超声波提取-气相色谱法测定土壤中残留六六六和滴滴涕

采用气相色谱法毛细管色谱柱分离、电子捕获检测器检测土壤中残留的六六六和滴滴涕含量。取风干过筛的土壤样品，用丙酮、石油醚（1：）浸泡，超声波提取，浸泡液经浓硫酸净化后进样测定。当土壤样品取样量为10g时，方法检测限α-六六六，γ-六六六为0.001mg/kg,β-六六六、δ-六六六、op'-DDT和pp'-DDT为0.004mg/kg,pp'-DDE,pp'-DDD为0.002mg/kg。加标回收率在77%-100%之间，相对标准偏差为2.5%-8.5%。方法简便、灵敏。     

运用热脱附/GC/MS分析研究室内空气中TVOC浓度及种类分布

利用热脱附/GC/MS联用技术定性、定量(半定量)分析了多组有代表性的室内空气样品。结果表明,室内空气挥发性有机气体的主要成分是苯系物、烃类、醛酮类、酯类等;装修后3个月内的家居室内空气中的苯25%超标,甲苯58%超标,二甲苯79%超标,TVOC 100%超标;一年后,仅TVOC还有11%的超标。办公室情况类似。     

Column experiments to study nonlinear removal of bacteriophages by passage through saturated dune sand

In a recent field study on dune recharge, bacteriophages MS2 and PRD1 were found to be removed 3 log10 over the first 2.4 m and only 5 log10 over the next 27 m. To understand the causes of this nonlinear removal, column experiments were carried out under conditions similar to the field: same recharge water, temperature (5 +/- 3 degrees C) and pore water velocity (1.5 m day(-1)). Soil samples were taken along a streamline between the recharge canal and the first monitoring well. Bacteriophage phiX174 was included for comparison. The high initial removal in the field was found not to be due to heterogeneity of phage suspensions but to soil heterogeneity. Phage removal rates correlated strongly positively with soil organic carbon content, and relatively strongly positively with silt content and the presence of ferric oxyhydroxides. Soil organic carbon content, silt content and the presence of ferric oxyhydroxides were found to decrease exponentially with travel distance. Removal rates of phiX174 were found to be 3-10 times higher than those of MS2 and PRD1 due to the lower electrostatic repulsion that the less negatively charged phiX174 experiences. It is suggested that the high initial removal in the field is due to the presence of favorable sites for attachment formed by ferric oxyhydroxides that decrease exponentially with travel distance. Similar removal rates may be found at both laboratory and field scale. However, due to local variations at field scale detailed knowledge on soil heterogeneity may be needed to enable a reliable prediction of removal.     

A wood preservative metabolite in river water

- A previously unknown pollutant in river water was identified to be 2-mercaptobenzothiazole (2-MBT) by interpretation and simulation of its GC/LRMS spectrum. Further GC/HRMS measurement of the isotope composition of the molecular ion verified this structure. 2-MBT is a well-known agent for corrosion inhibition and a stable metabolite of several other benzothiazoles. The present 2-MBT trace was most probably a metabolite of the wood preservative TCMTB which leaked from an upstream sawmill. The metabolite had been detected earlier in urine of the sawmill workers, but now was identified in the recipient water environment for the first time.     

Detection of indoor PCB contamination by thermal desorption of dust. A rapid screening method?

Although PCB in caulking materials has been forbidden for many years in most of Europe, including Denmark, there has been continued interest to measure PCB levels in the air of contaminated buildings and blood of the occupants (Mengon and Schlatter 1993, Fromme et al. 1996, Ewers et al. 1998, Currado and Harrad 1998, Gabrio et al. 2000). The relatively low priority for investigations of this contamination is probably due to the small quantities inhaled compared to exposure via food, and the rapid metabolism of the most volatile congeners demonstrated by low concentrations of all congeners in the blood of exposed persons (Ewers et al. 1998, Gabrio et al. 2000). There is, however, evidence that PCB containing caulking materials have been used even during the '90s (Fromme et al. 1996). In Denmark, it is estimated that 75 t PCB is still in buildings (Organization of Sealant Branch's Manufacturers and Distributors 2000). During an investigation of dust from buildings with excessive microbial growth (including 35 rooms from 9 buildings), the analysis of semivolatile compounds by thermal desorption-GC/MS of samples from a single building surprisingly revealed large amounts of PCBs containing 3, 4 and 5 chlorine atoms, 10-20 times the amounts found in samples from other buildings. Extraction of the dust by SFE followed by GC/ECD analysis for 12 PCB congeners showed that there was approximately 20 times the total PCB concentrations in dust from the polluted building compared to the levels in the other buildings. Subsequent headspace analysis of caulking material from the polluted building revealed this to be the source. Shelf dust functions as a passive sampling medium and, thus, can be used as a screening method to detect PCB and other semivolatile pollution indoors.     

