/kg)3.693.944.84相对标准偏差RSD%4.34.44.9表3方法精密度测试数据表平行样品编号It2-二氯苯备注测定结果(ug/kg)1IOL72542100.81233104.125494.7995592.2091698.2381平均值x(ug/kg)98.65标准偏差Si(ug/kg)4.49相对标准偏差 RSDj%4.5平行样品编号实际样品加标测试数据备注氯甲烷氯乙烯 1,b2、2-四氯乙烷样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00006.7540.00008.87190.00009.840220.00006.65780.00008.71620.000010.323130.00007.28310.00009.12760.000011.514340.00008.13890.00009.29430.000011.515550.000011.15980.000010.7560.000011.264460.00008.22680.00009.23090.000010.4963平均值元、y.(ug/kg)0.00008.040.00009.330.000010.8加标量(ug/kg )10.010.010.0加标回收率Pi(%)80.493.3108表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,2,3-二氯丙烷蔡样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00009.26581.8610.25820.00009.29261.629.167930.000010.33141.4599.021840.000010.72981.5418.973550.000010.52371.6128.786860.00009.86831.6237.0718平均值元、y.(ug/kg)0.000010.01.628.88加标量(ug/kg )10.010.0加标回收率Pi(%)10072.6

平行样品编号实际样品加标测试数据备注b1-二氯乙烯二氯甲烷 反式1，2・二氯乙烯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00006.69730.00009.84470.00007.180720.00007.03230.00008.03220.00006.627230.00007.15910.00008.39860.00006.291840.00007.05020.00007.69580.00006.925950.00006.85140.00007.55510.00006.877960.00007.26680.00009.67970.00006.9501平均值、y.(ug/kg)0.00007.010.00008.530.00006.81加标量(ug/kg )10.010.010.0加标回收率Pi(%)70.185.368.1表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,1-二氯乙烷顺式-1,2-二氯 一乙烯 飙仿样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00006.91520.00007.19160.00007.328320.00006.62630.00006.78450.00007.357530.00006.89930.00006.84360.00008.428140.00006.95720.00006.71530.00008.852650.00007.81430.00007.39720.000010.423160.00008.68230.00008.41250.000011.2801平均值、y.(ug/kg)0.00007.320.00007.220.00008.95加标量(ug/kg )10.010.010.0加标回收率 Pi(%)73.272.289.5平行样品编号实际样品加标测试数据备注1,I-二氯乙烷四氯化碳 苯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.69527.84962.312311.83870.00007.611020.64107.48622.826610.07990.00007.472930.63537.71462.81810.43200.00007.207840.62967.70802.875110.50450.00007.168850.62768.44863.368311.52890.00007.712160.63469.31603.389710.82300.00008.7467平均值三、y.(ug/kg)0.648.092.9310.870.00007.65加标量(ug/kg )10.010.010.0加标回收率Pi(%)74.579.476.5表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,2-二氯乙烷二氯乙烯 L2-二氯丙烷样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00006.8280.96518.72050.00008.32420.00006.64240.79578.41650.00008.357730.00007.19080.76848.22900.00008.223040.00007.48190.74938.29030.00008.368450.00008.38310.75428.24450.00008.946360.00009.82490.00009.92280.000010.0696平均值斤、y.(ug/kg)0.00007.730.818.640.00008.71加标量(ug/kg )10.010.010.0加标回收率Pi(%)77.378.387.1

