便携式GC-MS法快速测定固定污染源废气中的VOCs

采用便携式GC-MS法快速测定固定污染源废气中VOCs,32种VOCs在2×10~(-7)~1×10~(-6)范围内线性良好,方法检出限为2×10~(-9)~1×10~(-8),标准气体样品6次测定结果的RSD为1.9%~19.1%,环境空气样品的加标回收率为66.2%~116%。在实际现场监测固定污染源中VOCs时,使用速查(Survey)功能可初步判断样品浓度,确定稀释倍数。比对试验结果表明,气袋和玻璃注射器采样法对VOCs测定结果无显著性差异。     

Pollution characteristics of 23 veterinary antibiotics in livestock manure and manure-amended soils in Jiangsu province,China

The aim of this study was to investigate the pollution characteristics of typical veterinary antibiotics in manure and soil of livestock farms in Jiangsu province. This investigation employed solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). A total of 53 manure and 50 amended soil samples from 16 livestock farms in Jiangsu province were collected for analysis. In the manure samples, the highest detected frequencies and concentrations were those of tetracyclines (TCs, 54.1 ± 5775.6 μgkg^?1), followed by fluoroquinolones (FQs, 8.4 ± 435.6 μgkg^?1), sulphonamides (SAs, 3.2 ± 5.2 μgkg^?1) and macrolides (MACs, 0.4 ± 110.5 μgkg^?1). Statistical analysis was used to illuminate the pollution characteristics of 23 veterinary antibiotics for various animal types and different regions in Jiangsu province. The results showed that the pollution level in cow manure was relatively lower compared with pig and chicken manure due to the relative restriction of medication. Furthermore, contamination was serious in amended soil from chicken farms. The pollution level in manure among different regions was higher to the south and north compared with the centre of the region. The same outcome was found for soil. Antibiotic residues in organic fertilizer were also investigated in this study. We found that although the detected concentration was lower in organic fertilizer than in fresh manure, detection frequencies (10–90%) were high, especially for roxithromycin (90%) in MACs (30–90%). This finding suggests attention should be paid to the pollution levels in organic fertilizer. This study is the first extensive investigation of the occurrence and distribution of many kinds of typical veterinary antibiotics in manure and soil from livestock farms of Jiangsu province. This investigation systematically assesses veterinary antibiotics usage and related emissions in southeast China.     

固相萃取-气质联用法测定固体废物浸出液中的二硝基苯

建立了一种利用固相萃取法对固体废物浸出液(TCLP)中二硝基苯进行萃取,DB-5石英毛细管柱(30 m×0.25 mm×0.25μm)进行分离,质谱检测器检测二硝基苯的方法。方法在0.002 0~0.020 0 mg/L之间线性关系良好,二硝基苯三种同分异构体的检出限均为0.5μg/L,模拟样品加标回收率为93%~96%,RSD≤2%;实际固体废物样品测定的加标回收率为95%~98%。     

超临界二氧化碳萃取－GC／MS测定土壤中的多环芳烃

本文开发了一种采用超临界二氧化碳萃取土壤中多环芳烃、不须经过纯化步骤,直接可用于ＧＣ／ＭＳ分析的简便、高效的方法。本实验中超临界革取的流体是二氧化碳,改善剂是５％的二氯甲烷／甲醇,萃取温度为１２０℃、压力为３４ＭＰａ。ＧＣ／ＭＳ分析时除了采用外标外,还加入了６种同位素ＰＡＨｓ内标以校正各段ＰＡＨｓ的响应因子。采用本方法成功地测定了我国未开垦森林土壤中的ＰＡＨｓ。     

吹扫捕集与气相色谱-质谱联用测定饮用水和地表水中挥发性有机污染物

报道了Trap I(VOCARB 4000)柱捕集水中挥发性有机污染物的性能和条件,建立了吹扫捕集和气相色谱-质谱联用测定饮用水和地表水样中25种挥发性有机污染物的分析方法.水样的加标回收率在90%～110%之间,最低检测限在0.04～0.85μg/L之间,20μg/L的挥发性有机物标准溶液经重复6次测定,其相对标准偏差基本小于5.0%.该方法已成功地运用于饮用水和地表水中挥发性有机污染物的测定,结果令人满意.     

海水中有机污染物的气相色谱－质谱法鉴定

本文采用一种简便的连续萃取装置．对海水中痕量有机物进行富集,大量的海水被萃取后,萃取物经干燥浓缩在毛细管气相色谱上进行了分离,并用质谱－计算机自动检索装置进行了定性鉴定,共确定出３６种组分。本方法的检测限为辛烷１０ｐｐｔ。     

固相萃取-气质联机测定水中嗅味物质2-甲基异茨醇和土霉素

分别利用固相萃取剂XAD-2树脂和C18SEP柱富集,二氯甲烷洗脱,固相萃取装置浓缩,通过气质联机(GC/MS)测定了水中土霉化合物MIB和Geosmin。该方法重现性好,相对标准偏差5.4%~7.0%,回收率80%~92%,MIB和Geosmin检出限分别为5ng/L和2ng/L。两种固相萃取剂对MIB和Geosmin吸附效率相当,吸附效率不受嗅味物质浓度影响,但当水溶液中其它有机质增多时,C18SPE的回收率明显下降。利用该方法对不同培养时间的放线菌代谢产物进行了测定,培养25天后代谢产物MIB和Geosmin的浓度达到200ng/L和130ng/L。     

微波萃取-气相色谱/质谱法测定土壤中的有机氯农药

通过微波萃取提取土壤中的有机氯农药,萃取溶液经浓硫酸脱色、佛罗里硅土柱净化,最后用气相色谱/质谱法分析.以石英砂为基体进行加标回收测定,有机氯农药的回收率在75.5%～103%之间,检出限为0.01μg/kg.     

乌鲁木齐市新市区大气气溶胶中多环芳烃的GC/MS分析

采用气相色谱-质谱联用技术(GC/MS)分析测定了乌鲁木齐市新市区的大气气溶胶样品16种EPA优控多环芳烃(PAHs)的含量。通过索氏提取气溶胶样品,抽提物经硅胶层析柱分离,使用16种多环芳烃混合标准样品绘制标准曲线,以外标法对PAHs进行定量分析,并根据所得数据浅析了多环芳烃污染来源。结果表明,乌鲁木齐市新市区大气中由于汽车尾气排放和煤的燃烧造成的多环芳烃污染均存在。     

环境空气中痕量挥发性有机硫监测分析方法研究

采用预浓缩系统与GC MS联用,建立了环境空气中痕量挥发性有机硫的分析方法,该法用苏玛罐或Tedlar袋采集空气样品在预浓缩系统中经液氮于-160℃冷冻浓缩后,进入GC MS进行分析。甲硫醇、乙硫醇、甲硫醚、乙硫醚、二甲二硫的最低检出限分别为2 0、1 0、1 0、1 0、0 5μg m3。经6次的重复测定,其相对标准偏差小于9 0%。该方法已用于环境空气的测定,取得了令人满意的结果。