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。     

液液萃取-气相色谱-质谱法同时测定饮用水中的酞酸酯、百菌清和联苯胺

建立了液液萃取-气相色谱-质谱（LLE -GC/MS）同时测定饮用水中的6种酞酸酯类化合物、百菌清和联苯胺的方法。选用3种有机溶剂进行萃取，筛选出回收率高、操作简单的前处理方法，萃取后经气相色谱-质谱分析。方法表明：8种物质线性良好，相关系数为0．9978～0．9995，用二氯甲烷萃取回收率最佳，回收率在90．1％～118％之间，相对标准偏差在0．24％～7．21％之间。     

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-气质联用法测定饮用水源地水中SVOCs

采用乙酸乙酯-正己烷混合溶剂（体积比为2∶1）对饮用水源地水中阿特拉津、林丹、邻苯二甲酸二正丁酯（DBP）、邻苯二甲酸二（2-乙基己基）酯（DEHP）和滴滴涕（含4种）等8种半挥发性有机物进行1次水样萃取，用气质联用法同时测定。试验表明，方法在25．0μg/L～500μg/L范围内线性良好；检出限在0．006μg/L ～0．028μg/L 之间；空白水样3个质量浓度水平的加标回收率为87．6％～109％，平行测定6次的 RSD＜5．1％；测定集中式生活饮用水源地的实际水样，未检出目标化合物，加标回收率为98．6％～109％。     

液-液萃取-气相色谱法同时测定地表水中17种硝基苯类和氯苯类化合物

建立了液-液萃取-气相色谱法同时测定地表水中17种硝基苯类和氯苯类化合物的方法.水中的硝基苯类和氯苯美化合物用乙酸乙酯/正己烷(2:1,体积比)混合溶剂提取,经DB-35ms色谱柱分离后用ECD检测.方法灵敏度高,萃取定容后即可进样分析,无需进行高倍浓缩,17种化合物分离良好,检测灵敏度高,水中检出限为0.03～0.08μg/L,比饮用水源地限值低1～4个数量级.本法在40.0～400 μg/L浓度范围内线性相关性良好,方法相对标准偏差为1.4％～5.2％,实际样品加标回收率为96.3％～106％.     

固相萃取-毛细管气相色谱法测定地表水中硝基苯类化合物

建立了固相萃取-毛细管气相色谱测定地表水中硝基苯类化合物的方法，优化了试验条件。方法线性良好，10种硝基苯类化合物的检出限为0．05μg／L～0．15μg／L，实际样品测定的RSD为1．7％～5．0％，平均加标回收率为80．8％～117％。     

测定水中邻苯二甲酸酯类化合物液液萃取法与固相萃取法的选择

文章通过比较测定邻苯二甲酸酯类化合物常用的前处理方法液液萃取法和固相萃取法,主要对比了两种方法的空白干扰和加标回收率实验。实验数据表明:液液萃取法前处理在空白干扰和加标回收率上都优于固相萃取法。     

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%。     

磁性分散固相萃取气相色谱-质谱法测定地表水中邻苯二甲酸酯

本文建立了一种磁性分散固相萃取配合气相色谱-质谱测定地表水中痕量邻苯二甲酸酯的方法。减少了萃取剂的用量、萃取时间、解吸溶剂及盐度对实验结果的影响。在优化条件下,邻苯二甲酸酯类化合物的检出限在0.1～0.7μg/L,回收率在84.2%～111%,相对标准偏差在3.3%～5.5%。与传统的液液萃取及固相萃取相比,该方法具有简便、快捷和灵敏的特点,适用于水中低含量邻苯二甲酸酯类化合物的测定。     

液液萃取-气相色谱法测定水中硝基氯苯类化合物

建立了液液萃取-气相色谱法测定水中15种硝基氯苯类化合物的方法。中性条件下,在水样中加入氯化钠,用环己烷进行萃取,得到方法检出限为0.019~0.044μg/L,在10.0μg/L~1.0 mg/L范围内线性良好,相关系数均0.999。加标水平为2.5μg/L时,空白水样加标回收率为74.8%~104%,相对标准偏差为4.79%~11.5%;实际水样加标回收率为69.1%~111%,相对标准偏差为5.83%~17.6%。方法适用于成分不复杂的实际水样中硝基氯苯类化合物的检测。     

