CMA資質(zhì)擴(kuò)項認(rèn)證-方法確認(rèn)報告-固定污染源廢氣揮發(fā)性有機(jī)物的測定方法確認(rèn)報告

1、xxxxxxxxx分析測試中心方法確認(rèn)/證實(shí)報告檢測項目固定污染源廢氣揮發(fā)性有機(jī)物的測定檢測方法HJ734-2014確認(rèn)/證實(shí)人xxx審核人技術(shù)批準(zhǔn)審核結(jié)論因推薦使用不推薦使用需重新進(jìn)行方法確認(rèn)批準(zhǔn)日期目的通過方法驗證，確認(rèn)本中心在人、機(jī)、料、法、環(huán)、測等方面都達(dá)到標(biāo)準(zhǔn)方法要求，實(shí)驗室具備固定污染源廢氣揮發(fā)性有機(jī)物的測定HJ734-2014的方法測定能力。方法簡介2.1適用范圍本標(biāo)準(zhǔn)規(guī)定了固定污染源廢氣中24種揮發(fā)性有機(jī)物測定的固相吸附-熱脫附/氣相色譜-質(zhì)譜法。本標(biāo)準(zhǔn)適用于固定污染源廢氣中24種揮發(fā)性有機(jī)物的測定，24種揮發(fā)性有機(jī)物包括：丙酮、異丙醇、正己烷、乙酸乙酯、苯、六甲基二硅氧烷、3

2、-戊酮、正庚烷、甲苯、環(huán)戊酮、乳酸乙酯、乙酸丁酯、丙二醇單甲醚乙酸酯、乙苯、對/間二甲苯、2-庚酮、苯乙烯、鄰二甲苯、苯甲醚、苯甲醛、1-癸烯、2-壬酮、1-十二烯。當(dāng)采樣體積為300ml時，本標(biāo)準(zhǔn)的方法檢出限為0.0010.01mg/m3,測定下限為0.0040.04mg/m32.2方法原理使用填充了合適吸附劑的吸附管直接采集固定污染源廢氣中揮發(fā)性有機(jī)物，將吸附管置于熱脫附儀中進(jìn)行二級熱脫附，脫附氣體經(jīng)氣相色譜分離后用質(zhì)譜檢測，根據(jù)保留時間、質(zhì)譜圖或特征離子定性，內(nèi)標(biāo)法或外標(biāo)法定量。23測試流程簡介2.3.1吸附管的準(zhǔn)備同時采樣，且每批樣品采集一根串聯(lián)吸附采樣管，用于監(jiān)視采樣是否穿透。2.3

3、.3全程序空白采樣將密封保存的吸附采樣管帶到采樣現(xiàn)場，同樣品吸附管同時打開封帽接觸現(xiàn)場環(huán)境空氣，采樣時全程序空白吸附管關(guān)閉封帽，采樣結(jié)束時同樣品吸附管接觸環(huán)境空氣，同時關(guān)閉封帽，按與樣品相同的操作步驟進(jìn)行處理和測定，用于檢查從樣品采集到分析全過程是否受到污染。2.3.4分析流程熱脫附條件：吸附管初始溫度：室溫；聚焦冷阱初始溫度：室溫；干吹流量：30ml/min；干吹時間：2min；吸附管脫附溫度：300C；吸附采樣管脫附時間：3min；脫附流量：30ml/min；聚焦冷阱溫度:-11C；聚焦冷阱脫附溫度：300C；冷阱脫附時間：3min；傳輸線溫度：120C。色譜柱及分離條件：安捷倫HP-VO

