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1.
进样溶剂极性对地下水中有机氯农药色谱行为的影响 总被引：2，自引：2，他引：0
地下水中有机氯农药分析时采用正己烷为进样溶剂,而考核样品的溶剂通常为甲醇。正己烷和甲醇分别是典型的非极性溶剂和极性溶剂。文章研究了正己烷和甲醇两种溶剂对地下水中9种必测有机氯农药(六氯苯、α-六六六、β-六六六、γ-六六六、δ-六六六、p,p′-DDE、p,p′-DDD、o,p′-DDT、p,p′-DDT)色谱行为的影响。结果表明,溶剂的极性对有机氯农药的响应值有显著的影响:甲醇为进样溶剂时,由于极性强,造成汽化室内活性位点的暴露,导致某些待测组分被活性位点吸附,甲醇相的待测物响应值明显低于正己烷相待测物响应值。 相似文献
2.
微波萃取-气相色谱/气相色谱-质谱法测定土壤中18种有机氯农药 总被引：4，自引：3，他引：1
采用微波萃取-Florisil固相萃取柱净化分离、气相色谱和气相色谱-质谱相结合的方法测定土壤中的痕量半挥发性有机氯农药。优化了微波萃取和固相萃取柱净化条件,在最优条件下18种有机氯农药(α-HCH、β-HCH、γ-HCH、δ-HCH、七氯、艾氏剂、环氧七氯、硫丹Ⅰ、p,p′-DDE、狄氏剂、异狄氏剂、硫丹Ⅱ、p,p′-DDD、o,p′-DDT、异狄氏剂醛、硫丹硫酸酯、p,p′-DDT、甲氧滴滴涕)的回收率在89.56%~114.22%。对气相色谱和气相色谱-质谱法的仪器检出限、回收率、精密度和方法检出限进行对比,确定了采用气相色谱-质谱定性和气相色谱定量相结合的方法,测定实际土壤样品中的有机氯农药,使得定性和定量的准确度都得到提高。 相似文献
3.
2005年4月至2006年3月,利用大流量采样器采集青岛大气中气相和颗粒相样品,并分析气相和颗粒相中的有机氯农药(OCPs).结果表明,青岛大气中α-HCH、y-HCH、HCB、o,p′-DDT、p,p′-DDT和p,p ′-DDE的浓度平均值分别为(78±41) pg/m3、(289±236) pg/m3、(221±186) pg/m3、(81±62) pg/m3、(54±49) pg/m3和(60±44)pg/m3,远低于广州、天津等城市.大气中的有机氯农药浓度在一定程度上受温度影响,但相关系数并不高(R2＜0.4),斜率较缓,表明大气的长距离迁移对其浓度也有一定的影响.用后向气流轨迹法对气团来源追踪,发现当青岛受到东亚沙尘暴的影响时,有机氯农药的浓度升高,而当有来自黄海较干净的气团到达青岛时,大气中有机氯农药的浓度明显偏低. 相似文献
4.
采用5个浓度水平样品通过7家实验室进行协同评定试验,验证了地下水中六氯苯、α-HCH、β-HCH、γ-HCH、δ-HCH、p,p’-DDE、p,p’-DDD、o,p’-DDT、p,p’-DDT有机氯农药分析方法的稳定性与准确性。测量结果经一致性和离群值检验表明,地下水中9种有机氯农药组分在3.00～56.5 ng/L浓度水平范围内,重复性标准差为0.50～0.77 ng/L,再现性标准差为1.92～3.03 ng/L,单个样品中的2,4,5,6-四氯间二甲苯和二丁基氯菌酸酯替代物质量监控指标回收率分别为58.8%～99.5%和79.2%～117%。检测方法准确、可靠。 相似文献
5.
