气相色谱质谱联用技术在饮用水源地挥发性有机物特定项目中的应用研究

地表水环境质量标准(GB 3838-2002)中规定的集中式生活饮用水地表水源地特定项目中有20多项属于挥发性有机污染物,研究了吹扫捕集气相色谱质谱方法测定这些挥发性有机物特定项目.优化了色谱条件,测定结果线性良好,目标化合物加标回收率、检出限等指标均符合地表水环境质量标准的要求.     

超高压液相色谱/质谱联用法测定地表水中特定污染物

采用超高压液相色谱/质谱联用法测定地表水特定项目中包括微囊藻毒素-LR在内的13种污染物,对测定条件进行优化,使得各目标化合物均能在3min内检测完毕.试验表明,方法在各测定范围内线性良好,相关系数均〉0.99,各目标化合物的方法检出限为0.12μg/L～8.40μg/L,地表水样的加标回收率在62.0% ～104%之间,6次平行测定的RSD〈6%.用该方法测实际水样,阿特拉津和马拉硫磷被检出,质量浓度分别为0.6μg/L和0.7μg/L.     

河南省环境空气质量监测网优化的研究

在全省城市环境空气质量监测网优化并运行六年的基础上 ,采用历史数据计算法对河南省环境空气质量监测网进行了优化。通过优化方法和监测项目的探索 ,确定了省控站数目 ,特别是提出了系统、完整的优化指标 ,优化结果是令人满意的。     

“南京市环境质量监测网络体系的研究与应用”通过专家验收和鉴定

2010年5月15日，南京市科学技术委员会组织中国环境监测总站王瑞斌研究员、江苏省环保厅、上海市环境监测中心、江苏省环境监测中心、南京大学、南京理工大学等单位专家对南京市环境监测环境监测中心站承担的“南京市环境质量监测网络体系的研究与应用”的项目进行了验收与鉴定．市环保局张丹宁局长助理、监科处刘铁处长参加了验收会。该项目在优化南京市环境质量监测点位的基础上，提出了以信息化为统领，以自动化为手段，以质控为保障的南京市环境质量监测网络系统的整体解决方案，     

中国地表水环境质量标准修订研究(续)

中国地表水环境质量标准修订研究（续）夏青（中国环境科学研究院北京１０００２１）中国地表水环境质量标准修订后的基本项目３１项和特定项目４５项的分析方法见表３、表４。表３地表水环境质量标准基本项目分析方法基本项目分析方法检测限ｍｇ／Ｌ方法来源水温温度计法...     

中国地表水环境质量标准修订研究

提出了对ＧＢ３８３８－８８地面水环境质量标准的修订原则和目标。制定了ＧＢ３８３－９８地表水环境质量标准的总体框架。新标准有基本项目３１项,特定项目４５项,对４２面有机化学物质指标３项防止富养化指标和２项常规污染控制指标作了较详细地论述,对项目的分析方法亦作了增订和补充。     

SPME-GC同时测定地表水环境质量标准特定项目中硝基苯类和氯苯类化合物

针对地表水特定项目有机物中硝基苯类和氯苯类的测定,采用固相微萃取(SPME)前处理技术,用毛细管色谱柱进行色谱分离,用ECD检测器进行测定。SPME富集效率达118~1352倍,检出限为0.00004~0.05μg/L,方法的线性相关系数为0.9963~0.9999,RSD为2.0%~11.0%,加标回收率为87.0%~108%,所有技术参数均可满足地表水环境质量标准。该方法简单、快捷、无污染且省时省力,具有较好的推广性。     

辽河流域水环境监测网络优化技术研究

以辽河流域2009—2011年监测数据为基础,针对北方季节性河流,在制定了水环境监测网络优化原则的前提下,分别运用最优分割法、变异系数与水质类别相结合方法、连续3年未检出判断法进行了辽河流域水环境质量监测断面、监测频次和监测项目的优化。结果表明,辽河流域优化后的监测断面为18个,比优化前减少8个。在监测频次上,干旱少雨的月份中,1、5、10月应保持每个月2次的监测频次,2—4月、11—12月每月监测1次;湿润多雨的6—9月只监测1~2次即可,全年监测频次分布更合理。监测项目分为必测项目和选测项目,必测项目为12~20项,选测项目为3~11项。     

岷县地震灾害对当地水环境质量的影响分析

为了解地震对地表水环境质量的影响,文章以2013年7月甘肃省定西市岷县、漳县交界6.6级地震为背景,选取岷县受灾最严重的梅川镇和中寨镇,对所在主要河流洮河断面和集中饮用水取水口中11个常规项目和22个特定项目及生物指标项目进行分析评价,同时考虑地震后消杀物品使用量。经综合分析,岷县6.6级地震,整体上对主要河流洮河水质未造成影响,乡镇集中式饮用水水质也未受到影响,从水环境生物毒性分析结果来看,水质安全。     

黄河水质例行监测项目优化的设想

通过近８年对黄河兰州段水质例行监测结果统计分析,提出优化筛选监测项目和新增监测项目的建议,优化筛选监测项目,将会使今后的例行监测工作更加有的放矢,收到更好的经济效益,环境效益和社会效益。     