4、C,60m*0.32mm*1.80um；柱流量（恒流模式）：1.2ml/min；分流比：30:1。升溫程序：初始溫度35C，保持5min，以6C/min的速度升溫至220C，保持3min，在230C后運(yùn)行1min。質(zhì)譜條件：掃描方式：全掃描；掃描范圍：33270amu；離子化能量：70eV；傳輸線溫度：230C；離子源溫度：230C；四級桿溫度：150C。驗證內(nèi)容3.1實(shí)驗室資源確認(rèn)表1實(shí)驗室資源確認(rèn)情況姓名職稱/技術(shù)資格專業(yè)領(lǐng)域相關(guān)培訓(xùn)學(xué)習(xí)經(jīng)歷方法驗證過程分工人參加過安捷倫GC/GC-MS專業(yè)培訓(xùn)、Markes公司熱解析儀培參與過環(huán)境樣品中揮發(fā)性鹵代烴等樣品測試和方法開發(fā)工作。熟悉GC/GC

5、-MS儀器結(jié)構(gòu)原理、操作、樣品前處理等。及分析儀器設(shè)備方法要求實(shí)驗室是否具備性能是否滿足要求確認(rèn)人1、氣相色譜-質(zhì)譜儀（GC-MS）:安捷倫7890B-5977A。EI源2、色譜柱：安捷倫色譜柱HP-VOC或其他性能相近的色譜柱。3、不銹鋼吸附管：TeanaxTA；組合1吸附管，內(nèi)裝TenaxGR、CarbopackB；組合3吸附管，內(nèi)裝CarbopackC、CarbopackB、Carboxen1000。內(nèi)徑均為5mm。4、熱解析儀：MarkesTD-100及標(biāo)氣加載裝置。5、一般實(shí)驗室常用儀器和設(shè)備。口Y是N否Y是N否標(biāo)準(zhǔn)物質(zhì)22種VOCs混標(biāo)HJ734-2014,上海安譜實(shí)驗科技股份有限

6、公司，2000mg/l；乳酸乙酯和苯甲醛混標(biāo)HJ734-2014，上海安譜實(shí)驗科技股份有限公司，2000mg/l；替代物標(biāo)準(zhǔn)溶液：氘代1,2-二氯乙烷及氘代甲苯混標(biāo)，上海安譜實(shí)驗科技股份有限公司，1000mg/l?？赮是N否Y是N否試劑1、氮?dú)?，純?9.999%其他3.2標(biāo)準(zhǔn)曲線3.2.1標(biāo)液/標(biāo)準(zhǔn)溶液基本信息表2標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)溶液基本信息標(biāo)準(zhǔn)物質(zhì)名稱證書編號標(biāo)稱值是否有效甲醇中22種VOC混標(biāo)2771892000mg/L是甲醇中乳酸乙酯和苯甲醛混標(biāo)2807942000mg/L是1,2-二氯乙烷-d4和甲苯-d4混標(biāo)2757081000mg/L是3.2.2標(biāo)準(zhǔn)溶液配置與測定配置方法：a.22

7、種VOCs混標(biāo)儲備溶液：移取標(biāo)準(zhǔn)溶液原液0.25mL于1mL定量瓶中稀釋至刻度，則儲備液c1=500mg/L；乳酸乙酯和苯甲醛混標(biāo)儲備液：移取標(biāo)準(zhǔn)溶液原液0.25mL于1mL定量瓶中稀釋至刻度，貝M諸備液c2=500mg/L；替代物混標(biāo)儲備液：移取標(biāo)準(zhǔn)溶液原液0.50mL于1mL定量瓶中稀釋至刻度，則儲備液c3=500mg/L；將上述a、b、c儲備液分別移取10、20、50、100、160、200uL于1mL定容瓶中，混勻并稀釋至刻度。標(biāo)準(zhǔn)曲線配制(mg/L)配備將老化好的吸附管裝到熱脫附標(biāo)樣加載平臺上，用微量注射器取2.0“混標(biāo)溶液（步驟d）注入空白吸附管，用50ml/min的N2吹掃吸附管

