环境中有机锡化合物形态分析方法进展

本文综述了国内外近２０年来环境样品中有机锡化合物的分析技术。对有机锡样品的衍生技术进行了评价：系统介绍了检测有机锡化合物的气相色谱（ＧＣ）联用技术、高效液相色谱（ＨＰＬＣ）联用技术以及超临界流体液相色谱（ＳＦＣ）联用技术。     

痕量壬基酚及相关化合物的样品预处理和测定

对近年来环境样品中痕量内分泌干扰物壬基酚及相关化合物的分离富集方法和测定技术的研究进展进行了综合评述。重点讨论了索氏提取、液液萃取、液膜分离、回流萃取、固相萃取、固相微萃取、超临界流体萃取、超声提取八种样品预处理方法和气相色谱质谱联用、高效液相色谱两种测定方法,而且针对以上方面提出了尚需进一步研究的问题。     

有机汞形态分析检测仪器的联用技术研究

报道了流动注射固相萃取预富集，液相色谱分离，冷原子吸收检测的联用技术，并对有机汞的各形态进行了富集，分离和测定。由于采用在线排气技术和冷原子吸收测定，方法有很好的选择性，有机汞混合物经一次进样即可连续获得各形态的含量，操作简便，快速，可用于污染水体中各形态有机汞含量的测定。     

土壤中多氯联苯分析方法研究进展

文中综述了多氯联苯的分析技术及其研究进展。介绍了样品前处理技术如索氏萃取法、超声萃取法、微波辅助萃取、超临界流体萃取、加速溶剂萃取等在土壤样品中多氯联苯分析中的应用;阐述了气相色谱、液相色谱、气质联用技术在土壤样品中多氯联苯的检测,并对土壤中未来多氯联苯检测技术的发展提出了展望。     

地下水中农药的测定

自动测定技术为地下水中微量农药的监测提供了便利。S．Lacorte等报道了一种能测定万亿分之一浓度水平有机磷农药的方法。他们使用液相色谱和常压离子色谱进行自动固液革取和测定。将一个100mL的酸化水样通过液相色谱进入常压离子色谱而得以浓缩和洗提，操作在阳离子态或阴离子态。用选择离子监测方式，12种农药的定量测定限在5～37ng／L，测定的重现性为17％～25％，该方法的平均回收率大于95％。地下水中农药的测定@小刘     

焦化废水臭氧催化氧化过程的污染物降解特征

为了考察焦化废水臭氧催化氧化深度处理过程中污染物的降解特征,对处理过程中的废水进行了COD、TOC、BOD、紫外可见光谱、高效液相色谱、气相色谱-质谱联用(GC-MS)和凝胶色谱等多种分析。结果表明:经臭氧催化氧化处理后,废水的COD、TOC和UV_(254)均降低,降低速度大小为UV_(254)CODTOC;臭氧催化氧化可提高废水的可生化性,但氧化时间进一步延长,可生化性反而降低;液相色谱表明非极性物质优先得到去除;凝胶色谱表明分子量较小的物质优先去除;GC-MS结果表明焦化废水混凝出水中主要成分为苯酚类、杂环化合物、多环芳烃及其衍生物,臭氧催化氧化处理后这些化合物都得到有效降解。     

海洋环境中的有机锡及其对海洋生物的影响

本文综述了有机锡化占物对海洋环境的冲击及其对海洋生物的影响，介绍了有机锡化合物的分析方法，讨论了有机锡污染的预防和控制措施，并展望了有机锡研究的前景。     

不同pH下微生物燃料电池降解含硫偶氮染料废水的效能及其机理

构建单室空气阴极微生物燃料电池反应器(MFC)并用于处理含硫偶氮染料有机废水,研究初始pH对单室MFC的产电性能和对偶氮染料及硫化物的去除效果以及阳极生物膜电化学行为的影响.利用紫外可见光谱全波长扫描(UV-vis),高效液相(HPLC)和液相色谱-质谱联用(LC-MS)分析偶氮染料还原反应过程的中间产物.结果表明,以...     

