气提法富集气相色谱／质谱法测定水中痕量挥发有机物

作者改进了气提法富集水中痕量挥发性有机物装置。研究了实验条件对水中痕量有机物富集的影响，并确定了最佳富集条件。以气提法富集气相色谱／质谱法（ＧＣ／ＭＳ）测定了水样中痕量挥发性有机物，取得了满意的结果。     

乳化汽轮机油分离水中的有机物组成分析

通过采用GDX树脂富集，气相色谱／质谱法定性分析，建立了乳化汽轮机油分离水中有机物分析程序．共检测出有机物成分28种，其中5种为汽轮机油的典型添加剂，表明水分对汽轮机油添加剂洗脱作用明显．     

吹扫捕集-气相色谱/质谱法分析汉江有机污染物

采用恒温水浴吹扫捕集-气相色谱/质谱(P&T-GC/MS)法分析汉江水中挥发性有机物,提高了挥发性有机物分析的灵敏度;选用低空白的纯净水,降低了分析的干扰。采用避光的方法以及将水样直接过柱,提高了半挥发性有机物的回收率。用改进了的方法分析汉江水共检出有机物36种。此方法同样适用于其它地表水中有机物的分析。     

大体积固相萃取-气相色谱法测定水中17种氯代有机物

建立水中17种氯代有机物的大体积固相萃取–气相色谱检测方法。样品以3.0 mL/min的流量经大体积样品采样器Cleanert PS固相萃取柱富集,真空抽干后用10.0 mL丙酮洗脱,挥干洗脱液,用1.0 mL正己烷定容,在选定的色谱条件下进行分析。17种氯代有机物的质量浓度在0～100μg/L内与色谱峰面积呈良好的线性关系,相关系数均大于0.999,方法检出限为0.002 5～0.074μg/L。样品加标回收率为81.0%～116.0%,测定结果的相对标准偏差为0.56%～6.80%(n=6)。该方法快速、灵敏、准确,重现性好,具有一定的实用价值,适用于水中17种氯代有机物的同时测定。     

金沙江(渡口市江段)水中挥发性有机污染物分析

本文采用Chromosorb-106大孔树脂吸附,用CS_2洗脱,用玻璃毛细管气相色谱分离,用色谱-质谱-计算机联机定性等方法,对金沙江(渡口市江段)水中痕量挥发性有机污染物进行了分析。共检测出97个有机化合物,并对其中50种化合物取得了181个定量数据,单个化合物的最大浓度为0.4ppb,平均浓度36ppt。经与国内外某些江湖河以及人们迄今所知的有机化合物的毒性比较,该江段水中挥发性有机物污染的程度是较轻的。     

衍生化气相色谱－质谱法测定水中的路易氏剂及砷酸

本文研究了用气相色谱－质谱法测定水中微量路易氏剂及砷。在酸性条件下，路易氏剂及水解产物２，３－二巯基丙醇迅速反应形成挥发性的衍生物，大大提高了测定灵敏度。用选择性离子检测定量，最小检测量为每升水中１μｇ。路易氏剂的加标回收率为９５．６２％～１０５．８８％之间，砷的加标回收率为９６．３５％～１０６．０３％之间。     

固相萃取-气相色谱-高分辨质谱法测定巢湖水中半挥发性有机化合物

描述了巢湖水中半挥发性有机化合物的提取、测定过程和初步结果。湖水中半挥发性有机化合物的提取采用XAD-2和XAD-4混合树脂富集，用气相色谱-高分辨质谱法测定了所萃取的有机化合物，并给出相应的分子式和结构式。春季湖水中检测到14种有机化合物。     

多孔膜萃取/微捕集方法及在线测定水中挥发性有机物

基于多孔膜萃取水中挥发性有机物和微捕集技术,构建了一套水中挥发性有机物(Volatile OrganicCompounds,VOCs)样品前处理装置,可自动、在线、连续完成水中挥发性有机物萃取、富集、热解析,传输给气相色谱分离检测。实验分别对膜萃取材料、萃取温度、萃取时间、吹扫气流速等进行了系统优化,并用于氯仿、1,2-二氯甲烷、四氯化碳、三氯乙烯、甲苯、四氯乙烯、乙苯、氯苯、苯乙烯9种挥发性有机物的检测。研究结果表明,采用膜萃取/微捕集装置,与气相色谱联用,在萃取温度60℃,萃取时间30 min,吹扫气流速8 mL/min条件下,采用氢焰离子化检测器(Flame ionization detector,FID),对氯代烃的检出限达到0.003～0.041μg/L,精确度为2.7%～13.0%,线性相关系数均大于0.9936,适用于在线检测水中挥发性有机物。     

气相色谱-微波等离子体发射光谱研究Ⅱ颍．元素响应值与化合物结构的关系

 ]微波诱导等离子体发射光谱(MIP-AES)是一种气相色谱可进行多元素同时检测的选择性检测器。本文以烷烃、烯烃、芳香烃、多核芳烃、醇等同系物系列，含有饱和烃和不饱和烃（烷烃、烯烃、多核芳烃）的混合物，含氧化合物，各种氯代有机物、溴代有机物等类型的化合物为代表，考察了化合物结构对气相色谱-微波等离子体发射光谱(GC-MIP)的碳、氢、氯、溴等元素响应值的影响以及微波输入功率对元素响应值的影响。     