8、1min，迅速取下吸附管，用密封帽將吸附管兩端密封，得到含量為10.0、20.0、50.0、100、160、200ng的校準(zhǔn)系列吸附管。表4標(biāo)準(zhǔn)曲線基本信息序號項目名稱線性范圍(ng)回歸方程相關(guān)系數(shù)r2是否滿足標(biāo)準(zhǔn)要求丙酮10-200異丙醇10-20010-200y=1.265e+003*x+1.040e+004y=5.632e+003*x-2.268e+004y=4.476e+003*x+1.822e+0040.9990.9970.996正己烷y=6.026e+003*x+10-2000.9991.830e+003乙酸乙酯六甲基二硅氧烷10-200y=2.028e+004*x+4.088e

9、+0040.99810-2000.999y=3.706e+003*x-nqqsy=1.049e+004*x+3.382e+0040.99511環(huán)戊酮y=2.452e+003*x+10-200l.272e+30.99912乙酸丁酯y=5.854e+003*x-10-200l.43e+030.9951314乳酸乙酯丙二醇單甲醚乙酸酯10-200y=6.243e+003*x-1.992e+0040.999y=3.281e+003*x-10-2003.245e+040.999y=1.345e+004*x+10-2001.793e+00415乙苯20-400y=2.831e+004*x+1.610e+0

10、050.99916對/間二甲苯10-200y=5.406e+003*x-7.317e+0030.999172-庚酮10-200y=8.731e+003*x-1.359e+0040.99918苯乙烯10-200y=1.106e+004*x+3.020e+0040.99919鄰二甲苯10-200y=6.096e+003*x-9.752e+0030.999fiuHiI9話怖叮事口Jlttlz一241-十二烯10-200y=2.501e+003*x-8.661e+0030.999是25二氯乙烷-d4（替代物）10-200y=3.637e+003*x-7.086e+0030.999是結(jié)論標(biāo)準(zhǔn)曲線相關(guān)系數(shù)

11、r2均滿足大于0.995要求注1:標(biāo)準(zhǔn)曲線測試數(shù)據(jù)及計算結(jié)果詳見打印的附件資料。注2：間/對二甲苯為共流出物，計算時合并取兩者加和。標(biāo)準(zhǔn)樣品測定譜圖見表5,以標(biāo)準(zhǔn)曲線中10Ong濃度點(diǎn)為例。表5標(biāo)準(zhǔn)樣品測試譜圖分析項目：24種VOCs標(biāo)準(zhǔn)溶液濃度：100ng豐度11X)003150000314&000313DOCO312DOCO3111X)00313DOCO39DODO3SDOQOD7DOCO35DOCO35DOCO34COC033DOCO32&DCGD3.3空白實(shí)驗取7個全程序空白并進(jìn)行分析，測試結(jié)果如下表6。表6空白實(shí)驗測定結(jié)果序號測試空白濃度（ng）平均空白濃度（ng）標(biāo)準(zhǔn)給出的檢出限（

12、ng）標(biāo)準(zhǔn)給出的測定下限（ng）1丙酮4.990.004.045.700.004.034.033.260.6412.52異丙醇0.000.000.000.000.000.000.000.003.132.553正己烷0.000.000.000.000.000.000.000.001.064.244乙酸乙酯2.002.550.981.910.000.000.001.061.807.225六甲基二硅氧烷0.000.000.000.000.000.000.000.000.421.696苯0.000.000.000.000.000.000.000.001.164.637正庚烷0.001.201.201.

13、201.211.241.221.041.204.7883-戊酮0.000.000.000.000.000.000.000.000.642.549甲苯-d80.000.000.000.000.000.000.000.00-10甲苯0.000.000.000.000.000.000.000.001.234.9211環(huán)戊酮0.000.000.000.000.000.000.000.001.184.7012乙酸丁酯0.480.250.180.193.471.011.931.071.395.5513乳酸乙酯0.000.000.000.000.000.000.000.002.198.7714丙二醇單甲醚乙