气溶胶PM2.5中内分泌干扰物酞酸酯类的研究

通过选择17种酞酸脂的目标化合物的特征离子对PM2.5样品进行特征离子的扫描,有效建立了高灵敏度的PM2.5酞酸脂类(PAE)的GC-MS-SIM的测定方法;检出限均达到了ng级的水平。气溶胶PM2.5中酞酸脂类(PAE)的污染特征:清洁对照点以邻苯二甲酸二丁酯(DBP)为主;二类区以邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二丁酯(DBP)占主导成分。     

固相萃取-气相色谱法测定水环境中邻苯二甲酸酯

采用固相萃取法对水样进行提取富集,气相色谱法测定水中6种邻苯二甲酸酯类有机污染物,并对方法进行了探索、优化和验证。对水体pH在固相萃取过程中对邻苯二甲酸酯萃取回收率的影响进行了研究,解决了邻苯二甲酸2-乙基己基酯和邻苯二甲酸二正辛酯回收率不高的问题。在空白水加标实验中,邻苯二甲酸酯的回收率能达到93.2%~116.3%。除此之外,还对工业废水和地表水进行了加标回收实验,获得了较高的回收率及测定精度。     

化工废水中邻苯二甲酸酯的研究

对北京市五个化工厂的废水中8种邻苯二甲酸酯类环境激素进行分析和调查研究.在化工废水中普遍检出的邻苯二甲酸酯有邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二环己酯(DCHP),其中邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二正丙酯(DPrP)、邻苯二甲酸二戊酯(DAP)和邻苯二甲酸二正己酯(DHP)4种物质未检出.废水中DEHP和DBP的浓度均低于排放标准.     

土壤中酞酸酯类化合物监测方法的质量控制研究

从监测结果控制的角度对近10年的土壤中PAEs监测方法进行了探讨,重点比较了索氏萃取柱净化GC/MS、微波萃取柱净化GC、加速溶剂萃取柱净化GC/MS和加速溶剂萃取GPCGC/MS方法的检出限、精密度和准确度。旨在为中国土壤监测方法的建立提供基础支撑,为开展质量控制工作提供评价依据。     

Phthalates removal efficiency in different wastewater treatment technology in the Eastern Cape,South Africa

The removal capacity of different wastewater treatment plant (WWTP) technologies adopted in rural areas for phthalate was investigated in the Eastern Cape, South Africa. Wastewater samples collected from three selected WWTPs which use activated sludge (AS), trickling filter (TF), and oxidation pond (OP) technology were extracted using the solid-phase extraction method followed by gas chromatography-mass spectrometry (GC-MS) analysis. The six selected phthalate esters (PAEs) dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di(2-ethyl hexyl) phthalate (DEHP), and di-n-octyl phthalate (DOP) were detected in all the samples collected from the WWTPs. DBP was the most abundant compound in the influent, effluent, and sludge samples with a maximum detection of 2497 μgL^?1, 24.2 μgL^?1, and 1249 μg/g dW, respectively, followed by DEHP and BBP. There was a relatively high removal capacity achieved by AS in Alice, TF in Berlin, and OP in Bedford with a removal efficiency that varied between 77 and 99%, 76 and 98%, and 61 and 98%, respectively. A high significant correlation of PAE removal with total suspended solids (TSS) and turbidity suggests that the removal performance proceeded more through adsorption on settling particles and sludge than on biodegradation. However, the concentrations of PAEs detected in the final effluent and sludge samples exceeded acceptable levels allowed internationally for a safe aquatic environment. AS may have exhibited a more stable and better performance across the different seasons; however, pollution source control still deserves a special attention to prevent the risk posed by these micropollutants.     

北京公园水体中邻苯二甲酸酯类物质的测定及其分布特征

为了正确评估北京市公园水体受PAEs污染的程度,采集了北京11个公园湖水的水样,采用固相萃取-气相色谱联用技术检测了其中六种邻苯二甲酸酯类物质(PAEs)的含量,该方法加标回收率在73%～89.3%,RSD为5.9%～18.1%,检出限在0.40～4.58mg/L。实验结果为北京公园水体中总PAEs浓度在6.4～138.1μg/L,平均值为27.9μg/L,证明北京公园水体受到不同程度的PAEs污染,主要的污染物为邻苯二甲酸二丁酯(DBP)和邻苯二甲酸双(2-乙基己基)酯(DEHP),其中东南部以及西北部的公园污染较严重。分析了PAEs在公园湖水底泥中和水体中的分布特征,结果显示,PAEs在湖水底泥中的含量明显大于在水体中的含量。     

