萃取色层-原子吸收法测定废水中痕量铅和镉

本文采用吸附树脂GDX-301为支持体,以双硫腙-MIBK混合为萃取剂的萃取色层柱分离富集废水中痕量铅、镉,以0.5N盐酸洗脱后进行原子吸收测定。测定精密度优於5％,回收率96—104％,测定下限:铅50ppb,镉5ppb。方法可用於铀矿冶外排废水、一般工业废水和生活饮用水中微量铅、镉的测定。 文章对色层柱的基本特性及其制备、再生、萃取色层分离的条件、共存元素的干扰、方法的准确度、精密度进行了研究,结果比较满意。     

水中杀菌剂叶青双及其降解物的反相液相色谱测定

本文用反相液相色谱法测定水中叶青双及其降解物2-氨基5-巯基-1,3,4-噻二唑。平均回收率分别为91％和94％;对水样的最低检测浓度分别为2ppb和0.8ppb;叶青双与2-氨基-5-巯基-1,3,4-噻二唑的分离度为2.5。本法在柱效和灵敏度上比硅胶柱液相色谱法有明显的提高。     

蔬菜中三氯杀螨醇残留量分析方法研究

本文报道了在蔬菜中三氯杀螨醇残留量分析方法,主要有二个步骤:(1)萃取、净化后碱解;(2)用气相色谱电子捕获检测器(ECD)检测三氯杀螨醇碱解产物DBP。结果表明:最小检出深度为0.75ppb,在添加浓度0.01—1.00ppm范围,平均回收率为94.76％±7.96％,相对标准误差为5.50％。     

离子色谱/质谱联用分析水和食品中的高氯酸盐

摘要用离子色谱／质谱联用(IC／MS)测定低ppb水平高氯酸根离子的方法．IC／MS是根据EPA方法314开发出来的,原方法用Ic分离电导检测,检测范围为1ppb．IC／MS在整个测定范围内,高氯酸盐回收率不受干扰基质的影响．在饮料和废水中0．5和1ppb添加水平的测定回收率为90％-105％,方法检测限(DML)低于100ppt．     

分散液液微萃取-石墨炉原子吸收光谱法测定环境水样中的痕量镉

建立了分散液液微萃取分离富集一石墨炉原子吸收光谱法测定环境水样中痕量镉的新方法。以二乙基二硫代氨基甲酸钠为螯合剂、四氯化碳为萃取剂、丙酮为分散剂,详细考察YpH值、螯合剂质量分数、萃取剂体积、萃取时间等因素的影响。在优化的实验条件下,方法对水样中镉的检出限为4．2ng-L^-1,线性范围是20-300ng-L^-1,测定结果的相对标准偏差为3．5％,富集倍数达103。将建立的方法应用于三种实际环境水样中镉的检测,加标回收率在92％-108％范围内。本方法具有灵敏、准确、快速、环保的特点,是一种分析水样中痕量镉的较好方法。     

甲氰菊酯残留量的气相色谱分析

本文研究了用气相色谱分析植物、土壤和水中甲氰菊酯的残留量。样品于丙酮提取、石油醚萃取、微型弗罗里硅土层析柱净化后,用带有电子捕获检测器的气相色谱仪进行检测。土壤中添加浓度为0.10—4.00μg/g时,平均回收率为81.3±6.7％(±S％);植物中添加浓度为0.04—4.00μg/g时的平均回收率为93.1±3.6％;水中添加浓度为0.10μg/ml时,回收率为100.8±7.3％。     

高压液体色谱法测定工业废水中的烷基苯磺酸钠

采用反相高压液体色谱(HPLC)荧光法测定合成洗涤剂废水中的直链烷基苯磺酸钠(LAS),激发波长为232nm,发射波长为290nm。使用国产C_(18)色谱柱,甲醇/水体系作流动相,水样经微孔膜过滤后直接进入HPLC仪分析。当废水样中LAS浓度在17—24mg/l时,变异系数为0.8—2.4％;水样加标加收率为82±5％;最低检测浓度为0.016mg/l。     