14、酸酯3.200.003.193.193.190.003.212.281.536.1215乙苯0.000.000.000.000.000.000.000.001.917.6616對/間二甲苯0.000.000.000.000.000.000.000.002.8111.2172-庚酮1.361.361.361.361.361.361.371.360.351.4018苯乙烯1.631.631.622.041.581.561.571.661.204.8019鄰二甲苯0.000.000.000.000.000.000.000.001.184.7220苯甲醚0.000.000.000.000.000.00

15、0.000.001.014.04211-葵烯0.000.000.000.000.000.000.000.000.968.3822苯甲醛0.000.000.000.000.000.000.000.002.107.51232-壬酮0.000.000.000.000.000.000.000.000.863.43241-十二烯0.000.000.000.000.000.000.000.002.419.6425二氯乙烷-d40.000.000.000.000.000.000.000.00-結(jié)論HJ734-2014標(biāo)準(zhǔn)中認(rèn)為對于Tenax多孔聚合吸附劑，單個化合物的實(shí)驗室空白水平不應(yīng)大于7ng，說明本實(shí)驗

16、室具備按該標(biāo)準(zhǔn)分析空白的能力。注1:儀器測試記錄見報告附件材料。注2：代入標(biāo)準(zhǔn)曲線計算結(jié)果為負(fù)值時，均以0算，氘代替代物檢出限標(biāo)準(zhǔn)未給出。3.4檢出限的測定取7個全程序空白樣品，加標(biāo)濃度接近24種VOCs混標(biāo)中丙酮測定下限值濃度，加標(biāo)量為10ng，計算7次平行測定的標(biāo)準(zhǔn)偏差，乘以相應(yīng)的t值（n=7時，t=3.143）計算方法檢出限；測定下限為方法檢出限的4倍。按照標(biāo)準(zhǔn)方法，對7個全程序空白加標(biāo)樣品進(jìn)行分析，測量及處理結(jié)果見表7：表7檢出限測定數(shù)據(jù)及結(jié)果序號項目名稱樣品濃度/ng平均值/ng標(biāo)準(zhǔn)偏差t值檢出限/ng測定下限/ng12345671丙酮14.2014.8514.7115.2215.9

17、816.5316.9215.490.933.1432.9411.752異丙醇8.028.388.328.368.498.618.538.390.183.1430.562.263正己烷7.217.197.066.807.177.136.266.980.323.1431.003.994乙酸乙酯12.2212.4912.0811.3811.6211.8510.7311.770.543.1431.716.855六甲基二硅氧烷9.209.349.559.099.289.399.199.290.143.1430.441.766苯10.169.469.909.899.839.2010.299.820.353

18、.1431.104.407正庚烷10.4810.2410.9810.9011.0811.3910.7810.830.353.1431.114.4583-戊酮9.599.929.819.969.329.779.689.720.203.1430.642.569甲苯-d89.518.468.547.558.348.558.688.520.533.1431.676.6910甲苯13.8413.3112.7312.6112.9313.1912.6413.040.413.1431.295.1611環(huán)戊酮10.3710.109.939.4610.109.219.759.850.373.1431.174.70

19、12乙酸丁酯10.2011.1610.659.9710.1210.0810.3810.370.383.1431.204.8213乳酸乙酯11.0611.149.919.9710.219.909.9610.310.513.1431.606.4214丙二醇單甲醚乙酸酯9.0510.3910.129.769.999.0610.329.810.523.1431.636.5015乙苯10.5210.3210.669.129.869.0610.6210.020.643.1432.018.0416對/間二甲苯21.4219.3920.6019.5919.6118.7520.7020.010.863.1432

20、.6910.77172-庚酮9.629.619.249.539.519.499.399.480.123.1430.381.5318苯乙烯9.019.029.358.959.588.298.718.990.393.1431.214.8519鄰二甲苯11.2410.6210.3110.6210.5710.3411.2910.710.373.1431.164.6320苯甲醚8.899.209.438.389.128.818.458.900.363.1431.134.51211-葵烯8.338.828.858.999.258.919.308.920.303.1430.943.7522苯甲醛7.447.

