阻抑动力学测定痕量砷（Ⅲ）的研究

在硫酸介质中，痕量Ａｓ（Ⅲ）能阻抑溴酸钾、镍化钾和锆试剂之间的褪色反应，研究了阻抑褪色反应的最佳佳实验条件，建立了测定初量Ａｓ（Ⅲ）的方法，本方法的最低检测限为３．６×１０＾－５μｇ·ｍｌ＾－１，测定范围为０．０－１．０μｇ·２５ｍｌ＾－１，用于测定工业废水中的Ａｓ（Ⅲ），获得了满意的结果。     

3,3''''-二氯联苯胺盐酸盐合成工业酸性废水中污染物的高效液相色谱法测定

利用高效液相色谱法测定了３,３’－二氯联苯胺盐酸盐合成工业酸性废水中的污染物,色谱柱为Ｚｏｒｂａｘ－ＯＤＳ,流动相为乙腈－水(７０/３０,Ｖ/Ｖ),流速为０．５ｍｌ·ｍｉｎ－１,柱温４２℃,检测波长２８０ｎｍ．建立了废水水样预处理方法,主要污染物回收率在９０%以上．酸性废水中污染物包括３,３'－二氯联苯胺盐酸盐、邻氯苯胺等．     

环境样品中非邻位取代共平面多氯联苯的测定

本文对测定实际环境样品中痕量非邻位取代共平面多氯联苯的方法进行了研究。样品萃取，净化后，经活性碳性层析分离，利用ＧＣ－ＥＣＤ毛细管柱双柱定性，外标法进行定量，测定了土壤和鱼肌肉中μｇ·ｋｇ＾－１数量级的３，３‘，４，４’－四氯联苯及ｎｇ·ｇｋｇ＾－１数量级的３，３‘，４’，５－五氯联苯。     

PT—C18色谱预柱流动注射在线富集原子吸收测定环境样品中的铅

本文采用ＰＴ－Ｃ１８色谱预处理柱，以８－羟基喹啉为螯合剂，流动注射在线分离富集与原子吸收联机，成功地测定了环境样品中的铅。１ｍｉｎ富集（４．２ｍｌ）的检出限为７．５μｇ１＾－１，相对标准偏差１．７％。     

土壤中结合态苯氧羧酸类除草剂的测定

利用超临界ＣＯ２流体萃取的方法提取２甲４氯(ＭＣＰＡ),２,４－Ｄ和除草醚在三种土壤中的结合残留．结果表明,在培养２００ｄ的时间内,ＭＣＰＡ的结合残留量为１．０ｌ－５．１２ｍｇ·ｋｇ－１,占添加总量的２．０－１０．１%;２,４－Ｄ的结合残留量为０．２４－２．６５ｍｇ·ｋｇ－１,占添加总量的０．５－５．３%;除草醚的结合残留量为６．５３－１９．３０ｍｇ·ｋｇ－１,占添加总邑的１２．９—３８．２%．农药结合态与游离态含量的比值随时间的延长而增加．     

高效液相色谱法分析水中痕量多环芳烃

本文利用高效液相色谱法测定水中痕量多环芳烃（ＰＡＨｓ）。以二氯甲烷作溶剂,超声提取水中痕量ＰＡＨｓ;甲醇、水作流动相,梯度淋洗,用程序可变波长荧光检测器测定。ＰＨＡｓ浓度为０．００７＝０．６μｇ·ｍｌ＾－１范围时,线性相关系数均在０．９９９９以上;峰高、峰面积的相对标准偏差（ｎ＝１０）分别为１．０１－１．８５％,２．００－３．９４％;检测限（Ｓ／Ｎ＝２）为３．１－２３．０ｐｇ;实际水样的加标回收率     