离子色谱在饮用水消毒副产物及高氯酸盐分析中的应用

介绍了离子色谱在饮用水中消毒副产物及高氯酸盐分析中的应用。重点介绍了离子色谱测定饮用水中溴酸盐和高氯酸盐的方法。简单介绍了卤代乙酸和氯酸盐的离子色谱测定法及离子色谱-质谱联用技术在饮用水消毒副产物及高氯酸盐分析中的应用。     

离子色谱在饮用水消毒副产物及高氯酸盐分析中的应用

介绍了离子色谱在饮用水中消毒副产物及高氯酸盐分析中的应用。重点介绍了离子色谱测定饮用水中溴酸盐和高氯酸盐的方法。简单介绍了卤代乙酸和氯酸盐的离子色谱测定法及离子色谱-质谱联用技术在饮用水消毒副产物及高氯酸盐分析中的应用。     

Determination of selected quaternary ammonium compounds by liquid chromatography with mass spectrometry. Part II. Application to sediment and sludge samples in Austria

Soxhlet extraction and high-performance liquid chromatography (HPLC) coupled to tandem mass spectrometry detection (MS/MS) was used for the determination of selected quaternary ammonium compounds (QACs) in solid samples. The method was applied for the determination of alkyl benzyl, dialkyl and trialkyl quaternary ammonium compounds in sediment and sludge samples in Austria. The overall method quantification limits range from 0.6 to 3 microg/kg for sediments and from 2 to 5 microg/kg for sewage sludges. Mean recoveries between 67% and 95% are achieved. In general sediments were especially contaminated by C12 chain benzalkonium chloride (BAC-C12) as well as by the long C-chain dialkyldimethylammonium chloride (DDAC-C18) with a maximum concentration of 3.6 mg/kg and 2.1mg/kg, respectively. Maxima of 27 mg/kg for DDAC-C10, 25 mg/kg for BAC-C12 and 23 mg/kg for BAC-C14 were determined for sludge samples. The sums of the 12 selected target compounds range from 22 mg/kg to 103 mg/kg in the sludge samples.     

Synthesis and characterization of m- and p-methylbenzyl-mercapturic acids derived from m- and p-xylenes

Chemical synthesis and physical properties of two mercapturic acids suggested as urinary metabolites of m- and p-xylenes ace described. These compounds may be used for the identification and quantivative determination by high-performance liquid chromatography of the corresponding mercapturic acids in urine.     

Spatial distribution of organotins in sediments of lowland river catchments

A method is described for the measurement of nanogram quantities of a range of methyl and butyltin compounds. The method utilises a modified purge and trap/boiling point separation technique for the determination of organotin compounds in sediment samples. A spatial survey of sediment samples within 5 river systems in the East Anglia region of the United Kingdom was undertaken and identified a range of organotin compounds with concentrations of tributyltin (TBT) ranging from <3.9 ng g(-1) up to 1291 ng g(-1). The highest values were found in areas connected with boating activities. Wherever TBT was present, dibutyltin and monobutyltin were most commonly found along with small concentrations of certain methyltins.     

Pilot study on the contamination of drinking water by organotin compounds from PVC materials

Raw and treated water samples and tap water samples from four to six houses located on distribution lines where PVC pipe/tubing had been recently installed were collected in five Canadian municipalities for the analysis of organotin compounds. After derivatisation with sodium tetraethylborate the ethylated organotin compounds were extracted with hexane and analysed by gas chromatography-microwave induced plasma atomic emission spectrometry using a wavelength (326.234 nm) specific for tin. Organotin compounds, mainly methyltin and dimethyltin at concentrations ranging respectively from 0.5 to 257 ng Sn/L and from 0.5 to 6.5 ng Sn/L, were detected in samples from ten of the twenty-two houses. No organotin compounds were detected in raw water or treated water leaving the treatment plant, indicating that the organotin compounds were leaching into the water from some component of the distribution system.     

A study on organotin levels in Canadian drinking water distributed through PVC pipes

A study on organotin compounds in Canadian drinking water was carried out in winter-spring 1996 (28 sites) and autumn 1996 (21 sites). Approximately 29% and 40% of distribution waters supplied through PVC pipes installed recently (typically less than 6 months) contained organotin compounds in the winter-spring and autumn surveys respectively. Monomethyl-, dimethyl-, monobutyl- and dibutyltin levels ranged up to 291 ng Sn/L, 49.1 ng Sn/L, 28.5 ng Sn/L and 52.3 ng Sn/L, respectively. An additional study in summer 1996, of locations where the highest organotin levels were detected in the winter-spring survey, indicated that organotin levels had decreased in most distribution water samples. Samples of PVC pipe/tubing contained organotin compounds consistent with the organotin patterns found in the distribution water samples.     

Relationships between the abnormalities of the male reproductive organs and the accumulation of phenol compounds in the striped field mouse, Apodemus agrarius, inhabiting Korea

The relationships between the abnormalities of the male reproductive organs in striped field mice and the accumulation of endocrine-disrupting chemicals were assessed. Most mice collected at three areas were contaminated with phenol or organotin compounds. Fourteen to 42% of the mice at each area had abnormally shrunken reproductive organs, and some of them were contaminated with high levels of phenol compounds. Moreover, all the shrunken reproductive organs were damaged in the histological structure. The damage was observed also from several mice accumulating a high level of phenol compounds even though they had normally developed reproductive organs, although no damage was found in the mice accumulating a high level of organotin compounds. Collectively, the abnormalities of the reproductive organs in the mice seemed to be related to the accumulation of phenol compounds rather than of organotin compounds.     