超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素

采用固相萃取/超高效液相色谱-串联质谱法,建立了水样中磺胺类、四环素类、氟喹诺酮类、大环内酯类和氯霉素类15种抗生素的同时测定方法.水样经HLB固相萃取柱富集,ACQUITY UPLC BEH C_(18)色谱柱分离,以乙腈和5 mmol·L~(-1)乙酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,电喷雾离子源-串联质谱多反应监测模式检测.结果表明,同时测定15种抗生素的线性范围为5—100μg·L~(-1)(相关系数均大于0.997),检出限为2.1—22.0 ng·L~(-1),定量限为6.9—71.8 ng·L~(-1);空白水样在加标水平为5、10、20μg·L~(-1)时,抗生素的回收率为50.1%—109.0%,相对标准偏差为0.4%—8.5%(n=7).用本文建立的方法检测某农业小流域环境水样,发现5类抗生素可被不同程度检出,浓度范围为0.1—106.2 ng·L~(-1).     

除草醚在稻米中残留量测定方法的研究

本文报道了一个测定糙米中除草醚残留量的新方法。样品采用二氯甲烷提取,经中性氧化铝和弗罗里硅土混合吸附剂净化,用填充3％OV—17/Gas chrom Q 80—100目气相色谱柱和氮磷检测器测定。试验结果,样品的添加回收率为87.33—91.47％;变异系数为3.36为6.31％;最小检测浓度为0.0212ppm。     

利用对高锰酸钾-鲁米诺化学发光体系的抑制作用测定痕量碘离子

本文提出一个用化学发光测定痕量碘离子的新方法。基于碘离子对高锰酸钾-鲁米诺体系发光的抑制作用而测定其发光强度的减弱。碘离子浓度在0.4—20ppb呈线性关系。测定14.5ppb碘离子的变异系数为4.1％(n=6)。标准碘的回收率大于95％。本方法灵敏度高,检测限为0.4ppb。用于天然水中碘离子的测定得到满意的结果。     

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.     

Ventilatory responses of the shrimp Palaemon adspersus to sublethal concentrations of crude oil extract

The shrimp Palaemon adspersus Rathke was exposed to the water soluble fraction (WSF: 50; 100; 200 ppb) of North Sea crude oil. The ventilatory behaviour, measured with impedance techniques, was followed for 2 wk and in a subsequent recovery period for 5 wk. Exposure to WSF caused a gradual increase in arrhythmic scaphognathite activity. After 6 d of exposure to 200 ppb shrimps spent more than 50% of the time beating arrhythmically, persisting and sometimes increasing to 100% during the remainder of the exposure period. In the 100 and 50 ppb groups, the proportion of time spent beating arrhythmically increased gradually with exposure time reaching 30 and 20% respectively. After 4 wk in clean seawater no signs of recovery were evident for individuals previously exposed to 200 ppb while those previously in 50 ppb had all recovered. After 5 wk those previously in 100 ppb had recovered and the 200 ppb group showed signs of recovery. The disturbances in ventilatory behaviour when exposed to WSF is considered to be due to damage to gill membranes or to nerve tissue, especially to the neurons in the suboesophageal ganglion controlling scaphognathite activity.Supported by the Environmental Research Programme under the Commission of European Communities (Contribution No. ENV/350/DK (G))     

Effects of some pretreatments on germination of bladder-senna (Colutea armena Boiss. and Huet.) and smoke-tree (Cotinus coggygria Scop.) seeds

This study was carried out to determine effects of pre-treatments including floating in hot water(100 degrees C) followed by continual cooling for 24 hr in the same water floating in tap water for 24 hr submersion in concentrate (98%) sulphuric acid (H2SO4) and cold stratification for different durations (20, 40 and 60 days) and their combinations on seed germination and to investigate how to overcome dormancy of seeds of Colutea armena Boiss. and Huet. and Cotinus coggygria Scop. The seeds were sown in polyethylene pots in the greenhouse and on seedbeds under open field conditions. The statistical design was a randomized complete block design with three replications. The highest germination percentage (77.19%), the best germination rate (16 days) and the highest growth rate (69.01%) were obtained from Colutea armena seeds that were submersed in sulphuric acid for 30 min and sown in the greenhouse. The pre-treatment of submersion in sulphuric acid for 20 min with cold stratification for 60 days gave the highest germination percentage (82.77%) and the highest growth rate (79.37%) in the greenhouse for Cotinus coggygria seeds. On the other hand, the best germination rate (9 days) was obtained from smoketree seeds that were cold stratified 60 days and sown under open field conditions. It can be stated that there is an affirmative effect of the greenhouse condition on germination percentage and growth rate values of the seeds used in this study     