中国典型类型土壤中有机氯农药和多氯联苯成分分析标准物质的研制 总被引：3，自引：2，他引：1
目前我国有1个有机氯农药(OCPs)分析标准物质,3个多氯联苯(PCBs)分析标准物质;欧洲有1个OCPs分析标准物质和2个PCBs分析标准物质。美国、国际原子能机构和日本等组织研制了沉积物中OCPs、PCBs和多环芳烃的有机分析标准物质,这些标准物质的基质性质、浓度水平与我国地质样品基质性质、实际污染情况不符。本文针对我国土壤类型的分布特点、污染特征及实际样品检测情况,采集典型地区的土壤作为候选物,利用传统的气相色谱-质谱法、气相色谱-串联质谱法、气相色谱-电子捕获检测器法和现代分析技术方法——同位素稀释质谱法,严格按照国家一级标准物质技术规范和相关标准研制了6个土壤有机分析标准物质(编号为GBW07469~GBW07474),基本涵盖了我国典型土壤类型,包括褐土、水稻土、黄壤土和草甸土;定值化合物包括全国地质大调查必测的8种OCPs(α-HCH、β-HCH、γ-HCH、δ-HCH、p,p’-DDE、p,p’-DDD、o,p’-DDT、p,p’-DDT)和选测的7种PCBs(PCB28、52、101、118、153、138、180),含量范围为3.9μg/kg~2.31 mg/kg。此批标准物质的基质性质、目标组分的浓度水平和污染特征与实际环境样品具有较好的一致性,而且目标物种类多,含量范围宽,可以满足我国不同地区、不同程度污染的土壤样品中OCPs和PCBs同时测定的质量监控需求。 相似文献
6.
气相色谱-质谱在地下水检测过程中的重要性 总被引：1，自引：1，他引：0
采用气相色谱法、高效液相色谱法、气相色谱-质谱法对地下水样品中α-HCH、β-HCH、γ-HCH、δ-HCH、p,p’-DDE、p,p’-DDD、o,p’-DDT、p,p’-DDT、六氯苯、苯并(a)芘等组分进行测定时,通过气相色谱-质谱在测量复杂基体待测样品组分中的识别作用、在高浓度待测样品组分检测中的确认作用以及对样品检测结果假阳性现象的判断作用等内容,论证了气相色谱-质谱技术在测定复杂基体或高浓度地下水样品过程中的重要性,确保了地下水调查项目测量数据准确可靠。 相似文献
7.
吉林省中部土壤有机氯农药的含量及组成 总被引：11，自引：0，他引：11
用气相色谱法对吉林省中部土壤样品中有机氯农药的分析结果表明,吉林省中部土壤中有机氯农药以六六六(HCH)和滴滴涕(DDT)为主,艾氏剂、氯丹、狄氏剂、异狄氏剂和七氯等也有不同程度的检出。总DDT含量为0.02～69.35μg/kg,平均含量为3.01μg/kg;总HCH含量为0.47～13.47μg/kg,平均含量为2.00μg/kg。p,p′-DDE和p,p′-DDD为DDT的主要存在形式,主要为过去输入的DDT的降解产物,但近期仍有少量DDT的输入;HCH的4种异构体中以β-HCH为主,α-HCH与γ-HCH的比值较低,表明HCH在土壤中残留的时间很长。 相似文献
8.
9.
9种有机氯农药(α-HCH、β-HCH、γ-HCH、δ-HCH、六氯苯、p,p’-DDE、p,p’-DDD、o,p '-DDT和P,p’-DDT)和7种指示性多氯联苯(PCB 28、PCB 52、PCB 101、PCB 118、PCB 138、PCB 153和PCB 180)是我国地下水水质调查的必测和选测的持久性有机污染物.目前采用的气相色谱-电子捕获检测器和气相色谱-质谱-选择离子监测分析技术,无法对地下水中这16种痕量和超痕量典型含氯持久性有机污染物进行准确的定性和定量分析.本文建立了地下水中16种典型含氯持久性有机污染物的固相圆盘萃取-气相色谱-高分辨质谱分析方法,目标物检出限为0.10 ～0.20 ng/L,基体加标回收率为61.9％ ～93.3％,精密度(RSD,n=5)为2.41％ ～20.0％,能够对地下水中痕量目标物进行准确定性和定量.应用该方法检测了两个地区16个地下水样品中的目标物.结果表明,两地实际样品中均未检出多氯联苯,而普遍检出急性毒性最强的γ-HCH和致癌活性最高的α-HCH,根据α-HCH和γ-HCH浓度的比值可以初步判断,两个地区的地下水样品有受到新的HCH排放源污染的可能性. 相似文献
10.