Specific detection of organotin compounds with a recombinant luminescent bacteria

Organotin compounds are widely used as biocides in marine and terrestrial environments. Several currently used techniques allow either the measurement of the chemicals or their effects on living organisms. Our current research focuses on the development of a complementary method based on a bacterial bioluminescence-based bioassay for the specific detection of organotin compounds. The performance of the bioassay was assessed. The Escherichia coli bacterial strain used in this study is specific for TBT and DBT (with Cl, Br or I as the halogen group) with the central tin atom important for light production. The assay is conducted after overnight culture of the bacterial strain, followed by 60 min of contact time with the organotin compound for significant light production. The detection limits were found to be 0.08 microM for TBT (26 microgl(-1)) and 0.0001 microM for DBT (0.03 microgl(-1)) with a linear range of one logarithm. The repeatability of the bioassay is 8% and the reproducibility for TBT and DBT was approximately 14%. Lyophilization of the strains did not significantly modify the detection limit as well as the range of detection. Applications of the bioassay to environmental samples are discussed.     

HPLC-PFD determination of priority pollutant PAHs in water,sediment, and semipermeable membrane devices

High performance liquid chromatography coupled with programmable fluorescence detection was employed for the determination of 15 priority pollutant polycyclic aromatic hydrocarbons (PPPAHs) in water, sediment, and semipermeable membrane devices (SPMDs). Chromatographic separation using this analytical method facilitates selectivity, sensitivity (ppt levels), and can serve as a non-destructive technique for subsequent analysis by other chromatographic and spectroscopic techniques. Extraction and sample cleanup procedures were also developed for water, sediment, and SPMDs using various chromatographic and wet chemical methods. The focus of this publication is to examine the enrichment techniques and the analytical methodologies used in the isolation, characterization, and quantitation of 15 PPPAHs in different sample matrices.     

Polycyclic aromatic hydrocarbons in crude oil-contaminated soil: A two-step method for the isolation and characterization of PAHs

A two-step analytical method is developed for the isolation and characterization of polycyclic aromatic hydrocarbons (PAHs) in crude oil contaminated soil. In the first step, those crude oil components were isolated which are easily mobilized with water from the contaminated soil (determination of groundwater pollution potential). In the second step, the fraction containing the remaining crude oil compounds was extracted using toluene. After the cleanup of the fractions, both fractions were analyzed using high-performance liquid chromatography (HPLC). The HPLC of the toluene extracted fraction shows that along with the sixteen priority pollutants from the US-EPA list, many other polycyclic aromatic hydrocarbons (PAHs) are present as well. It is evident from the chromatograms that a significant amount of PAHs are present as is also the case in the fractions eluted by water. The described method allows the determination of total organic pollutants from crude oil, some of them being potential groundwater contaminants. The major part of the total pollutants could not be mobilized by water and therefore remains in the soil, which was extracted in the second step.     

An intercomparison of formaldehyde measurement techniques at ambient concentration

A study was conducted to evaluate five techniques for determining ambient formaldehyde concentrations. One technique used a spectroscopic determination, and the other four techniques used derivatization followed by fluorometric analysis or high-performance liquid chromatography with detection by u.v. absorption. Formaldehyde was generated by two techniques. In the first technique, zero air was bubbled through a solution of aqueous formaldehyde to produce gas-phase formaldehyde. Various compounds serving as possible interferences were added singly or in combination to these air mixtures. In the second technique, formaldehyde was generated as a product from controlled irradiations of hydrocarbons and nitrogen oxides in a smog chamber operated in a dynamic mode. The study was conducted as a blind intercomparison with no knowledge by the participants of the HCHO concentrations or the interferences added.The data from each of the techniques were compared against mean values in each sampling period. For formaldehyde in zero air, average deviations for each of the techniques ranged between 15 and 30%. At a formaldehyde concentration of 10 ppb, each technique showed no evidence for interferences by O₃ (190 ppbv), NO₂ (300 ppbv), SO₂ (20 ppbv), and H₂O₂ (7 ppbv). The agreement for formaldehyde concentrations measured for the photochemical mixtures was similar to that of the mixtures in zero air.Ambient measurements were also performed on three evenings and for one 36-h period. Ambient formaldehyde concentrations ranged from 1 to 10 ppbv. Ambient H₂O₂ measurements were also performed. A strong correlation in the diurnal concentration profile for formaldehyde and H₂O₂ was observed over the 36-h period.