高效液相色谱法测定水环境中壬基酚聚氧乙烯醚及其生物降解产物

应用固相萃取－高效液相色谱法调查了嘉陵江和长江重庆段的壬基酚聚氧乙烯醚(ＮＰｎＥＯ,ｎ＞３)的污染状况．在四月份,长江的Ａ,Ｂ和Ｃ,嘉陵江的Ｄ和Ｅ采样点都测定出了ＮＰｎＥＯ(ｎ＞３)．长江上游Ａ点的浓度最高,为３７．２８μｇ·ｌ－１,嘉陵江的下游Ｄ点的总浓度最低,为７．２１μｇ·ｌ－１．七月的水样中仅在Ａ,Ｄ,Ｅ点检测出ＮＰｎＥＯ(ｎ≥３),其总浓度最高为１．９９μｇ·ｌ－１．但其分解产物ＮＰ的浓度比四月份高．     

用SPE法萃取,GC／NPD检测全血中氯氮平药物

本文报道了用固相萃取技术（ＳＰＥ）富集分离全血中的氯氮平药物，采用气相色谱氮磷检测器（ＧＣ／ＮＰＤ）分析方法凤ＳＫＦ５２５Ａ为内标物，在１ｍｌ全血中加入２．０μｇ药物，回收率为９０．０％，ＲＳＤ为７．９５％，血中最低检出浓度为５８ｎｇ．ｍｌ＾－１，该方法具有简单、快速、准确、１灵敏的优点。     

酸性高锰酸盐指数(Imn)的测定

１ 监测条件的选择和控制高锰酸钾标准溶液 按《水和废水监测分析方法》(三版)要求高锰酸钾浓度准确到０．０１ｍｏｌ·１－１,实际调配较难,只要在标定时,消耗的高锰酸钾体积在１０±０．５ｍｌ范围内即可．滴定、标定 高锰酸钾与草酸钠反应,合适温度为６０－８０℃,这就促使滴定、标定要迅速,时间要短．取出处理后的样品,先观其颜色,如仍为紫红色,那么滴定时消耗的高锰酸钾常在５ｍｌ以下,如为棕红色,则滴定时消耗的高锰酸钾常在７ｍｌ以上．知道所需高锰酸钾的体积,就能控制滴定速度     

环境基质中药物残留的固相提取与分析

废水流出物常常不可避免地进入地表水和用于饮用水资源的含水层．因废水再循环常常进入饮用水层,各种废水中的污染物最终会污染饮用水．以往环保部门一直比较注重农药和工业污染物,但最近的研究发现:废水流出物中的某些药物残留已达到了相当令人关注(１μｇ·１－１即ｐｐｂ)的程度．传统的分析技术(如液液萃取和ＧＣ/ＭＳ) 对极性较弱的化合物(ＰＣＢｓ和许多农药)比较有效,但对于极性相对较强的药物污染物而言,固相提取(ＳＰＥ)与ＬＣ/ＭＳ技术更适合于样品提取分析。     

水中痕量亚当氏剂和二苯胺的固相微萃取方法研究

研究了固相微萃取(SPME)-高效液相色谱(HPLC)测定水样中痕量亚当氏剂和二苯胺的分析方法.对SPME的条件如萃取纤维、萃取时间、萃取温度、离子强度、解吸方式、解吸溶剂、解吸时间进行了优化,并用于地下水等实际水样的分析.SPME优化的条件为:选用60μmPDMS/DVB萃取纤维在室温25℃下直接萃取60min,磁力搅拌速度为1100r.min-1,然后萃取纤维在解吸室内静态解吸9min后进行HPLC分析.液相色谱分离条件为ZORBAXSBC18柱(4.6mmi.d.×250mm,5.0μm),流动相为甲醇-水(70:30,V/V),流速为1.0ml.min-1,二极管阵列检测器波长为280nm.方法线性范围为0.005mg.l-1—0.5mg.l-1(R>0.99),两种物质的检出限(S/N=3)分别为0.003mg.l-1和0.002mg.l-1.加标回收率分别在89.6%—100.4%和97.5%—100.1%(n=5)之间,相对平均标准偏差(RSD)分别在4.5%—6.2%和3.8%—6.7%之间.该方法快速、简便,无需使用有机溶剂,适于水样中痕量物质的分析.     

