工业废水锑排放标准限值的制订

分析了国内外锑标准的研究现状,总结了工业废水锑排放标准的制订原则,并以太湖流域某湖泊水体为例,介绍了工业废水锑排放标准限值的制订流程。通过建立环境容量模型,计算区域水体允许纳污量,推算出在上游来水为极端最枯流量、枯水年平均流量、平水年平均流量情形下,研究区域内相关企业允许排放到水体中的锑质量浓度分别为19.10μg/L、28.47μg/L、48.92μg/L。考虑最不利情形,兼顾锑污染处理的技术经济可行性,建议直排点源及印染废水集中式污水处理厂的出水锑质量浓度标准限值为20μg/L。     

长江干流江苏段水质中邻苯二甲酸酯的测定及分布现状

采用气相色谱-质谱联用法测定水质中6种邻苯二甲酸酯(PAEs),方法在0μg/L~500μg/L范围内线性良好,方法检出限为15 ng/L~20 ng/L。将该方法用于2014年长江干流江苏段4个断面的水质样品的采集与测定,并讨论PAEs的分布现状。结果表明,6种PAEs的测定均值为8.56μg/L~21.1μg/L,其中DBP与DEHP含量占比超过50%,PAEs总质量浓度与其他河流相比基本处于同一水平。     

高效液相色谱法测定地表水中四乙基铅

系统研究了地表水中四乙基铅的液相色谱分析方法,水中四乙基铅经二氯甲烷萃取浓缩后,用高压液相色谱柱分离,在280 nm波长处检测,根据保留时间定性,外标法定量,检出限及测定下限分别为0.02μg/L和0.06μg/L,低于地表水限值0.1μg/L,地表水平行测定的相对标准偏差均小于5%,地表水和废水样品加标回收率分别为79.4%～82.0%和62.5%～106.6%。     

深圳主要河流中雌激素污染调查

调查了深圳市10条主要河流雌激素污染现状,结果表明,双酚A在深圳市河流中28个监测点中27个点有检出,检出率96.4％,质量浓度为未检出～6.042 μg/L;17β雌二醇(E2)在深圳市河流中28个监测点中8个点有检出,检出率28.6％,质量浓度为未检出～0.011 6μg/L,能检出的17β雌二醇(E2)值大都在0.001 5μg/L～0.003 9 μg/L之间;雌三醇(E3)仅在1个监测点(新洲河河口)有检出,对壬基酚均未检出.     

气相色谱法测定地表水中百菌清和菊酯类农药

采用正己烷萃取地表水中的百菌清和6种菊酯类农药,通过毛细管气相色谱法-电子捕获检测器(GC-ECD)定性定量。供试农药的线性范围:百菌清为10.0μg/L～200μg/L,6种菊酯类为50.0μg/L～1 000μg/L;方法检出限分别为:百菌清0.054μg/L,甲氰菊酯0.62μg/L,三氟氯氰菊酯0.68μg/L,氯菊酯0.40μg/L,氯氰菊酯0.65μg/L,氰戊菊酯0.78μg/L,溴氰菊酯0.15μg/L;对地表水样品3个质量浓度水平的平均加标回收率为91.3%～118%,6次平行测定的RSD<5%。     

微波消解-电感耦合等离子体质谱法同时测定废水中20种元素

采用微波消解-电感耦合等离子体质谱法,同时测定了废水中Be、V、Cr、Mn、Co、Ni、Cu、Zn、As、Se、Mo、Ag、Cd、Sb、Ba、Hg、Tl、Pb、Th、U等20种元素,比较了5种不同消解体系对废水样品的加标回收结果,确定采用硝酸+过氧化氢消解体系。Hg在0.050μg/L～2.00μg/L、其他元素在5.00μg/L～500μg/L范围内线性良好,检出限为0.01μg/L～0.2μg/L,国家有证标准物质的测定结果符合要求,废水样品平行测定的RSD为2.6%～6.5%,加标回收率为84%～110%。     

气动进样原子荧光法测定环境水样中痕量汞和砷

以硼氢化钾作为还原剂原子荧光法测定环境水样中的汞和砷,配合以气动进样,方法简单、试剂用量少、灵敏度高.测汞时KBH4-KOH浓度为0.01%～0.0005%,样品中王水浓度3%(v/v),检测限为5.8×10-3μg/L;测砷时KBH4-KOH浓度为2.6%～1.0%,样品中盐酸浓度5%(v/v),检测限为4.9μg/L.     