21、668.427.087.108.068.697.780.593.1431.847.36232-壬酮8.429.009.199.308.698.768.718.870.293.1430.903.60241-十二烯7.709.269.859.969.569.328.999.230.703.1432.208.8025二氯乙烷-d411.7012.0312.2111.3612.0912.4111.3211.870.393.1431.234.92結(jié)論：檢出限測試結(jié)果符合標(biāo)準(zhǔn)規(guī)定的檢出限要求。注1:儀器測試記錄見報告附件材料。注2：計算公式及檢出限測試依據(jù)：環(huán)境監(jiān)測分析方法標(biāo)準(zhǔn)制修訂技術(shù)導(dǎo)則(HJ168-

22、2010)附錄A.1方法檢出限。3.5精密度測試參照HJ734-2014空白加標(biāo)計算精密度，因吸附管采樣樣品，實(shí)際采樣采樣一般為水平面平行采樣兩個，且使用熱脫附法僅能用于一次實(shí)驗分析，故報告本精密度測試選取6根現(xiàn)場空白吸附管，均注入2ul5mg/L標(biāo)準(zhǔn)溶液，通過標(biāo)氣加載裝置配成各組分含量為10ng的樣品管6個進(jìn)行測定(6個平行)，根據(jù)6個平行測定結(jié)果的標(biāo)準(zhǔn)偏差和平均值計算方法的相對標(biāo)準(zhǔn)偏差。表8精密度測試數(shù)據(jù)空白加標(biāo)樣品精密度測試數(shù)據(jù)項目名稱平行次數(shù)樣品測定結(jié)果/ng樣品測定平均值/ng標(biāo)準(zhǔn)偏差/ng相對標(biāo)準(zhǔn)偏差/%丙酮114.2015.250.795.17214.85314.71415.22

23、515.98616.53異丙醇18.028.360.182.2028.3838.3248.3658.4968.61正己烷17.217.090.141.9427.1937.0646.8057.1767.13乙酸乙酯112.2211.940.373.11212.49312.08411.38511.62611.85六甲基二硅氧烷19.209.310.141.5529.3439.5549.0959.2869.39苯110.169.740.323.2429.4639.9049.8959.8369.20正庚烷110.4810.840.383.52210.24310.98410.90511.08611.39

24、3-戊酮19.599.730.222.2529.9239.8149.9659.3269.77甲苯-d819.518.490.576.7128.4638.5447.5558.3468.55甲苯113.8413.100.413.12213.31312.73412.61512.93613.19環(huán)戊酮110.379.860.404.07210.1039.9349.46510.1069.21乙酸丁酯110.2010.360.413.99211.16310.6549.97510.12610.08乳酸乙酯111.0610.370.535.11211.1439.9149.97510.2169.90丙二醇單甲醚

25、乙酸酯19.059.730.515.27210.39310.1249.7659.9969.06乙苯110.529.920.646.45210.32310.6649.1259.8669.06對/間二甲苯121.4219.890.874.39219.39320.60419.59519.61618.752-庚酮19.629.500.121.3129.6139.2449.5359.5169.49苯乙烯19.019.030.404.4129.0239.3548.9559.5868.29鄰二甲苯111.2410.620.312.89210.62310.31410.62510.57610.34苯甲醚18.8

26、98.970.333.7229.2039.4348.3859.1268.811-葵烯18.338.860.273.1028.8238.8548.9959.2568.91苯甲醛17.447.630.496.4027.6638.4247.0857.1068.062-壬酮18.428.890.303.3929.0039.1949.3058.6968.761-十二烯17.709.280.758.0729.2639.8549.9659.5669.32二氯乙烷-d4111.7011.970.342.88212.03312.21411.36512.09612.41結(jié)論各物質(zhì)6個平行樣品測定結(jié)果的相對標(biāo)準(zhǔn)偏差