平行样品编号实际样品加标测试数据备注甲苯b12-三氯乙烷 四氯乙烯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.42086.57670.00006.88272.398910.118020.39746.83070.00007.99852.51399.216430.05966.77670.0000&0622.50139.130240.23446.80730.00008.28142.70199.016550.37588.62990.000010.16072.81529.795660.2367.09880.00008.33672.922710.4093平均值斤、y.(ug/kg)0.297.120.0000&292.649.61加标量(ug/kg )10.010.010.0加标回收率Pi(%)68.382.969.7表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注氯苯bbb2-四 7廿氯乙烷 乙苯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00007.80090.00007.85580.00006.951020.00007.89300.0000&8380.00007.373830.00007.80600.00008.75870.00006.973540.00007.79360.00008.77150.00006.953050.00008.34350.000010.27550.00006.690060.00007.97800.00008.86750.00006.5869平均值、y.(ug/kg)0.00007.940.0000&890.00006.92加标量(ug/kg )10.010.010.0加标回收率Pi(%)79.488.969.2平行样品编号实际样品加标测试数据备注间，对■—甲苯邻-二甲苯 苯乙烯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.000013.71380.00007.68070.00007.370720.000013.57570.00007.79760.00007.400530.000013.41960.00007.76470.00007.215740.000013.44170.00007.78260.00007.214450.000013.63980.00008.05730.00007.098760.000013.98210.00008.07990.00007.4473平均值元、y.(ug/kg)0.000013.630.00007.860.00007.29加标量(ug/kg )20.010.010.0加标回收率Pi(%)68.278.672.9表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,4-一氯本b2-一氯本样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.00007.92820.00007.736820.00006.30970.00006.229230.00006.44170.00006.645440.00006.65580.00006.98650.00007.25510.00007.125760.00006.77940.00007.1729平均值、y.(ug/kg)0.00006.890.00006.98加标量(ug/kg )10.010.0加标回收率Pi(%)68.969.8

平行样品编号实际样品加标测试数据备注氯甲烷氯乙烯 bb2、2-四氯乙烷样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.000065.1060.000070.38490.000081.811220.000084.61730.00008&24430.000097.421530.000067.8070.000071.01780.000067.203740.000068.84820.000068.64540.000084.069950.000068.30380.000067.16450.000067.040860.000062.24840.000061.20850.00006&68平均值元、y.(ug/kg)0.000069.50.000071.10.000077.7加标量(ug/kg )100100100加标回收率Pi(%)69.571.177.7表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,2,3-二氯内烷蔡样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.000077.21791.8669.787720.000092.13861.6289.013630.000064.23191.45962.544540.000081.18421.54169.468250.000064.31901.61264.337060.000066.37691.62360.7066平均值元、y.(ug/kg)0.000074.21.6269.3加标量(ug/kg )100100加标回收率Pi(%)74.267.7

平行样品编号实际样品加标测试数据备注b1-二氯乙烯二氯甲烷 反式1，2・二氯乙烯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.000071.87270.000082.53140.000078.716820.000088.47140.0000101.29050.000098.435230.000071.35580.000080.93010.000078.444640.000071.13490.000087.07140.000076.410650.000068.75620.000081.29030.000075.796360.000062.18610.000075.45730.000067.5979平均值元、y.(ug/kg)0.000072.30.000084.80.000079.2加标量(ug/kg )100100100加标回收率Pi(%)72384.879.2表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,1-二氯乙烷顺式-1,2-二氯 一乙烯 氯仿样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.000082.16530.000085.27460.000087.237420.0000101.90990.0000103.92220.0000110.123830.000080.93010.000082.42990.000084.512240.000084.84650.000084.45470.000089.807450.000080.19970.000081.05850.000084.455760.000074.37570.000074.6510.000077.4128平均值、y.(ug/kg)0.000084.10.000085.30.000088.9加标量(ug/kg )100100100加标回收率 Pi(%)84.185.388.9平行样品编号实际样品加标测试数据备注1,I-二氯乙烷四氯化碳 苯样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.695284.13262.312386.93930.000090.759120.6410103.53832.826610&15630.0000111.712430.635383.04762.81887.23020.000086.829340.629684.02972.875185.93710.000086.445450.627681.54943.368384.55040.000084.465560.634673.96473.389775.95270.000077.8524平均值2、y.(ug/kg)0.6485.02.9388.10.000089.7加标量(ug/kg )IOOIOO100加标回收率Pi(%)84.485.289.7表4方法准确度测试数据表平行样品编号实际样品加标测试数据备注1,2-二氯乙垸二氯乙烯 L2-二氮内烷样品加标样品样品加标样品样品加标样品测定结果(ug/kg)10.000094.43140.965194.00410.000092.411720.0000114.10620.7957112.30420.0000112.79430.000088.68880.768490.71940.000089.2657