水样中痕量十溴联苯醚的分散液-液微萃取条件的优化

采用正交设计和Box-Penhnken响应面设计,对分散液-液微萃取技术萃取水样中痕量十溴联苯醚的条件进行了筛选和优化,得到最佳条件:四氯乙烯为萃取剂(10μl)、丙酮作分散剂(1ml)、pH范围5~9、离子强度,2%NaCl及萃取时间10min。此优化条件下分散液-液微萃取技术的萃取回收率可达92.37%~104.38%,富集倍数为508~611。优化条件下方法的线性范围为0.01~100ng/ml,检出限(S/N=2)为3.0pg/ml,加标回收率为96.25%~102.16%,精密度为5.44%~6.34%。     

分散液液微萃取气相色谱-质谱法测定水中15种硝基苯类化合物

建立了超声辅助基质分散液液微萃取（UA-DLLME）作为前处理联合气相色谱串联质谱（GC-MS）同时测定地下水和地表水中15种硝基苯类化合物的分析方法。萃取剂、分散剂、萃取温度、萃取时间和离子强度等影响因素采用Plackett-Burman设计，快速筛选出最显著影响因素，利用中心组合设计（CCD）简化实验步骤优化显著因素，结合响应曲面图最终确定最佳的萃取条件：5 mL水样在3%氯化钠条件下迅速加入40 μL四氯化碳（萃取剂）和0.5 mL乙腈（分散剂），50 ℃下超声4 min，混合液4 000 r/min离心3 min。结果表明：15种硝基苯类化合物在50.0~1 000.0 μg/L的浓度范围内线性相关系数均大于0.995；采用超声辅助基质分散液液微萃取时，方法检出限（MDL）为0.018~0.039 μg/L；15种目标物的加标平均回收率为83.31%~99.08%，相对标准偏差均不高于5.0%（n=6）。     

分散液液微萃取-气相色谱法测定地表水中松节油

采用分散液液微萃取-气相色谱法测定地表水中松节油,通过试验优化萃取剂、分散剂的种类和用量、盐度等影响萃取效率的条件,使该方法在10.0μg/L~500μg/L范围内线性良好,方法检出限为1.6μg/L。用该方法测定实际水样,结果未检出。实际水样的3个质量浓度水平加标回收率为83.6%~104%,RSD为2.1%~8.3%。     

分散液液微萃取与超高效液相色谱-串联质谱联用测定土壤和沉积物中三丁基锡

建立了分散液液微萃取与超高效液相色谱-串联质谱联用技术测定土壤和沉积物中三丁基锡的方法。考察了影响分散液液微萃取的因素(包括有机萃取溶剂、萃取剂体积、分散剂、分散剂体积、萃取时间和盐效应)。在最佳实验条件下,方法在0.5~50μg/kg范围内线性关系良好,相关性系数为0.999 0,方法检出限(3倍信噪比)为0.1μg/kg,加标回收率为83.1%~104%,相对标准偏差小于8.5%(n=6),适用于土壤和沉积物中三丁基锡的检测。     

超声辅助离子液体微萃取-液相色谱-串联质谱法测水中六溴环十二烷

建立了超声辅助离子液体液-液微萃取(USA-IL-DLLME)结合液相色谱-串联质谱测定水中六溴环十二烷3种异构体(α-HBCD、β-HBCD、γ-HBCD)的分析方法。实验中分别考察了离子液体萃取剂的种类及体积、超声时间、样品p H及盐浓度等因素的影响。在最佳条件下,HBCDs 3种异构体在0.5~100μg/L质量浓度条件下有较好的线性关系,相关系数大于0.998,最低检出限分别为156.4、84.6、85.5 ng/L,测定下限分别为0.626、0.339、0.342μg/L。相对标准偏差(n=5)为5.3%~9.7%。采用该方法对实际环境水样进行了检测与加标回收实验,在1、20μg/L 2个添加水平下,加标回收率为71%~102%。方法具有简单快速、有机溶剂用量少、绿色环保的特点。     