气相色谱法测定海洋生物体中有机磷农药残留

建立了气相色谱法测定海洋生物体中乐果、甲基对硫磷和马拉硫磷残留量的方法.海洋生物体中有机磷农药残留用丙酮经超声波提取、弗罗里硅土净化后,用DB-1701毛细管色谱柱分离,火焰光度检测器(FPD)直接测定.在鱼、虾、贝类等样品中添加浓度为0.008×10-6、0.08 ×10-6和0.8×10-6的回收率(n=11)范围为72.6%～112%,相对标准偏差(RSD)为5.7%～9.0%,乐果、甲基对硫磷和马拉硫磷的检出限分别为0.002×10-6、0.002×10-6和0.004×10-6.本方法具有灵敏、快速、简便等特点,能满足海洋生物体中有机磷农残的监测要求.     

Analysis of vapor phase organics in air of Beijing, Langfang and Tianjin by capillary GC and GC/MS

The vapor phase organics (VPOs) in the air of Beijing, Langfang and Tianjin were detected by a capillary gas chromatography and GC/MS during the winter and the summer separately. The tentatively identified compounds include alkanes, cyclic hydrocarbons, alkenes, aromatics, acids, alcohols, aldehydes, ketones, esters, halocarbons and so on. The numbers of VPOs found are 118 in Beijing, 83 in Lang-fang and 65 in Tianjin in the winter, and 56, 39 and 72 in the summer respectively. Based on the data of some representative compounds determined quantitatively by GC and GC/MS, a profile of organic pollution in the air of the three cities is presented.     

用毛细管色谱法和同位素技术研究呋喃丹及其有毒代谢物在棉籽和土壤中的残留

使用OV-101玻璃毛细管柱气相色谱法测定棉籽和土壤中的呋哺丹和3-羟基呋喃丹,减少了农药在柱上的吸附和分解,分开了农药与植物中的干扰物质,减少了样本的前处理步骤,其回收率分别约为80％,变异系数小于20％。以~(14)C标记呋喃丹测定各前处理步骤的损失率,表明农药的损失主要是由于酸解及固体物质的吸附。两年三地田间试验的结果说明,按照推荐药量在棉田使用呋喃丹,棉田和土壤中的残留均低于检测限。     

防虫蛀织物中有机杀虫剂残留的GC／MS测定

织物试样由丙酮－正己烷混合溶剂浸渍后进行超声提取，提取液经Celite层析柱净化。40℃为转蒸发浓缩、定容，由GC／MS测定试样中的DCB、Naphthalene,PCP及Permethrin含量，本方法适合毛织物中防虫蚊整理剂、防霉剂及驱虫制剂残留的定性量分析，方法在目标化合物的检测限（LOQs)D0.1-0.5Mg/Kg之范围内，平均回收率介于89.2-94.6%之间，相对标准偏差为2.3-8.1%。     

质谱/质谱法快速检出国产五氯酚中的痕量剧毒杂质—四氯二苯并呋喃

多氯二苯并二(口恶)(口英)(PCDD)及多氯二苯并呋喃(PCDF)是化学结构相象的二组剧毒化合物.1976年意大利的Seveso发生污染事件后,它们对人体的伤害及生态环境的影响受到了世界上环境学家和生态学家的广泛重视.PCDD和PCDF各有75个和135个异构体,其毒性差别可达1000—10000倍,其中的十个异构体(包括2,3,7,8-四氯二苯并二(口恶)(口英),TCDD)已被列入对动物具有最大毒性的一批天然和人为毒物之内,它们会引起肝损伤、氯痤疮、神经系统损伤及致突变、致畸、致癌.急性皮肤毒性的LD_(50)值为1—100μg/kg,对猴子的LD_(50)值,TCDD是30—70μg/kg,TCDF是1000μg/kg,Kara-sek建议人体(50kg体重)对TCDD和TCDF的允许暴露水平是2 pg/day(致癌性).这类化合物具有脂溶性,易被土壤吸附,在自然环境中代谢降解速度缓慢,从而增加了环境