柳州岩溶地下河水体有机氯农药分布特征 总被引：6，自引：3，他引：3
采用气相色谱(配ECD检测器)对柳州鸡喇和龙寨两条岩溶地下河不同位置水体中18种有机氯农药(OCPs)组分进行分析。结果表明,除异狄氏剂醛外,其余17种OCPs均有不同程度检出,OCPs浓度变化范围为107.68～1101.55ng/L,均值为532.515ng/L。OCPs主要组分为:α-HCH、β-HCH、γ-HCH、δ-HCH、p,p'-DDE、o,p'-DDT、p,p'-DDD、p,p'-DDT、六氯苯、七氯、艾氏剂。其中DDTs和HCHs含量最高,二者之和占到总OCPs的75.8%～96%。对其污染源进行分析,发现地下河水体中DDTs主要源自土壤。HCHs来源相对复杂,可能源于工业品或者长距离大气运输,也可能是近期有林丹的输入使其浓度增高。与国内外各水体相比,本次研究的两条岩溶地下河有机氯农药含量相对较高。 相似文献
11.
山东烟台地区苹果果园土壤中DDTs和HCHs残留分布特征与来源解析 总被引：1，自引：1，他引：0
为研究不同土壤类型中有机氯农药的残留特征、降解程度和来源途径,采集了山东烟台9个不同地质单元苹果园根系土壤和剖面土壤样品,用电子捕获检测器气相色谱法测定其中的滴滴涕(DDTs)和六六六(HCHs)。结果表明,研究区所有类型根系土壤中DDTs和HCHs均未超出《土壤环境质量标准》的二级土壤限值(500 ng/g);土壤中DDTs的残留量及检出率均高于HCHs,DDTs检出率为100%,平均残留量为71.7ng/g,而HCHs的检出率为19.70%,平均残留量为7.9 ng/g;根系土壤中DDTs各异构体平均浓度依次为p,p’-DDT>p,p’-DDE>o,p’-DDT>p,p’-DDD,而HCHs大部分以α-HCH形式存在,部分以β-HCH、γ-HCH存在。不同类型土壤中有机氯农药残留分布特征明显不同:DDTs在棕壤土(臧家庄)中最高(145.5 ng/g),在中粗粒砂土(武宁)中最低(24.1 ng/g);而HCHs在细砂质壤土(蛇窝泊)中最高(27.9ng/g)。各剖面土壤DDTs均在<20 cm层位中残留最高。DDTs和HCHs来源解析表明:研究区土壤为好氧条件;麻砂棕壤(官道和桃村)、黏细壤土(牟平)、细砂质壤土(蛇窝泊)和棕壤土(臧家庄)近年来仍有新的DDTs输入;大部分根系土壤均未发现HCHs新来源,但麻砂棕壤(桃村)在HCHs禁用后可能仍存在林丹的使用。 相似文献
12.
Norma Tombesi Karla Pozo Andrés Arias Mónica Alvarez Petra Pribylova Ondrej Audy Jana Klánová 《Environmental Earth Sciences》2018,77(11):403
The present study fills a gap in the knowledge in regards to the occurrence of banned pesticides at both coastal and inland locations at the Southwest Buenos Aires region, Argentina. Superficial sediment and soil samples were collected from different sites along the Bahia Blanca Estuary and surrounding sites to assess the concentration levels and spatial distribution of 12 selected organochlorine pesticides (OCs); 13 spatial locations including inland and shore-coast were sampled to evaluate occurrence and concentration levels of hexachlorocyclohexanes α-HCH, β-HCH, δ-HCH, γ-HCH, dichlorodiphenyltrichloroethane and its degradation products (DDXs: p,p′-DDT, o,p′-DDT, p,p′-DDE, o,p′-DDE, p,p′-DDD, o,p′-DDD) and the polychlorobenzenes PeCB (pentachlorobenzene) and HCB (hexachlorobenzene). After cleaning and extractions steps, samples were analyzed by means of gas chromatography/mass spectrometry. ∑OCs (sum of all studied compounds) ranged between 0.206 and 1040 ng g?1 dw (mean?=?82.4 and SD?=?277 ng g?1 dw). Total HCHs (sum of α-HCH, β-HCH, γ-HCH and δ-HCH) ranged from 0.0858 to 0.876 ng g?1 dw (mean?=?0.43 and SD?=?0.23 ng g?1 dw), DDXs (sum of p,p′and o,p′ isomers) from 0.080 to 1040 ng g?1 dw (mean?=?81.3 and SD?=?277 ng g?1 dw). Lower concentrations were found for PeCB (mean?=?0.095 and SD 0.17 ng g?1 dw) and HCB (mean?=?0.56 and SD 1.7 ng g?1 dw). Principal component analysis (PCA) permitted the extraction of underlying information about common factors, providing an overview of the distribution of pesticides and allowing the characterization of sites in regards to the major pesticide signature. 相似文献
13.
