基于弱阴离子交换(WAX)小柱富集水样中的六价铬,三价铬则不被小柱保留而直接被去除,采用AS20柱分离、KOH溶液为淋洗液洗脱,采用串联四极杆质谱在电喷雾电离负离子模式下多反应监测模式(MRM)测定六价铬.研究了样品的净化条件、三价铬的去除和色谱质谱条件.结果表明,六价铬质量浓度在1.0～200μg/L范围内呈良好的线性,相关系数(R2)优于0.9995,方法定量限(LOQ)和检出限(LOD)分别为为1.0和0.3μg/L,加标回收率在72.5％～94.0％之间,相对标准偏差(RSD)为5.2％～8.6％.用所建立的方法对本地区代表性的51个工业废水样品进行了测定.

Two kinds of olfactory substances, i.e. dimethyl isocamphthenol (2－MIB) and GSM in water sources and drinking water have been determined by the liquid－liquid extraction combined with gas chromatography－mass spec-trometry process, the cell walls in water bodies broken, and the intracellular and extracellular olfactory substances detected. 2－MIB and GSM have been subject to the addition of sodium chloride, normal hexane liquid－liquid extra-ction, concentration, and sample introduction, analyses and determination by gas chromatography－mass spectrometry process, and the selection of ion mode quantity. The results show that the method has good separation effect. The lin-earity of both 2－MIB and GSM is good in the standard curve of 10－100 μg/L. The regression coefficient R2 is more than 0.995. When the sampling volume is 1 000 mL,the detection limits are 2.58 ng/L and 2.45 ng/L,respectively. The standard recovery rate of 2－MIB and GSM are 86.7%－103.0%,and 87.5%－91.8%,respectively. The RSD of 2－MIB and GSM are 3.8%－7.9% and 4.1%－9.8%,respectively.

为评估曹娥江流域水体中传统持久性有机污染物(POPs)和部分新型工业污染物残留特征及其对生态环境和人体健康的危害,作者在研究区采集7个水样,分析滴滴涕(DDTs),六六六(HCHs),多氯联苯(PCBs),邻苯二甲酸酯类化合物(PAEs)及多环芳烃类化合物(PAHs)的残留特征.利用非致癌风险和致癌风险计算模型进行健康风险评价,并应用双荧光报告基因内分泌干扰效应检测实验评价水体有机污染物潜在的内分泌干扰效应.结果表明,除排污口邻苯二甲酸二丁酯(DBP)浓度超过饮用水安全参考指标限值外,其余水样有机污染物均未超过相应限值,水样中有机污染物对人体均无致癌及非致癌风险.双荧光报告基因结果显示,排污口水体中有机污染物具有甲状腺干扰效应.总体而言,曹娥江流域有机污染物生态和健康风险不大,但考虑长期暴露,其潜在内分泌干扰尤其是甲状腺干扰还需深入研究.

An ion chromatography(IC) method was developed for the determination of acid red 26 in dyeing wastewater.100 mmol/L sodium perchlorate solution–acetonitrile(1∶1) was used as the eluent at flow rate of 1.0 mL/min.The analytical column was DIONEX IonPac AS16(250 mm×4 mm).The detection was performed by a Dionex VWD3100 UV/Vis detector.The quantitive analysis of external standard calibration curves was used.The linear range of the method for acid red 26 was 0.1–20 mg/L(r=0.999?9).The average recoveries were 98.4%–101.0% with the relative standard deviations(RSD) no more than 0.5%.The detection limit(S/N=3) was 0.03 mg/L.The RSDs of the retention time,peak area and peak height were 0.10%,0.50% and 0.15%,respectively.The interference of many anions in dyeing wastewater was elimated by using the UV detecter.

A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1:1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C, column (150 mm x 2. 1 mm, 5 microm) and with the gradient elution of acetonitrile and 0. 1% formic acid. The eight pesticides were determined in the modes of electrospray ionization (ESI) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1 - 100 microg/L for fipronil, and in 5 -200 microg/L for the other pesticides. The limits of quantification (LOQs, S/N> 10) were 2 p.g/kg for fipronil and 10 microg/kg for the other pesticides. The average recoveries ranged from 75. 5% to 115.0% with the relative standard deviations of 2.7% - 7.7% at the spiked levels of 2, 5, 50 microg/kg for fipronil and 10, 50, 100 microg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 "Evaluation and Expression of Uncertainty in Measurement". Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea.

Amounts of nitrobenzenes in water sample were determined by GC with microelectron capture detector.Nitrobenzene compounds in water sample were extracted with a mixture of ethylacetate,benzene and diethyl ether(2+1+0.02),and separated on HP-1701 capillary column(30 m×0.25 mm,0.25 μm).The 9 nitrobenzenes were separated within 11.5 min.Linear relationships between values of peak area and mass concentration of the 9 nitrobenzenes were obtained in the same range of 0.001-5.0 mg·L-1.Test for recovery was made by standard addition method,giving recovery in the range of 92.0%-108% with RSD′s(n=5) less than 5.0%.

It was found that the precision of the results of determination of volatile organic compounds(VOC′s) in water samples by GC using the HP 7694E head space automatic sampler was poor and unsatisfactory,and that the cause was the designing defect of its heating device.Measure for improvement was proposed by preheating the water samples to a temperature close to the temperature of the detection chamber(25±2) ℃ in water bath,and setting the conditions of head-space sampling at 55 ℃ and 15 min.Four VOC′s(i.e.CHCl3,BrCHCl2,Br2CHCl and CHBr3) were determined under the prescribed conditions.Values of RSD′s(n=5) found were in the range of 2.2% to 3.3%.

JAIN SLEE,as the core of an asynchronous,event-driven,converged network application environment,its reliability requires persistence program to save and restore the states related to service building blocks.However,JAIN SLEE lacked for the technology of asynchronous persistence at present.An asynchronous persistence program is proposed in this article,and then the persistence resource adaptor is designed and implemented.After testing,the program can guarantee the reliability of JAIN SLEE,with higher performance compared with the mature,synchronization persistence program of J2EE.

The protection of raw water reservoir is the key point of high quality drinking water supply.By intensive monitoring of Tangpu Reservoir on sensitive parameters for five years,we believed that pH,DO,CODMn,TN,TP and algae are most important and sensitive for water protection and water supply;And their status,characteristics and tendency are studied.By this way the practicable guidance for reservoir administration and water treatment are proposed.Besides,the eutrophication level of Tangpu Reservoir is estimated and the recommendation on water quality monitoring and estimation of drinking water reservoir are pointed out.