共查询到19条相似文献,搜索用时 203 毫秒
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G C/MS法测定环境空气中痕量POPs类有机氯农药及降解产物 总被引:4,自引:0,他引:4
采用快速溶剂萃取-氟罗里硅土柱净化-气相色谱/质谱联用法测定环境空气中POPs类有机氯农药及其降解产物.艾氏剂、狄氏剂、异狄氏剂、六六六、滴滴涕,七氯、氯丹、灭蚁灵及其降解产物的检出限为2.0 ng~4.6 ng,空白加标回收率为62.1%~118%,RSD为6.8%~15.2%. 相似文献
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建立了用加速溶剂萃取法(ASE)提取、气相色谱-串联质谱法分析土壤中20种有机氯农药的方法。用正己烷和丙酮(1∶1,V/V)的混合溶剂为提取剂,萃取温度100℃,压力1 500 psi,静态提取10 min,循环提取2次,提取液经石墨化碳黑固相萃取柱净化,浓缩后进行GC-MS/MS测定,外标法定量。试验结果表明,采用串联质谱多反应监测模式,降低了背景干扰,当取5 g土壤时,有机氯农药的检出限在0.1~3.0μg/kg之间,低浓度水平(8μg/kg)的基体加标回收率为70.3%~134%,相对标准偏差〈23%。测定方法背景干扰低,灵敏度高,适合土壤中20种有机氯农药残留的同时测定。 相似文献
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王英健 《环境监测管理与技术》2010,22(2):55-57
以正己烷/丙酮混合溶剂(体积比为1∶1)为提取剂,采用Florisil柱净化、气相色谱电子捕获检测器测定土壤中菊酯类农药残留,优化了提取条件。4种菊酯类农药在0.010 mg/L~1.00 mg/L范围内线性良好,方法检出限为0.005 mg/L~0.010 mg/L,甲氰菊酯回收率为85.2%~103%,RSD为2.3%~5.4%;氯氰菊酯回收率为80.5%~103%,RSD为2.8%~6.7%;氰戊菊酯回收率为80.2%~103%,RSD为2.3%~6.0%;溴氰菊酯回收率为80.8%~103%,RSD为2.4%~6.2%。 相似文献
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固相萃取-GC/MS法测定水中有机氯农药 总被引:10,自引:2,他引:8
建立了固相萃取-气相色谱/质谱联用测定水中痕量六六六、滴滴涕和环氧七氯的方法。采用C18固相萃取柱富集水样,二氯甲烷/丙酮混合溶剂洗脱,加入菲-d10作为内标,利用气相色谱/质谱联用仪选择离子监测模式检测,内标法定量,定性、定量准确,线性响应良好,干扰小,按采样1 L计算,方法检出限为4.26ng/L~19、2ng/L,RSD在0、4%-6、3%之间,平均加标回收率在77.7%~118%之间,实际样品测定结果表明方法能满足环境水体中痕量有机氯农药的监测要求。 相似文献
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采用自动净化-高分辨气相色谱/高分辨质谱(HRGC/HRMS)测定废气中的17种2,3,7,8位取代的多氯代二噁英和呋喃(PCDD/Fs)。废气样品经索氏提取,DEXTech系统全自动净化,浓缩和定容后,以HRGC/HRMS对废气样品中的PCDD/Fs进行了定性和定量分析。结果表明,17种二噁英和呋喃采样内标平均回收率为93%~99%,提取内标平均回收率为80%~97%;17种二噁英和呋喃自动净化实测结果与手工净化测试结果基本一致。该方法不但满足相关国家标准要求,还极大提高了样品的净化速度,减少人体对有机试剂的暴露。 相似文献
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多环芳烃测定中净化方法的研究 总被引:2,自引:1,他引:1
对多环芳烃测定中的净化方法进行研究,为了选出最佳净化柱,在一定条件下分别采用硅胶LC-Si、弗罗里LC-Florisil和C18固相萃取净化柱对一定浓度的多环芳烃标准溶液进行净化,测定吸附后流出液多环芳烃浓度,计算吸附率;测定洗脱后流出液多环芳烃浓度,计算洗脱率。测定结果为硅胶、弗罗里和C18固相萃取净化柱对多环芳烃的吸附率分别在87.1%~100%,99.5%~100%和96.6%~100%之间,洗脱率分别在0~106%,78.7%.109%和79.0%~115%之间。结果表明,GC/MS内标法测定样品中多环芳烃使用最理想的净化柱为弗罗里净化小柱,其次为C18净化小柱,最后为硅胶净化小柱。 相似文献
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超声波萃取-GC/MS法测定土壤中多氯联苯 总被引:3,自引:0,他引:3
建立了超声波萃取、氟罗里硅土柱净化、气相色谱/质谱联用选择离子扫描模式测定土壤样品中多氯联苯Arochlor系列的方法.方法线性良好,灵敏度高,RSD为9.5%~12.2%,加标回收率为65.0%~105%,标准土壤样品的测定结果也符合要求. 相似文献
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超声波萃取-气相色谱/质谱法测定土壤中15种Pops类有机氯农药 总被引:2,自引:1,他引:1
用探头式超声波萃取仪、己烷/丙酮混合溶剂提取土壤中的15种Pops类有机氯农药(包括六氯苯、七氯、六六六、氯丹、艾氏剂、狄氏剂、异狄氏剂、灭蚁灵、滴滴涕),萃取溶液经氟罗里硅土柱净化、氮吹浓缩,用气相色谱/质谱仪(GC-MS)进行测定。方法检出限0.4~1.4μg/kg,空白样品有机氯农药加标回收率为52.8%~118%、有机氯标记替代物回收率为71.0%~122%,RSD为6.8%~16.5%。 相似文献
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Rynö M Rantanen L Papaioannou E Konstandopoulos AG Koskentalo T Savela K 《Journal of environmental monitoring : JEM》2006,8(4):488-493
In order to characterize and compare the chemical composition of diesel particulate matter and ambient air samples collected on filters, different extraction procedures were tested and their extraction efficiencies and recoveries determined. This study is an evaluation of extraction methods using the standard 16 EPA PAHs with HPLC fluorescence analysis. Including LC analysis also GC and MS methods for the determination of PAHs can be used. Soxhlet extraction was compared with ultrasonic agitation and pressurized fluid extraction (PFE) using three solvents to extract PAHs from diesel exhaust and urban air particulates. The selected PAH compounds of soluble organic fractions were analyzed by HPLC with a multiple wavelength shift fluorescence detector. The EPA standard mixture of 16 PAH compounds was used as a standard to identify and quantify diesel exhaust-derived PAHs. The most effective extraction method of those tested was pressurized fluid extraction using dichloromethane as a solvent. 相似文献
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微波萃取-气相色谱法测定土壤中有机氯残留 总被引:3,自引:0,他引:3
采用微波萃取-硅镁吸附剂净化-气相色谱法测定土壤中有机氯农药,优化了试验条件。方法线性良好,8种有机氯农药的检出限为0.09ng/g-0.62ng/g,样品测定的RSD为2.6%-13.2%,基质加标平均回收率为93.7%-112%,质控样的测定结果与参考值相吻合。 相似文献