The application of solid-phase micro-extraction (SPME) to the analysis of polycyclic aromatic hydrocarbons (PAHs)

There are many established extraction techniques regularly used in the isolation and analysis of PAHs and similar organic compounds from various phases. These include Soxhlet or ultrasonic extractions from solids, and liquid-liquid or solid-phase extraction from aqueous samples. However, these methods have some inherent disadvantages; most require large volumes of organic solvents, they can be time consuming and many involve multi-step processes that always present the risk of the loss of some analytes (Zhang et al., 1994). Solid-phase micro-extraction (SPME) is a relatively new technique that has been used with much success in the analysis of a variety of compounds including PAHs. Experiments are being carried out to determine the optimum range of conditions for the extraction of a range of PAHs. Parameters under investigation include temperature, equilibration time, salinity and compound concentration. Presented here are some preliminary experiments into the applicability of SPME for PAH analysis. Further work will investigate the reproducibility of the technique, limits of detection and matrix effects. When an optimised method has been developed the technique will be used in investigations into PAH profiles in sediment cores.     

Determination of selected semi-volatile organic compounds in water using automated online solid-phase extraction with large-volume injection/gas chromatography/mass spectrometry

A rapid, sensitive, and cost-effective analytical method was developed for the analysis of selected semi-volatile organic compounds in water. The method used an automated online solid-phase extraction technique coupled with programmed-temperature vaporization large-volume injection gas chromatography/mass spectrometry. The water samples were extracted by using a fully automated mobile rack system based on x-y-z robotic techniques using syringes and disposable 96-well extraction plates. The method was validated for the analysis of 30 semivolatile analytes in drinking water, groundwater, and surface water. For a sample volume of 10 mL, the linear calibrations ranged from 0.01 or 0.05 to 2.5 ??g·L^?1, and the method detection limits were less than 0.1 ??g·L^?1. For the reagent water samples fortified at 1.0 ??g·L^?1 and 2.0 ??g·L^?1, the obtained mean absolute recoveries were 70%?C130% with relative standard deviations of less than 20% for most analytes. For the drinking water, groundwater, and surface water samples fortified at 1.0 ??g·L^?1, the obtained mean absolute recoveries were 50%?C130% with relative standard deviations of less than 20% for most analytes. The new method demonstrated three advantages: 1) no manipulation except the fortification of surrogate standards prior to extraction; 2) significant cost reduction associated with sample collection, shipping, storage, and preparation; and 3) reduced exposure to hazardous solvents and other chemicals. As a result, this new automated method can be used as an effective approach for screening and/or compliance monitoring of selected semi-volatile organic compounds in water.     

新型固相萃取器用于污染水样中痕量杀虫剂的浓缩及热解吸气相色谱-质谱分析

1　IntroductionSolid phasemicro extraction (SPME)asasimpleandrapidextractiontechniqueiswidelyusedinvariousareasforextractingdiluteanalytesfromliquid ,gaseousandsolidsamplesbecauseofitshighextractionefficiency[1 ].Recently ,astirbarsorptiveextraction (SBSE…     

磁性介孔硅胶萃取剂的制备及萃取性能研究

合成了C18基团修饰的磁性介孔硅胶材料,并利用该材料建立了磁性固相萃取-色谱分析方法,测定了几种环境水样中酞酸酯类(PAEs)污染物的含量.结果表明,该材料具有较大的比表面积(273 m.2g-1)和饱和磁通量(29 emu.g-1),对水样中痕量的PAEs有较强的萃取能力,而且萃取剂的磁分离特性使得萃取操作更为方便、快捷.在优化条件下,30 mg萃取剂在40 min内即可从500 mL水样中萃取痕量PAEs,回收率可达80%以上.此外,该萃取剂在处理复杂环境样品时仍能保持较强的萃取能力,环境水样中4种PAEs的检测限可达15.6—32.5 ng.L-1,加标回收率为62%—109%,相对标准偏差为2%—8%.     