全自动固相萃取气质联用法测定废水中硝基苯类化合物

采用全自动固相萃取处理废水,气相色谱-质谱联用法测定废水中的15种硝基苯类化合物,通过优化试验条件,使方法在0.100mg/L～10.0mg/L范围内线性良好。方法检出限为0.012μg/L～0.038μg/L,标准溶液11次测定结果的RSD为1.0%～7.5%。对实际水样做2个质量浓度水平的加标回收试验,平均加标回收率为78.0%～107%。     

HPLC-ICP/MS联用测定废水中甲基汞和无机汞

采用高效液相色谱(HPLC)-电感耦合等离子体质谱(ICP/MS)联用测定废水中可滤态的甲基汞和无机汞,优化了仪器工作条件,讨论了方法干扰及校正办法。甲基汞和无机汞在0.500μg/L~25.0μg/L范围内线性良好,检出限分别为0.03μg/L和0.07μg/L,废水样品平行测定的RSD分别为6.5%~7.6%和6.2%~6.8%,加标回收率分别为84.0%~87.0%和88.0%~92.4%。     

HPLC-MS/MS法测定三角帆蚌中多种N-亚硝胺类化合物

采用基质分散固相萃取-同位素稀释-HPLC-MS/MS法同时测定三角帆蚌肉中9种N-亚硝胺类化合物(NAs),通过优化前处理和仪器条件,使方法在5.00μg/L～200μg/L范围内线性良好,方法检出限为2.58μg/kg～8.86μg/kg。对样品做2个质量比水平的加标回收试验,各组分的平均回收率为78.1%～90.3%,RSD值≤6.8%。将该方法用于测定20个河蚌样品,9种NAs均为未检出。     

电导和直流安培双检测器离子色谱法测定清洁水样中的碘化物

选用配备了2种不同检测器(电导检测器和直流安培检测器)的离子色谱仪对稀释后过0.22μm滤膜的水样进行分析。配备有直流安培检测器的离子色谱仪测定水中碘化物的方法在0.100~20.0μg/L范围内线性关系良好,相关系数(r)=0.9999,方法检出限为0.030μg/L,测定下限为0.120μg/L,样品加标回收率为95.0%~104%,相对标准偏差为1.06%~1.64%;配备有电导检测器的离子色谱仪测定水中碘化物的方法在20.0~2.00×105μg/L范围内线性关系良好,相关系数(r)=0.9995,方法检出限为2.00μg/L,测定下限为8.00μg/L,样品加标回收率为99.0%~110%,相对标准偏差为0.71%~3.12%。离子色谱-直流安培检测器法测定水中碘化物的方法准确度高、灵敏度高、精密度好,检出限相对较低,适用于测定ρ(碘化物)≤20.0μg/L的清洁水样;离子色谱-电导检测器法主要适用于测定ρ(碘化物)≥20.0μg/L的水样。     

自动进样系统结合分光光度法快速测定水质中总磷

基于自动进样系统结合分光光度法,通过对波长、消解条件及显色条件的优化,建立了水中总磷的快速检测分析方法。在优化条件下,总磷的检出限为0.005 mg/L,测定下限为0.020 mg/L。对地表水、生活污水和工业废水3种不同基质的样品进行了加标测定,其回收率为95.0%~102%,相对标准偏差为0.5%~2.7%;与国标方法钼酸铵分光光度法测定水体中总磷进行比对研究,对国家有证标准样品、地表水、生活污水和工业废水测试的结果显示,方法相对偏差为0.4%~3.5%。该方法操作简单、快速、准确,可为应对突发环境事件中总磷的测定提供技术参考。     

Tracking sewage derived contamination in riverine settings by analysis of synthetic surfactants

A study has been made of the presence and reactivity of the most commonly used surfactants, both anionic (linear alkylbenzene sulfonates, LAS, and alkyl ethoxysulfates, AES) and non-ionic (alcohol polyethoxylates, AEOs, and nonylphenol polyethoxylates, NPEOs), in water and surface sediments from the middle stretch of the Guadalete River in SW Spain (12 stations). Average values were between 0.1 and 3.7 mg kg(-1) in sediment, and between 0.2 and 37 μg L(-1) in water. The sorption of surfactants was dominated by hydrophobic mechanisms, so those homologues having longer alkyl chains (e.g. C(18)AEO) showed higher relative percentages and concentrations in sediments compared with water. Local and sharply higher concentrations of these compounds were observed at three sampling stations (7, 9 and 12), indicating the occurrence of wastewater discharges into the river. By analysing the distributions of different surfactant homologues and their metabolites we were able to distinguish between sewage contamination from sources discharging treated and untreated wastewaters. Upstream (stations 1-2), LAS concentrations were below 30 μg L(-1) and the composition of their degradation intermediates (sulfophenyl carboxylic acids, SPCs) (160 μg L(-1)) was dominated by short-chain homologues (C(6)-C(9)SPCs), indicating that the degradation of this surfactant is at an advanced stage. The highest concentration (487 μg L(-1)) of SPCs was detected near the effluent outlet of a sewage treatment plant (STP) (station 12). Sampling stations (7 and 9) affected by untreated wastewater discharges were the only ones showing the presence of the most reactive and biodegradable SPC isomers and homologues (e.g. C(11)SPC). Here, LAS reached the highest concentration values measured (>2 mg L(-1)), and showed a homologue distribution closer to that of commercial mixtures than LAS found at the other stations.     