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A study of polycyclic aromatic hydrocarbons (PAHs) pollution in roadside soil was conducted at a developing city locations of Jalandhar (Punjab), India in winter season to ascertain the contamination levels and their distribution behavior in roadside soil. PAHs concentration level of ten locations was measured at 1, 2, and 3 m distances from roadside soil covering all the major traffic intercepts within a city. Samples were extracted in acetone and dichloromethane (1:1) using soxhlet extraction. The extracts were filtered on a silica gel micro column to remove impurities and eluate was subjected to GC-FID. The total average PAHs concentration (city average) was found to be 4.04 μg g(-1), whereas the concentration of 16 individual PAHs was found to vary between 0.008 and 28.4 μg g(-1). The average concentration of noncarcinogenic and carcinogenic PAHs in all the samples was 2.17 and 6.41 μg g(-1) (ratio 1:2.95). The concentration of five ringed PAHs was found to be 45% to 60%, whereas two ringed PAHs were found to be in the range from 0.28% to 0.56% in all most all locations. The average highest PAHs concentration for any individual location was found as 12.23 μg g(-1) at DAV Chowk at 1 m distance and minimum concentration was 0.98 μg g(-1) at Maqsuda Chowk at 1 m distance from roadside. DiB (ah) A was the individual PAHs found in highest concentration in all the intercepts ranging between 1.26 and 28 μg g(-1). At most of the city intercepts, total carcinogenic PAHs concentration was found to range from 60% to 80% in comparison to noncarcinogenic PAHs (20%-40%) at most of the intercepts. The pollution level our study was compared with other cities of India/worldwide. 相似文献
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Chye Peng Ong Hian Kee Lee Sam Fong Yau Li 《Environmental monitoring and assessment》1991,19(1-3):63-71
A rapid and simple method is described for the quantitative determination of polycyclic aromatic hydrocarbons in aqueous environmental samples. A microscale on-line supercritical fluid extraction-supercritical fluid chromatography system using carbon dioxide is employed. The extract is analysed using capillary supercritical fluid chromatography with UV detection. Detection was carried out at 254 nm. An extraction efficiency of as high as 91% was obtained for the PAHs. 相似文献
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Determination of Polycyclic Aromatic Hydrocarbons in Rougan, a Traditional Chinese Barbecued Food, by Capillary Gas Chromatography 总被引:1,自引:0,他引:1
J. Wu M. K. Wong H. K. Lee C. Y. Shi C. N. Ong 《Environmental monitoring and assessment》1997,44(1-3):577-585
Several polycyclic aromatic hydrocarbons (PAHs), including those which are carcinogenic, have been detected in rougan, a traditional Chinese barbecued pork dish. The food samples were cleaned up by caustic digestion, solvent extraction, liquid-liquid partition, and column chromatography. The determination was carried out using capillary gas-chromatography with a flame ionization detector. A 25-m HP-1 capillary column was used. Fluorene, phenanthrene, anthracene, benzo[a]anthracene, chrysene and benzo[k]fluoranthene were detected in three of the five samples within the range of 3-17 ng/g. Fluoranthene and pyrene were detected in only two of the samples at similar levels. Two potent carcinogenic compounds, benzo[a]pyrene and benzo[b,j,k]fluoranthene, were not detected in any of the samples. No detectable PAHs have been found in meat cooked without the direct contact of food with flame and smoke. In barbecuing over an open charcoal fire, animal fat and juices dripping onto the open fire probably enhanced the formation of PAHs. 相似文献
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建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1~100 ng/mL(BDE-209为10~1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004~0.1 ng/g,方法回收率为75%~110%,方法精密度为2.4%~15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。 相似文献