Distribution and potential sources of organochlorine pesticides in the karst soils of a tiankeng in southwest China 总被引：1，自引：0，他引：1
Yinghui Wang Yiyin Xu Shihua Qi Xiaoming Li Xiangsheng Kong Daoxian Yuan Oramah I. Theodore 《Environmental Earth Sciences》2013,70(6):2873-2881
This research was conducted in an attempt to assess the concentration levels and potential sources of organochlorine pesticides (OCPs) in the karst soils of Dashiwei tiankeng, southwest China. The tiankeng is a karst surface expression that can act as a focal point for introduction of contaminants to groundwater system, which may serve as condenser and receiver for semi-volatile persistent organic pollutants such as OCPs. In this study, surface soil samples from Dashiwei tiankeng were collected and 23 organochlorine pesticide compounds were analyzed. The results showed that the concentration was 0.019–3.605 ng/g for DDTs (sum of p,p’-DDD, p,p’-DDE, o,p’-DDT, p,p’-DDT), 0.001–0.218 ng/g for HCHs (sum of α-, β-, γ-, δ-HCH), 0.003–0.290 ng/g for CHLs (sum of heptachlor, heptachlor epoxide, TC, CC and trans-nonachlor), 0.001–0.064 ng/g for endosulfan (sum of α-endosulfan and β-endosulfan), 0.008–1.630 ng/g for HCB and 0.023–0.928 ng/g for other OCPs (sum of aldrin, dieldrin, methoxychlor, endrin, endrin aldehyde and endrin ketone). The total OCPs concentrations varied from 0.055 to 5.216 ng/g. The ratio of DDT/(DDE + DDD) in the floor soils of Dashiwei tiankeng ranged from 0.434 to 0.797, suggesting a mostly historical residue of technical DDT contamination. However, the ratio of DDT/(DDE + DDD) in the upper rim soils was higher than one, which that there was fresh DDT application nearby. Both the floor and upper rim soils of Dashiwei tiankeng had high ratios of o,p’-DDT/p,p’-DDT (range of 0.016–10.833 with mean of 5.424 and 4.667–7.714 with mean of 5.723, respectively), which implied that the primary source of DDTs was probably from dicofol-type DDT products. The average ratios of α-/γ-HCH were 24.435 in the floor soils and 1.067 in the upper rim soils, together with the averaged percentages of β-HCH among the total HCH isomers (accounting for 33.772 %), indicating that the HCHs were a dominant contribution from technical HCH usage in the past. 相似文献
14.
根据《地质矿产实验室测试质量管理规范》的要求,为保证地下水污染调查中样品的准确测定,需采取质量控制方法。文章阐述了地下水样品的前处理和测定过程的质量控制措施,建立了地下水有机组分分析过程的质量控制流程,确保其检测数据达到规范所允许的范围。 相似文献
15.
Determination of HCH and DDT in soils following Wenchuan 5.12 Violent Earthquake in China 总被引：1，自引：0，他引：1
Weiwei Cui Qiangbin Zhang Xianlei Zhu Yunyang Wan Zhihuan Zhang Zhihua Fan Tieguan Wang 《中国地球化学学报》2011,30(1):125-131
A large number of disinfectants and insecticides were used on a large scale after the Wenchuan 5.12 Violent Earthquake. The disinfectants and insecticides, including HCH (hexachlorocyclohexane) and DDT (dichlorodiphenyltrichoroethane) as representative OCPs, could lead to serious environmental problems. In order to disclose the residues of HCH and DDT in soils following the Wenchuan 5.12 Violent Earthquake, surface soils in Dujiangyan City and Beichuan County were sampled in 2009. The samples were analyzed by GC/MS after pre- treatment by ultrasonic solvent extraction. It has been found that the concentra-tions of γ-HCH, β-HCH and 4,4’-DDT in soils of Beichuan County were 94–102.4, 14.1–36.1 and 2.9–4.3 times high their concentrations in those of the Wolong Nature Reserve, and the concentrations in soils of Dujiangyan City were 52.4–61.6, 8.8 –45.3 and 5.4–6.2 times high their concentrations in soils of the Wolong Nature Reserve, respectively. According to the isomers of HCHs and metabolites of DDTs, it could be concluded that these areas may have additional inputs of lindane and 4,4’-DDT. 相似文献