液液萃取-气相色谱/串联质谱法测定水中五氯酚及其钠盐

采用液液萃取处理水样,用气相色谱-串联质谱法测定样品中五氯酚及其钠盐,通过优化测定条件,使方法在1.00μg/L~500μg/L范围内线性良好。检出限和定量限分别为1.00μg/L和5.00μg/L,空白水样五氯酚钠3个质量浓度水平的加标回收率为89.8%~98.4%,5次平行试验测定结果的RSD为5.5%~10.7%。     

HPLC-FLD determination of 4-nonylphenol and 4-<Emphasis Type="Italic">tert</Emphasis>-octylphenol in surface water samples

A simple, sensitive and reliable HPLC-FLD method for the routine determination of 4-nonylphenol, 4-NP and 4-tert-octylphenol, 4-t-OP content in water samples was developed. The method consists in a liquid–liquid extraction of the target analytes with dichloromethane at pH  3.0–3.5 followed by the HPLC-FLD analysis of the organic extract using a Zorbax Eclipse XDB C8 column, isocratic elution with a mixed solvent acetonitrile/water 65:35, at a flow rate of 1.0 mL/min and applying a column temperature of 40°C. The method was validated and then applied with good results for the determination of 4-NP and 4-t-OP in Ialomi?a River water samples collected each month during 2006. The concentration levels of 4-NP and 4-t-OP vary between 0.08–0.17 μg/L with higher values of 0.24–0.37 μg/L in the summer months for 4-NP, and frequently <0.05 μg/L but also between 0.06–0.09 μg/L with higher values of 0.12–0.16 μg/L in July and August for 4-t-OP and were strongly influenced by sesonial and anthropic factors. The method was also applied on samples collected over 2 years 2007 and 2008 from urban wastewaters discharged into sewage or directly into the rivers by economic agents located in 30 Romanian towns. Good results were obtained when the method was used for analysis of effluents discharged into surface waters by 16 municipal wastewater treatment plants, during the year 2008.     

SPE-GC-MS/MS法测定水源水中多种有机氯EDCs

采用C 18柱固相萃取(SPE)-三重四级杆气相色谱-质谱法同时测定水中18种含有机氯的环境内分泌干扰物,方法在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.04 ng/L^0.8 ng/L,空白水样的加标回收率为61.3%~108%,6次测定结果的RSD为3.8%~18.0%。将该方法用于饮用水源水监测,18种目标化合物的测定值为未检出~1.5 ng/L,平均加标回收率为71.9%~109%,平行测定结果的RSD<15%。     

Wastewater quality of natural gas fertilizer factory, Fenchuganj and water quality of Kushiara River at the down stream

The physical, chemical and biological characteristics of the wastewater of Natural Gas Fertilizer Factory Ltd. Fenchuganj, Sylhet were determined through extensive laboratory tests in the months of March, July, October and December of the year 2005. Concentration of Suspended Solids was within the range of 445 to 950 mg/L. Bangladesh Industrial Effluent Standards for Suspended Solids is 100 mg/L. Suspended Solids were found above the limit in all the samples. Concentration of Dissolved Solids was found to vary from 576 to 1,456 mg/L. Bangladesh Industrial Effluent Standards, for Dissolved Solids is 2,100 mg/L. Dissolved Solids were found within the limit. Concentration of BOD(5) was found to vary from 4.5 to 8.4 mg/L. Bangladesh Industrial Effluent Standards for BOD(5) is 50 mg/L. For the year 2005, the BOD(5) was found below the limit in all the samples. Dissolved Oxygen of the wastewater was found to be between 2.0 to 3.0 mg/L, which do not satisfy the standard (4.5-8 mg/L). Oil and grease concentration were found in the range of 28 to 68 mg/L, whereas the standard is 10 mg/L for discharge into the inland surface water. In 2005, concentration of Cr(+ 6) was found to vary from 0.01 to 0.156 mg/L in the wastewater. Bangladesh Industrial Effluent Standards, for Cr(+6) is 0.1 mg/L. The concentration of chromium was found above the limit in three samples. Concentration of NO(3) was found to vary from 4.5 to 15.2 mg/L in the wastewater. Bangladesh Industrial Effluent Standards for nitrate is 10 mg/L. The nitrate was found above the limit in three samples. Maximum concentration of ammonia in lagoon 1 was found 1,710 mg/L in month of December. Bangladesh Industrial Effluent Standards for ammonia nitrogen is 100 mg/L. For the year 2005, the ammonia nitrogen was found above the limit in all samples.     

气相色谱-电子捕获法直接测定水体中的五氯酚钠

建立了不经衍生直接测定水体中五氯酚钠残留量的气相色谱-电子捕获(GC-ECD)方法。用乙酸乙酯提取目标化合物,浓缩后上机测定。五氯酚钠标准溶液的线性范围在0.35～400μg/L之间,相关系数为0.9992;池塘水中五氯酚钠的添加浓度为1.0、5.0、10.0μg/L时,其加标回收率为95.8%～98.7%,相对标准偏差≤3.6%;检出限(信噪比为3时)为0.35μg/L,定量限(信噪比为10时)为1.0μg/L。     

毛细管柱气相色谱法测定水质五氯酚

用乙酸酐衍生，正己烷液一液萃取，毛细管柱气相色谱-电子捕获检测器对地表水、废水中五氯酚进行了测定，确定五氯酚浓度范围在5．0—500μg/L之间时，样品的测定精度、回收率及方法检出限均能满足要求。