液-液小体积萃取GC-MS方法快速测定地表水中的氯苯类化合物

建立了一种液-液小体积萃取GC-MS快速测定地表水中氯苯类化合物的分析方法。该方法具有操作简单快速、适用性广和试剂用量很少等特点。当萃取试剂用量为2ml时(约为一般常规液-液萃取用量的数十分之一),萃取富集效率可达300~500倍,回收率为93%~98%,相对标准偏差为4%~8%,检出限为0.1~0.3μg/L。     

分散液液微萃取-气相色谱法测定白洋淀水中PAEs

以四氯化碳为萃取剂,乙腈为分散剂,采用分散液液微萃取-气相色谱法测定水中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二丁基苄基酯、邻苯二甲酸二（2-乙基己酯）和邻苯二甲酸二正辛酯,优化了萃取条件。6种邻苯二甲酸酯在1.00μg/L～100μg/L范围内线性良好,方法检出限为0.18μg/L～2.5μg/L,标准溶液测定的RSD≤6.1%,白洋淀水样的加标回收率为70.9%～119%。     

分散液液微萃取-气相色谱/质谱联用法测定饮用水源水中的四乙基铅

采用分散液液微萃取与气相色谱/质谱法联用技术建立了测定水样中四乙基铅的方法。考察了影响分散液液微萃取的因素,包括萃取溶剂、分散剂、萃取次数、萃取时间和盐效应等。在最佳条件下,四乙基铅的富集倍数为330倍,检出限为0.01μg/L(S/N=3),线性范围为0.10~10.0μg/L,线性相关系数为0. 9992。测定饮用水源水中的四乙基铅,加标回收率为87.7%~105%,相对标准偏差为4.8%~7.3%(n=3)。     

液液萃取-气质联用法测定水中20种农药类有机物

采用液液萃取-气质联用法同时测定水中20种农药类有机物。对前处理过程中萃取剂的选择、用量，萃取时间，盐析剂用量，有机改进剂的加入等条件进行了优化，使得各组分在0．500μg/L～50．0μg/L范围内线性良好。方法检出限为0．02μg/L～0．19μg/L；平行测定7次混合标准溶液，RSD为0．3％～9．1％；对20种农药类有机物混合标准溶液进行加标回收试验，回收率为90．5％～110％。该方法优化了《生活饮用水标准检验方法》（ GB 5750-2006）中农药类有机污染物的检测方法，满足常规测定的要求。     

液液萃取-气相色谱法测定饮用水中硝基苯类化合物

采用液液萃取－气相色谱法测定饮用水中10种硝基苯类化合物，通过萃取条件优化试验，选择正己烷为萃取剂，使目标物在0μg／L～38.5μg／L之间线性良好，检出限为0.002μg／L ～0．005μg／L。实际饮用水样的加标回收率为80.8％～104％，RSD＜3％。用该方法测定桂林市4个水厂饮用水，结果硝基苯、间－二硝基苯、2，4－二硝基氯苯未检出，其余7种硝基苯类化合物虽有检出，但检出值均低于标准规定的限值。     

Determination of PAHs by On-Line Polarization Synchronous Fluorescence with HPLC

A novel analytical method has been established for on-line simultaneous determination of fluorene and acenaphthene,chrysene and benzo[a]anthracene (B[a]A) by polarization synchronous fluoromet.y (PSF) coupled to high performance liquid chromatography (HPLC). The detection limits were: 0.039, 0.046, 0.016 and 0.042 mgL-1 for fluorene, acenaphthene, chrysene and B[a]A, respectively. The proposed method has been successfisily applied to simultaneous determination of these PAHs in environmental air and marine sediment samples.     