漓江桂林段酞酸酯类污染调查

对漓江桂林段酞酸酯类污染为期一年的调查结果表明，漓江桂林段已检出酞酸酯，并且河水中酞酸酯含量的高低与环境温度有直接关系，气温高时，河水中酞酸酯含量高，当河流流泾城市时，大量生活废水的汇入，不会导致河水中酞酸酯含量的增加。     

Impact of irreversible sorption of phthalate acid esters on their sediment quality criteria

The equilibrium partitioning (EqP) method has been applied to establish sediment quality criteria (SQC); however, it does not consider the nonlinear irreversible sorption of many organic contaminants. In this research, the sorption and desorption of two phthalate esters (PAEs), dimethyl phthalate (DMP) and di(2-ethylhexyl) phthalate (DEHP), in four natural sediments collected from the Yangtze River and the Yellow River were studied; the impact of irreversible sorption of DMP and DEHP on SQC has been evaluated. Based on the reversible and irreversible biphasic sorption model, the values of maximum irreversible sorption capacity (q(max)(irr)) were 125.19 μg g(-1)-337.37 μg g(-1) for DMP and 515.87 μg g(-1)-591.40 μg g(-1) for DEHP. The q(max)(irr) value was positively related to the organic carbon and black carbon contents, cation exchange capacity, and surface area of the sediments. The values of the irreversible sorption coefficient K(oc)(irr) for both DEHP and DMP in the four sediments approximated to a constant of 10(6.46 ± 0.38), which was 1-2 orders of magnitude higher than their reversible sorption coefficient K(oc)(irr). The values of SQC for PAEs based on the EqP method were modified by involving the irreversible sorption. The modified SQC of DEHP could be 2 to 20 times higher than the value predicted by the EqP method, and the assessment results for DEHP contamination in the sediments with the modified SQC were more reasonable than those with the non-modified SQC. It indicated that the current SQC based on the EqP method may be unnecessarily strict for specific organic compounds and the irreversible sorption should be taken into account.     

Organophosphate and phthalate esters in indoor air: a comparison between multi-storey buildings with high and low prevalence of sick building symptoms

An extensive study has been conducted on the prevalence of organophosphorous flame retardants/plasticizers and phthalate ester plasticizers in indoor air. The targeted substances were measured in 45 multi-storey apartment buildings in Stockholm, Sweden. The apartment buildings were classified as high or low risk with regard to the reporting of sick building symptoms (SBS) within the project Healthy Sustainable Houses in Stockholm (3H). Air samples were taken from two to four apartments per building (in total 169 apartments) to facilitate comparison within and between buildings. Association with building characteristics has been examined as well as association with specific sources by combining chemical analysis and exploratory uni- and multivariate data analysis. The study contributes to the overall perspective of levels of organophosphate and phthalate ester in indoor air enabling comparison with other studies. The results indicated little or no difference in the concentrations of the target substances between the two risk classifications of the buildings. The differences between the apartments sampled within (intra) buildings were greater than the differences between (inter) buildings. The concentrations measured in air ranged up to 1200 ng m(-3) for organophosphate esters and up to 11?000 ng m(-3) for phthalate esters. Results in terms of sources were discerned e.g. PVC flooring is a major source of benzylbutyl phthalate in indoor air.     

Flame ionization gas chromatographic determination of phthalate esters in water, surface sediments and fish species in the Ogun river catchments, Ketu, Lagos, Nigeria

The detection and quantification of four phthalate esters??dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), and diethylhexyl phthalate (DEHP)??in water, sediment, and some fish species were carried out using flame ionization gas chromatography. The samples were collected from the Ogun river catchments, Ketu, Lagos. The DMP was not detected in the water and fish samples but was detected in sediments collected from four of the six sampling sites. The concentration of DEP, DBP, and DEHP in the fish species ranged from 320.0?C810.0, 380.0?C1,080.0, and 40.0?C150.0 ??g/kg in Tilapia sp.; 310.0?C860.0, 400.0?C1,170.0, and 40.0?C110.0 ??g/kg in Chrysichthys sp.; and 320.0?C810.0, 400.0?C3,970.0, and 30.0?C300.0 ??g/kg (DEHP) in Synodontis sp., respectively. The differences in fish phthalate levels are not statistically significant at p?<?0.05, an indication that phthalate esters accumulation is not fish species dependent. The DEP, DBP, and DEHP values recorded are considerably higher than the maximum allowed concentrations for drinking water prescribed by the US Environmental Protection Agency. The phthalate pollution index and biosediment accumulation factor values were also calculated.