Monitoring toxicity of an azo dye methyl red and a heavy metal Cu,using plant and animal bioassays

Toxicities of an azo dye methyl red and a heavy metal copper (Cu) were quantified, using growth and mortality as end points, in four plant species and three animal species by subjecting them to short-term (4 days for animals, 10 days for plants) static bioassays. Lemna aequinoctialis Welwitch (EC₅₀: 7–16 ppm) was found to be the most sensitive species for methyl red, Ceratophyllum demersum L. (EC₅₀: 25 ppm) and Lactuca sativa L. (EC₅₀: 56 ppm) were intermediate, while Oryza sativa L. shows reduction in seedling vigor (9–27%) of <50%, being the least sensitive amongst the tested plant species. Methyl red toxicity is almost 3–5-fold higher in growing medium (pH = 5.8–6.0), even at high nutrient levels, while Cu toxicity is higher in nutrient-poor alkaline medium at alkaline pH (8.3–8.7; EC₅₀: Ceratophyllum = 104–200 ppb; Lemna = 100–170 ppb) compared to nutrient-rich acidic medium (pH = 5.4–5.7; EC₅₀: Ceratophyllum = 2600–3175 ppb; Lemna = 4350–4715 ppb). Rice tolerance (EC₅₀: 6500 ppb) was found to be higher than hydrophytes while lettuce was most tolerant to Cu. Fish sensitivity toward the test chemicals was almost parallel to Ceratophyllum and Lemna [Gambusia affinis Baird and Gerard (LC₅₀: 250 ppb for Cu) and Poecilia reticulata Peters (LC₅₀: 24 ppm for methyl red)]. Similar to the plants, dye toxicity increased markedly (LC₅₀: 7 ppm) in the acidic medium (pH = 6.0). Amongst the tested organisms, Daphnia was found to be most sensitive to methyl red (EC₅₀: 6 ppm) while its sensitivity to Cu (EC₅₀: 230 ppb) was similar to hydrophytes and fish. Initially, the combination of dye and Cu (at their sublethal concentrations) had additive effects in duckweed, while dye concentration ruled afterward. These results indicate that hydrophytes and animals are equally sensitive toward the test chemicals. Dye toxicity in hydrophytes and fish was pH dependent, while in the case of Cu, it is related to the nutrient status of the growth medium of plants.     

Burden of skin lesions of arsenicosis at higher exposure through groundwater of taluka Gambat district Khairpur, Pakistan: a cross-sectional survey

Prior surveys conducted have found higher proportion of arsenic-contaminated wells in villages along river Indus in Pakistan. This study aims to determine the prevalence of arsenicosis skin lesions among population exposed to higher exposure in taluka Gambat district Khairpur in Sindh. The cross-sectional survey was conducted from August 2008 to January 2009 among 610 households. A total of 707 water sources (hand pumps/wells) were tested from the villages of union councils of Agra and Jado Wahan for arsenic levels with Quick rapid arsenic field test kits. A total of 110 households exposed to arsenic levels >50 ppb were identified. Case screening for arsenic skin lesions was performed for 610 individuals residing in these 110 high-risk households. Information regarding household and socio-demographic characteristics, height and weight measurements and arsenic exposure assessment were collected. Physical examinations by trained physicians were carried out to diagnose the arsenic skin lesions. After data cleaning, 534 individuals from all age groups were included in the final analysis which had complete exposure and outcome information. Overall prevalence of arsenicosis skin lesions was 13.5 % (72 cases). Of the 534 individuals, 490 (91.8 %) were exposed to arsenic levels of ≥100 ppb in drinking water (8.2 % to >50–99 ppb, 58.6 % to 100–299 ppb, 14.6 % to 300–399 ppb and 18 % to ≥400 ppb). Prevalence rate (per 100 population) of arsenicosis was highest at arsenic levels of 100–199 ppb (15.2 cases) followed by ≥400 ppb (13.5 cases) and 300–399 (12.8 cases). Prevalence rate was higher among females (15.2) compared to males (11.3). Our study reports arsenicosis burden due to exposure to higher arsenic levels in drinking water in Pakistan. Exposure to very high levels of arsenic in drinking water calls for urgent action along river Indus. Prevalence of skin lesions increases with increasing arsenic levels in drinking groundwater. Provision of arsenic-free drinking water is essential to avoid current and future burden of arsenicosis in Pakistan.     