Occurrence of naproxen,ibuprofen, and diclofenac residues in wastewater and river water of KwaZulu-Natal Province in South Africa

The present paper reports a detailed study that is based on the monitoring of naproxen, ibuprofen, and diclofenac in Mbokodweni River and wastewater treatment plants (WWTPs) located around the city of Durban in KwaZulu-Natal Province of South Africa. Target compounds were extracted from water samples using a multi-template molecularly imprinted solid-phase extraction prior to separation and quantification on a high-performance liquid chromatography equipped with photo diode array detector. The analytical method yielded the detection limits of 0.15, 1.00, and 0.63 μg/L for naproxen, ibuprofen, and diclofenac, respectively. Solid-phase extraction method was evaluated for its performance using deionized water samples that were spiked with 5 and 50 μg/L of target compounds. Recoveries were greater than 80% for all target compounds with RSD values in the range of 4.1 to 10%. Target compounds were detected in most wastewater and river water samples with ibuprofen being the most frequently detected pharmaceutical. Maximum concentrations detected in river water for naproxen, ibuprofen, and diclofenac were 6.84, 19.2, and 9.69 μg/L, respectively. The concentrations of target compounds found in effluent and river water samples compared well with some studies. The analytical method employed in this work is fast, selective, sensitive, and affordable; therefore, it can be used routinely to evaluate the occurrence of acidic pharmaceuticals in South African water resources.     

直接进样-热脱附-GC-MS快速测定大气细颗粒物中有机示踪物

建立了直接进样-热脱附-GC-MS快速测定细颗粒物中甾烷类和藿烷类有机示踪物的方法。经实验条件优化,13种目标化合物的线性回归方程的相关系数均在0.990以上,空白加标回收率为81.4%~102.3%,实际样品加标回收率为79.1%~112.9%,相对标准偏差小于13.2%。当采样体积为24 m~3时,各目标化合物的检出限为0.008~0.084 ng/m~3,方法灵敏度高。利用该方法测定了北京城区采暖季和非采暖季PM2.5实际样品,结果表明:各目标物均有检出,且采暖季的甾烷类和藿烷类化合物的总量均明显高于非采暖季。该方法无需复杂的前处理和有机溶剂,操作简便快捷,在颗粒物中非极性化合物的快速检测方面具有很大的应用价值。     

Occurrence of orthophosphate monoesters in lake sediments: significance of myo- and scyllo-inositol hexakisphosphate

Orthophosphate monoesters often constitute a significant fraction of total phosphorus in lake sediments. The knowledge on the specific composition and recalcitrance of these compounds is however limited. The main aim was therefore to identify and quantify specific orthophosphate monoesters in sediment from 15 Danish lakes by solution (31)P NMR spectroscopy. The four most quantitatively important orthophosphate monoesters were myo-inositol hexakisphosphate (myo-IP(6)), scyllo-inositol hexakisphosphate (scyllo-IP(6)) α-glycerophosphate (α-GP) and β-glycerophosphate (β-GP). The compounds were identified in 9, 4, 8 and in all 15 lakes, respectively. In total these four components made up 46-100% of the orthophosphate monoester pool. The glycerophosphates (GPs) are most likely degradation products of phospholipids, created as an artifact by the alkaline extraction procedure used for (31)P NMR spectroscopy, while the inositol hexakisphosphates (IPs) are naturally occurring compounds. There was a significant positive correlation between myo-IP(6) and total aluminium in the sediment and a negative correlation between myo-IP(6) and lake water pH, suggesting that myo-IP(6) is stabilized in the sediment by adsorption at slightly acidic or neutral conditions. In three lakes, the depth distribution of the orthophosphate monoesters was investigated. The content of scyllo-IP(6) and myo-IP(6) was constant with sediment depth in two of the lakes while the content of myo-IP(6) decreased with depth in one of the lakes. In all cases the IPs seem to be preserved with sediment depth to a higher extent than the orthophosphate diesters and especially the GPs suggesting that IPs can be a sink for phosphorus in the lake ecosystem or at least delay P-recycling for years.     

气相色谱-串联质谱法测定水中痕量有机磷农药和甲萘威

采用二氯甲烷萃取水样，气相色谱-串联质谱法同时测定水中有机磷农药和甲萘威。试验表明：方法在20．0μg/L ～1000μg/L范围内，各目标化合物线性良好；方法检出限为0．004μg/L～0．01μg/L；对实际水样进行3个质量浓度水平的加标回收试验，回收率在71．8％～94．5％之间，RSD为3．7％～8．5％，满足水中痕量有机磷农药和甲萘威的测定要求。     

吹扫捕集-气相色谱法同时测定水中的乙醛、丙烯醛和甲醛

研究了吹扫捕集-气相色谱法同时测定水中乙醛、丙烯醛和甲醛的方法并优化了实验条件.实验结果表明,该方法操作简便,灵敏高效,目标化合物的检出限分别为0.037、0.012、0.0006mg/L,相对标准偏差在3.9％ ～15.8％之间,实际水样的加标回收率在73.0％ ～118％之间,能很好满足《地表水环境质量标准》中相关项目的要求.     