高效液相色谱法测定环境水样中嘧磺隆

环境水体中的嘧磺隆在ｐＨ＝２－３的Ｈ２ＳＯ４介质中用二氯甲烷萃取富集，然后用高压液相色谱法分离和紫外光（２５４ｎｍ）检测器检测，外标法定量。用此方法测定了井水和生产单位排放的综合污水中的嘧磺隆，结果满意，最大相对标准偏差为５％，样品加标回收率在９３～１０７％之间，最低检测限量为２ｎｇ，最低检出浓度为０．００４ｍｇ／Ｌ。     

固相萃取-高效液相色谱法测定水中氯酚类化合物

采用固相萃取-高效液相色谱法测定水中7种氯酚类化合物,Waters OASIS WAX柱萃取效率最高,最佳萃取时间和洗脱时间分别为60和5 min。该法的线性范围为1.0~40 mg/L,检出限为0.015~0.5μg/L,精密度为0.558%~2.22%,回收率为83.2%~105%。该法适用于地表水及饮用水中氯酚类化合物的检测。     

高效液相色谱-柱前衍生法测定水中有机磷除草剂

建立了水样中痕量草甘膦、草铵膦和氨甲基磷酸的FMOC柱前衍生-高效液相色谱-荧光检测分析方法。草甘膦,草铵膦和氨甲基磷酸的平均加标回收率分别为94.2%、90.8%、98.6%;相对标准偏差分别为4.8%、0.68%、2.8%;方法的定性下限和定量下限分别为0.05、0.04、0.009μg/L和0.16、0.12、0.03μg/L。水样放置两天后,水样中的草甘膦、草铵膦分别降解了17.8%和19.5%,而水样经过衍生后在5天内是稳定的。     

Assessment of groundwater corrosiveness for unconfined aquifer system at Kalpakkam

Groundwater samples from the shallow unconfined aquifer were collected from fifteen borewells in Kalpakkam nuclear plant site and were analysed for various physico-chemical parameters. The pH, temperature, salinity, TDS and EC were measured in the field. The borewell samples were analysed in the laboratory for Ca(2+), Mg(2+), Na(+), Cl(-), [Formula: see text], [Formula: see text], [Formula: see text] and [Formula: see text]. The Piper Trilinear diagram showed that majority of the borewell samples fall in Na - Cl +SO(4) type and Na - CO(3)+HCO(3) type. The Cl: HCO3 ratio of some borewell samples are categorized under injuriously contaminated to highly injurious type. The higher salinity levels encountered in some borewells emphasized the need for better understanding of groundwater corrosiveness. Accordingly, the Langeliar saturation Index (SI), Aggressivity index (AI) and Larson ratio (LnR) were evaluated for assessing the corrosive nature of the groundwater. The saline water incursion in the southern part of the study area increased the ionic concentration of Cl(-) and [Formula: see text] that made the groundwater corrosive.     

Environmental and Biological Monitoring of Organochlorine Residues after the Plague Epidemic in Surat, India - A Preliminary Study

In late August 1994, an outbreak of human pneumonic/bubonic plague was reported in Surat, India. During the epidemic, large amounts of pesticides, such as benzene-hexachloride (BHC) and other organochlorinated compounds were used to control the vector that might have transmitted the plague. In order to evaluate the extent of contamination, both environmental samples (9 water samples and 4 soil samples) and biological samples (5 blood and urine samples) were collected and analyzed for organochlorine residues. Samples were analyzed after hexane extraction by gas chromatography equipped with electron capture detector (GC-ECD), using a PTE-5 capillary column. The results showed that the levels of 1,1-(2,2-dichloroethenylidene)-bis[4-chlorobenzene] (DDE), a major metabolite of DDT, were low in environmental samples (water, soil), while BHC levels were relatively high in one of the water sample as well as two soil samples. The BHC and DDE levels in the biological samples were not higher than those reported earlier from India, except for serum DDE. Further studies are needed to evaluate the effect of long-term exposure as the present study was based on limited samples.     