固相萃取/气相色谱质谱法测定灰尘中的氯代多环芳烃

建立了固相萃取(SPE)/气相色谱质谱(GC/MS)联用检测灰尘中氯代多环芳烃(ClPAHs)的方法.以正己烷和二氯甲烷混合液为提取溶剂,索氏提取灰尘样品中的20种ClPAHs,活性硅胶层析柱与活性炭混合硅胶SPE柱协同净化.净化后的提取液采用GC/MS测定,SIM模式扫描,并用质谱特征离子定量分析.结果表明,填充量为0.2 g(W(活性炭)∶W(硅胶)=1∶40)的活性炭混合硅胶SPE小柱能有效地将ClPAHs分离出来,载样后采用反向溶剂洗脱,既提高了回收率又减少了洗脱剂甲苯的用量,净化效果好.处理灰尘样品后检测分析,20种ClPAHs的平均回收率稳定在60.4%—120.1%,相关系数>0.99,检出限为0.04—0.17 ng.g-1,相对标准偏差为1.6%—10.2%.本方法前处理简单,定性、定量准确可靠,可广泛应用于环境介质中氯代多环芳烃的检测.     

水中丁基锡化合物的气相色谱分析

本文介绍了一种测定水中痕量三丁基锡和二丁基锡化合物的方法。二氯甲烷萃取和硼氢化钠氢化同时进行，用ＯＶ－１０１色谱柱分离，火焰光度检测器测定，方法最低检测浓度，三丁基锡为０．１ｐｐｂ，二丁基锡为０．４ｐｐｂ。测得青岛、上海和大连港口海水中有三丁基锡化合物存在。     

Cleanup by solid‐phase extraction and HPLC of organochlorine insecticides and PCBS in various nonfatty and fatty samples

An accurate, simple and cheap extraction and cleanup procedure for capillary GC analysis of organo‐chlorine insecticides (OCs) in vegetables (cabbage and carrots) at the ng/g level, and for soil at the μg/g level is presented. The cleanup is carried out on solid‐phase extraction (SPE) cartridges, filled with 500 mg silica, 1 g of deactivated Florisil (10% w/w water), and 100 mg of anhydrous sodium sulphate. Recoveries >90% are obtained. The cleanup of OCs in fatty samples on an HPLC LiChrosorb Si 100 column is evaluated for subsequent capillary GC analysis. Fractionation of OCs and Aroclor 1254 and 1260 on an HPLC Nucleosil 100 column appears to be satisfactory.     

Carbon nanotubes and cyclodextrin polymers for removing organic pollutants from water

Some organic compounds are major water pollutants. They can be toxic or carcinogenic even at low concentrations. Current technologies, however, fail to remove these contaminants to parts per billion (ppb) levels. Here we report on the removal of organic pollutants from water using cross-linked nanoporous polymers that have been copolymerized with previously functionalized carbon nanotubes. These novel polymers can remove model organic species such as p-nitrophenol by as much as 99% from a 10 mg/L spiked water sample compared to granular activated carbon and native cyclodextrin polymer that removed only 47 and 58%, respectively. These polymers have also demonstrated the ability to remove trichloroethylene (10 mg/L spiked sample) to non-detectable levels (detection limit <0.01 ppb) compared to 55 and 70% for activated carbon and native cyclodextrin polymers, respectively.