基于磁性分离测定水样中的吲哚美辛

免疫磁性微球(SMPPA)应用于水样中吲哚美辛的分离富集,并应用高效液相色谱法对吲哚美辛进行测定。在优化的淋洗和洗脱条件下,70%甲醇和10%甲醇分别作为洗脱液和淋洗液,其回收率能达到90%。选择了湖水、河水、自来水、污水厂进口水以及医院排水为真实样品进行测定,其中湖水、河水、自来水3种真实水样中未能检测出吲哚美辛,污水厂进口水以及医院排水中吲哚美辛的含量分别为0.762、35.4 ng/m L。对这5种水进行加标回收吲哚美辛,加标回收率为92.7%~113%,RSD为1.09%~7.73%。该方法具有简便、快速、特异性等特点,能有效地分离富集水样中的目标物,对其他目标物具有广泛的实际应用价值。     

热解吸/GC/MS联用测定石化工业区大气环境中挥发性有机物

采用二次热解吸／气相色谱／质谱联用测定石化工业区大气环境中挥发性有机物，质谱检测器同时进行全扫描和选择离子扫描，全扫描定性，选择离子扫描和内标法定量。方法线性良好，50种目标化合物的检出限为0.14ng-2.45ng，在3个浓度水平的加标回收试验中，1，1-二氯乙烯和二氯甲烷回收率较低，氯仿和苯低浓度回收率较差，其余46种目标化合物的回收率为83.4％-116％，RSD为0.5％-8.9％。     

Solid-phase extraction followed by liquid chromatography-time-of-flight-mass spectrometry to evaluate pharmaceuticals in effluents. A pilot monitoring study

The present work provides a multi-residue analytical method for determining a selection of 20 pharmaceuticals from diverse therapeutical classes in hospital effluent wastewater. The method is based on the simultaneous extraction of the target compounds by solid phase extraction (SPE), followed by liquid chromatography-time-of-flight-mass spectrometry (LC-TOF-MS) analysis. Using TOF-MS, accurate mass measurements within 2 ppm error were obtained for most of the pharmaceuticals studied. Empirical formula information can be obtained by this method, allowing the unequivocal identification of the target compounds in the samples. Validation studies showed that LC-TOF-MS analysis is a valuable new tool for identification and quantification of pharmaceuticals in wastewater. Recoveries, using Oasis HLB cartridges at pH 7, were higher than 75% for all pharmaceuticals, except for ranitidine, 4-methylaminoantipyrine (4-MAA), cefotaxime and omeprazole, which needed specific pH conditions for their extraction. Linearity of response over two orders of magnitude was demonstrated (r > 0.99). Matrix effects resulting in suppression of the response were observed. For most of the compounds ion suppression was less than 39%, except for metronidazole, carbamazepine 10,11-epoxide, naproxen and erythromycin, where the signal suppression was 42%, 59%, 46% and 95%, respectively. A simple and effective approach to minimize or avoid matrix interferences was the 1 : 4 dilution of the SPE extracts. Method detection limits (MDLs) and quantification limits (MQLs) ranged between 4-115 ng l(-1) and 14-384 ng l(-1), respectively. The precision of the method, calculated as relative standard deviation (RSD), ranged from 1.1-19.8% and 1.7-21.7% for intra- and inter-day, respectively. The developed analytical method was applied to the analysis of hospital effluent wastewater during a survey study. 18 of the 20 pharmaceuticals studied were detected at concentration levels of microg l(-1), reaching in some cases concentrations over 100 microg l(-1), and in the case of the analgesic and antipyretic dipyrone metabolite, higher than 1000 microg l(-1).     

海水石油类分析的影响因素

石油类是衡量海水水质的重要指标,海洋石油的首要污染源是原油泄漏,因此海水石油类的具体成分与原油成分基本一致,主要为弱极性的烷烃、环烷烃和芳香烃。在3种国标分析方法中,紫外分光光度法的应用最为广泛。采用该法分析时,建议统一选择HJ油标准作为标准溶液,透光率90%的正己烷作为萃取剂,标准曲线斜率在斜率控制图内的上下辅助限之内;萃取过程中调节水样p H值2,人工萃取时间120 s,萃取后不能立即分析时,在5℃冰箱内保存不超过2周。     

Solid-phase microextraction coupled to gas chromatography-mass spectrometry for the study of soil adsorption coefficients of organophosphorus pesticides

A solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method for the simultaneous determination of the organophosphorus pesticides (OPPs), phorate, diazinon, methyl-parathion, fenitrothion, malathion, fenthion, ethyl-parathion and methidathion, has been developed to study their soil/water distribution. The method was used in conjunction with a conventional 'batch equilibrium method' to assess the soil adsorption coefficients (Koc) of the target compounds in different soil samples with known organic carbon content. Contrary to traditional techniques, the present method is fast, solvent-free and highly sensitive, thus permitting the assessment of the Koc values of the target compounds even at low soil concentration levels, close to those encountered in real field contamination, where the Freudlich adsorption isotherms can be considered to be linear. The estimated Koc values were found to be in good agreement with those reported in the literature.