Hydrochemical Identification of Groundwater Resources and Their Changes under the Impacts of Human Activity in the Chah Basin in Western Iran

Chemical properties and pollution of water resources were studied in the Chah basin that is located in the Hamadan province, western Iran. Water quality was characterized according to its major constituents and the geological features of the area. Chemical analysis results indicate that groundwaters show wide concentration ranges in major inorganic ions, reflecting complex hydrochemical processes. Groundwater in the studied area is, for the most part, weakly to moderately mineralized and dominated by the calcium (Ca(2+)) and bicarbonate (HCO3-) ions. Within the basin, three different hydrogeochemical facies have been identified: Ca-HCO(3), Ca-SO(4) and Mg-HCO(3). The predominant water type of groundwater samples is the Ca-HCO(3) facies in the recharge area and has a tendency toward Mg-HCO(3) and Ca-SO(4) facies along the direction of water flow. The samples were classified into four groups based on chloride (Cl(-)) and nitrate (NO3-) concentrations and the processes that control water chemistry has been discussed. The results explained the importance of cation exchange, mineral weathering, and anthropogenic activities on groundwater chemistry. It was indicated that cation exchange and Cl-salt inputs are the major process controlling the water chemistry of the low Cl(-) and high [NO3-] (group 2) and high Cl(-) and [NO3-] (group 4). Groundwaters low in NO3- and high in Cl(-) (group 3) and low in NO3- and Cl(-) (group 1) are mainly affected by cation exchange and mineral dissolution. Pollution of groundwaters appeared to be affected by the application of fertilizers, irrigation practice, and solubility of mineral phases and discharge of domestic sewage. Measuring and predicting the mass loading of pollutant to groundwater from specific agricultural systems seems to be useful aids in controlling pollutions in groundwater.     

固相萃取-高效液相色谱法同时测定水中12种磺酰脲类除草剂

采用固相萃取-高效液相色谱法同时测定水中12种磺酰脲类除草剂,样品经磷酸调节pH值为2后,经Watens Oasis HLB SPE柱净化浓缩,乙腈洗脱,选择检测波长为230 nm,以乙腈-水溶液(0.02%磷酸)为流动相梯度洗脱,保留时间在14 min～32 min范围内.12种磺酰脲类除草剂在0.050 mg/L～...     

Ultrasound-assisted ionic liquid-based microextraction combined with least squares support vector machines regression for the simultaneous determination of aluminum,gallium, and indium in water and coal samples

A new simple and rapid ultrasound-assisted ionic liquid-based microextraction method was applied to preconcentrate aluminum(III), gallium(III), and indium(III) ions from water samples as a prior step to their simultaneous spectrophotometric determination using least squares support vector machines regression. In the novel procedure, 1-hexyl-3-methylimidazolium hexafluorophosphate [C₆MIM][PF₆] was dispersed into the aqueous sample solution as fine droplets by ultrasonication, and the analytes were extracted into the ionic liquid phase after complexation with 1,2,5,8-tetrahydroxy anthraquinone (quinalizarine). After centrifuging, the fine droplets of extractant phase were settled to the bottom of the conical-bottom glass centrifuge tube. The detection limits for Al(III), Ga(III), and In(III) were 1.70, 2.02, and 2.06 ng mL⁻¹, respectively. The precision of the method, evaluated as the relative standard deviation obtained by analyzing a series of ten replicates, was below 3.2% for all elements. The method was successfully applied for the determination of Al(III), Ga(III), and In(III) in real samples.     

高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素

建立高浓度有机废水中5种喹诺酮类抗生素的高效液相色谱-串联质谱测定方法。水样经HLB固相萃取小柱富集净化,12 ml甲醇洗脱、浓缩并加入内标溶液后,定容至1 mL待测。以C18柱为分离柱,含0.01%甲酸的甲醇-含0.01%甲酸的水溶液为流动相,目标物质在10 min内分离。在0.25~1 250 ng/mL范围内,目标物质线性关系良好(R20.99)。基质加标试验结果表明,纯水中的回收率为61.40%~91.92%,废水中的回收率为54.92%~101.87%,检出限为0.25~2.5 ng/L,方法定量限为0.36~3.99 ng/L。应用该方法对21家猪场的64份废水样品进行分析,5种喹诺酮类抗生素的检出频率为47%~95%,平均检出浓度为980~5 734 ng/L。该方法快速、准确,适用于高浓度有机废水中喹诺酮类抗生素的同时测定。