27、為1.38.07%，符合標(biāo)準(zhǔn)要求。注1:儀器測試記錄見報告附件材料，精密度測試與檢出限測試附件材料部分共用。3.6方法準(zhǔn)確度測試按照標(biāo)準(zhǔn)方法選取空白加標(biāo)樣品進(jìn)行加標(biāo)回收率測試，加標(biāo)量為10ng。取6個平行的樣品加標(biāo)測定，計算加標(biāo)回收率（準(zhǔn)確度）。表9樣品加標(biāo)回收率測試數(shù)據(jù)項目名稱平行次數(shù)加標(biāo)前測定值（ng）加標(biāo)后測定值（ng）加標(biāo)里（ng）回收率（）平均加標(biāo)回收率（%）丙酮異丙醇14.9914.2010.0092.1121.2220.0014.85148.534.0414.71106.745.7015.2295.250.0015.98159.864.0316.5312510.008.0210.

28、0080.283.6320.008.3883.830.008.3283.240.008.3683.650.008.4984.960.008.6186.110.007.2172.120.007.1971.930.007.0670.670.9340.006.806850.007.1771.7正己烷60.007.1310.0071.312.0012.22102.222.5512.4999.430.9812.08111107.0041.9111.3894.750.0011.62116.2乙酸乙酯60.0011.8510.00118.510.009.209220.009.3493.430.009.559

29、5.593.0840.009.0990.9六甲基二硅50.009.2892.8氧烷60.009.3910.0093.910.0010.16101.620.009.4694.630.009.909997.4040.009.8998.950.009.8398.3苯60.009.2010.0092正庚烷11.2210.4810.0092.696.3321.2010.2490.431.2010.9897.841.2010.909751.2111.0898.761.2411.39101.510.009.5995.920.009.9299.230.009.8198.1Q7OQ40.009.9699.69/

30、2850.009.3293.23-戊酮60.009.7710.0097.710.009.5195.120.008.4684.630.008.5485.40/1Q940.007.5575.584.9250.008.3483.4甲苯-d860.008.5510.0085.510.0013.84138.420.0013.31133.130.0012.73127.340.0012.61126.1131.0250.0012.93129.3甲苯60.0013.1910.00131.910.0010.37103.720.0010.1010130.009.9399.3QOg40.009.4694.698.62

31、50.0010.10101環(huán)戊酮60.009.2110.0092.1乙酸丁酯10.4810.2010.0097.294.3320.2511.16109.130.1810.65104.740.199.9797.853.4710.1266.561.0110.0890.710.0011.06110.620.0011.14111.430.009.9199.11HQ40.009.9799.7103.6550.0010.21102.1乳酸乙酯60.009.9010.009913.209.0558.520.0010.39103.933.1910.1269.343.199.7665.7/6.00丙二醇單甲53

32、.199.9968醚乙酸酯60.009.0610.0090.610.0010.52105.220.0010.32103.230.0010.66106.6QQ9Q40.009.1291.299.2350.009.8698.6乙苯60.009.0610.0090.610.0021.42214.220.0019.39193.930.0020.60206198.9340.0019.59195.9對/間二甲苯50.0019.6110.00196.160.0018.75187.511.369.6282.681.4021.369.6182.531.369.2478.841.369.5381.751.369.

33、5181.52-庚酮61.369.4910.0081.311.639.0173.821.639.0273.931.629.3577.373.5742.048.9569.151.589.5880苯乙烯61.568.2910.0067.310.0011.24112.420.0010.62106.230.0010.31103.1106.1740.0010.62106.250.0010.57105.7鄰二甲苯60.0010.3410.00103.410.008.8988.920.009.209230.009.4394.389.7240.008.3883.850.009.1291.2苯甲醚60.008.