斑马鱼幼鱼运动行为测试评价饮用水安全

饮用水安全直接关乎人类的健康与安全,当前迫切需要全新的毒性测试方法对饮用水的潜在人类健康风险进行全面、准确和灵敏的评估和预警。本研究以反渗透技术(RO)取代常用的固相萃取,分别浓缩饮用水厂的进厂水、出厂水和管网水进行毒性试验水样的前处理。反渗透技术前处理方法可以避免传统固相萃取方法中使用的有机溶剂对行为学测试体系的干扰。RO浓缩后的饮用水对斑马鱼胚胎进行持续暴露,采用Viewpoint行为测试软件量化分析出生后第6天(6 dpf)斑马鱼幼鱼的运动行为,选择运动距离和转向行为作为测试终点,分析进厂水、出厂水及管网水的潜在毒性及可能变化。结果表明,暴露在进厂水的幼鱼出现了明显的行为变化,尤其在较高浓度(20倍浓缩)暴露时,运动距离相比对照组显著减少,同时伴有剧烈的转向等异常行为;管网水对斑马鱼幼鱼行为存在一定程度的影响,而出厂水对幼鱼的运动行为没有显著影响。研究结果反映出当前饮用水厂深度处理工艺可以有效降低进厂水的潜在毒性和健康风险,但是经供水管网输送后,其水质可能发生了改变,导致管网水可能存在潜在的毒性。本研究所采用的反渗透技术前处理技术及斑马鱼幼鱼的运动行为学测试方法,可用于未来建立评估饮用水水质安全的早期预警系统。     

利用HS-SPME-GC技术分析环境水样中超痕量的六氯苯,DDT及其代谢产物

利用顶空固相微萃取(HS-SPME)和气相色谱检测技术,通过对三种不同的SPME萃取头(PDMS,PMPVS,PA)实验条件的优化,并参照液液萃取的方法,对水相中六氯苯,DDT及其代谢产物的萃取效果进行了比较．结果表明,SPME方法比液液萃取方法在检测限和回收率上有很大的提高,其中PDMS对检测六氯苯,DDT及其代谢产物的效果较其它两种萃取头好．     

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

• Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.     

Simultaneous analysis of five taste and odor compounds in surface water using solid-phase extraction and gas chromatography-mass spectrometry

In this paper, a method using solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) was developed to simultaneously analyze five taste and odor compounds in surface water, i.e., 2-methylisoborneol (2-MIB), 2,4,6-trichloroanisole (TCA), 2-isopropyl-3-methoxy pyrazine (IPMP), 2-isobutyl-3-methoxy pyrazine (IBMP), and trans-1,10-dimethyl-trans-9-decalol (geosmin, GSM). The mass spectrometry was operated in selective ion monitoring (SIM) mode. Three kinds of SPE columns and three eluting solvents were compared, the C18 column was chosen as optimum SPE column, and methanol was chosen as the optimum eluting solvent. It was found that the method showed good linearity in the range of 1–200 ng·L^-1 and gave detection limits of 0.5–1.5 ng·L^-1 for individual compounds. Good recoveries (93.5%–108%) and relative standard deviations (1.58%–7.31%) were also obtained. Additionally, concentrations of these taste and odor compounds in Jinan’s surface and drinking water were analyzed by applying this method, and the results showed that GSM and 2-MIB were the dominant taste and odor compounds in Jinan’s raw water.     

Removal of pesticides from water samples by adsorption with fatty acids supported on barium sulphate

Oleic or linoleic acid supported on barium sulphate was used to remove atrazine and terbuthylazine in the range of 0.1–2.0 μg/L using spiked water samples. The sorption of atrazine depends on the stirring time and the best value is 150 min. Terbuthylazine is removed well with a stirring time of 60 min and its adsorption is about 90%. Detection of the residual pesticide in treated waters, after solid phase extraction (SPE), was carried out by GC‐MS operating in selected ion monitoring (SIM) using a calibration curve by direct injection of standard solutions of herbicide.