34、8110.0088.110.008.3349.220.008.8253.582.9030.008.8554.41-葵烯40.008.9910.0055.850.009.2558.460.008.915510.007.4474.420.007.6676.630.008.4284.2%9740.007.0870.8/O.Z/50.007.1071苯甲醛60.008.0610.0080.610.008.4241.320.009.0047.430.009.1943.9QQQ240.009.3044.9OO.VJ50.008.6944.42-壬酮60.008.7610.0045.110.007.7042

35、.120.009.2657.930.009.856340.009.9664.57厶/D50.009.5660.71-十二烯60.009.3210.0058.510.0011.7011720.0012.03120.330.0012.21122.111QQ40.0011.36113.6iiV.0/50.0012.09120.9二氯乙烷-d460.0012.4110.00124.1結(jié)論:各物質(zhì)6個平行樣品平均加標(biāo)回收率為70.93121.22%，符合標(biāo)準(zhǔn)方法的準(zhǔn)確度控制要求。3.7替代物采樣分析及穿透實(shí)驗替代物采樣時，采樣前在老化好的吸附管中通過標(biāo)氣加載裝置加入lOOng的氘代替代物標(biāo)準(zhǔn)溶液，并在其

36、中一根吸附采樣管后串聯(lián)一根吸附采樣管。分析結(jié)果如下表10。表10替代物采樣分析及穿透實(shí)驗數(shù)據(jù)化合物編號化合物名稱現(xiàn)場空白/ng樣品/ng樣品平行/ng樣品穿透/ng樣品平均值/ng1丙酮0.560.320.130.410.232異丙醇0.003.544.490.004.023正己烷0.000.000.000.000.004乙酸乙酯0.230.900.620.540.765六甲基二硅氧烷0.000.000.000.000.006苯0.000.000.000.000.007正庚烷0.001.421.410.001.4183-戊酮0.000.000.000.000.009甲苯-d80.0088.23

37、85.4789.5086.8510甲苯0.211.371.390.401.3811環(huán)戊酮0.004.254.450.004.3512乙酸丁酯0.243.583.490.343.5313乳酸乙酯0.000.000.000.000.0014丙二醇單甲醚乙酸酯0.000.000.000.000.0015乙苯0.000.150.160.000.1516對/間二甲苯0.000.000.000.000.00172-庚酮0.000.000.000.000.0018苯乙烯0.001.621.720.191.67穿透效率/%9.89是否發(fā)生穿透樣品回收率/%以甲苯-d8算以二氯乙烷-d4算平均值86.8573.

38、7580.3019鄰二甲苯0.000.000.000.000.0020苯甲醚0.000.000.000.000.00211-葵烯0.000.000.000.000.0022苯甲醛0.000.000.000.000.00232-壬酮0.000.000.000.000.00241-十二烯0.000.000.000.000.0025二氯乙烷-d40.0076.9270.5873.8073.75TVOCs1.2317.1317.861.8817.50結(jié)論：回收率符合回收率要求范圍；穿透效率9.89%,目標(biāo)化合物TVOCs總量小于規(guī)定值10%，米樣樣品未穿透。注1:儀器測試記錄見報告附件材料。3.8質(zhì)控

39、樣測定通過標(biāo)氣加載裝置加入2ul50mg/L的混標(biāo)溶液制備標(biāo)準(zhǔn)吸附管，配制成質(zhì)控樣品。由于部分揮發(fā)性有機(jī)物存在吸附效率等的差異,標(biāo)準(zhǔn)曲線計算后的測定值換算后部分結(jié)果偏離標(biāo)稱值范圍，質(zhì)控樣測定值結(jié)果總體判定為合格。表11質(zhì)控樣品測試數(shù)據(jù)序號化合物名稱保留時間/min質(zhì)控樣測試結(jié)果/ng（進(jìn)樣量2ul）質(zhì)控測定值/mg/L稀釋倍數(shù)測定值/mg/L有證標(biāo)準(zhǔn)物質(zhì)標(biāo)稱值/mg/LZK160819-01ZK160819-02平均值1丙酮8.1699.81100.0099.9049.9521401998.08198532.262異丙醇8.19197.5796.3796.9748.48485401939.39198425.53正己烷11.848107.2897.2