顶空-气相色谱-质谱法测定水中25种挥发性有机物的含量

采用顶空-气相色谱-质谱法测定水中25种挥发性有机物的含量。水样经80℃、30min静态顶空提取后,在气相色谱分离中用HP-VOC色谱柱为固定相。在质谱分析中采用全扫描和选择离子监测模式。25种挥发性有机物在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限在0.13~2.06μg·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在75.1%~109%之间,测定值的相对标准偏差(n=6)在2.2%~9.8%之间。     

Concentration and determination of trace organic pollutants in water

Organic pollutants in water are isolated on a mini-sampler tube containing a macroporous resin. The sorbed pollutants are next thermally transferred to a second sorption tube and then to an analytical column where they are separated and determined by temperature-programmed gas chromatography. Excellent recoveries were obtained for tests in which model organic compounds of various classes were added to water. The water sample is much smaller than that required with previous analytical methods.     

Contamination by Organochlorine Pesticides in the Estuaries of Southeast China* 06 A

Persistent organic pollutants(POPs) such as organochlorine pesticides are of global concern due to their widespread occurrence and persistence. This paper reports recent research studying the distribution and fate of organochlorine pesticides in the Jiulong River, the Minjiang River and the Pearl River estuaries in Southeast China. Eighteen organochlorine pesticides were extracted from water, pore water and sediment samples, followed by analysis by GC-ECD. The results showed that the contamination levels were similar in these three estuaries.The levels of the total organochlorine pesticides in porewater were significantly higher than those in surface water, due to the high affinity of these hydrophobic compounds for sediment phase. Among the hexachlorocyclohexane (HCH) compounds, β-HCH was found to be the most important isomer. The analysis of 1, 1,1-trichloro-2,2-bis-chlorophenyl-ethane(DDT) and its metabolites showed that 1, 1-dichloro-2[o-chlorophenyl]-2[p-chlorophenyl]-ethylene (DDE) was dominant in the group.Koywords Organochlorine insecticides, DDT, Lindane, Jiulong River Estuary, Minjiang River Estuary, Pearl River Estuary, Water, Sediment     

高效液相色谱法同时分析城市河水中的多种抗生素

结合固相萃取（SPE）与高效液相色谱（HPLC）分析,建立了一种适用于我国城市水环境中多种抗生素的分析方法,同时分析城市水体中3种磺胺类(磺胺嘧啶、磺胺甲唑和磺胺二甲基嘧啶)、3种喹诺酮类(氧氟沙星、诺氟沙星和环丙沙星)、氯霉素以及甲氧苄氨嘧啶等8种抗生素污染物。水样品由稀盐酸调节pH值后经HLB固相萃取小柱萃取,用内标法通过HPLC定量分析上述抗生素污染物。采用Agilent Zorbax Eclipse XRD C18液相色谱柱(150 mm×3.0 mm,3.5 μm),用乙腈-水(含0.1%甲酸)二元流动相进行梯度洗脱,流速为0.25 mL/min,柱温25 ℃。喹诺酮类抗生素使用荧光检测器(FLD)定量,其他抗生素则采用紫外检测器定量。该方法对自来水加标的回收率为80%～120%,对地表水样品加标的回收率为63%～106%,方法的定量检测限为0.030～0.080 μg/L,相对标准偏差小于18%。利用该方法对珠江广州河段的水体进行了分析,检测到磺胺甲唑、氧氟沙星、诺氟沙星及环丙沙星,质量浓度范围为0.197～0.510 μg/L。     

Electron Pyrolysis,a New Method of Organic Microanalysis

Organic compounds incubated with tritiated water of specific activity 5 Ci/ml are specifically fragmented. The β-active fragments can be detected in very small quantities by chromatographic separation. Chemical identification of these fragments provides information about the original compounds, as has been shown by experiments with amino acids, esters, lactones, amides, quinones, terpenes, nitrogen-sulfur heterocycles, and natural products.     

Determination of total inorganic nitrogen by means of the air-gap electrode

A method for determining the total inorganic nitrogen content of aqueous solutions is described. The inorganic nitrogen is reduced by Devarda alloy to ammonia which is thus measured by means of the air-gap electrode. On a sample volume of 100 μl, the assay takes only 5–6 min, the standard deviation being less than 3%. Organic nitrogen-containing compounds do not interfere. The method has been tested on solutions of nitrate and nitrite, with and without organic nitrogen-containing compounds present, and has been applied to samples of river water, untreated waste water and biologically treated waste water.     

Determination of total phosphorus in water by photochemical decomposition with ultraviolet irradiation

A simple and convenient photochemical decomposition method has been developed for the determination of total phosphorus in natural and sewage water. Organic phosphorus compounds and inorganic polyphosphates may be completely converted into orthophosphate in the presence of 0.3M sulphuric acid and 0.12% potassium persulphate with 50 min irradiation. The relative standard deviations found for analysis of natural water (P 35 microg/l.) and sewage (P 2.4 mg/l.) were 5.7% and 1.0% respectively. The method gives results comparable to those obtained by digestion with persulphate.     

SIMULATION MODELLING OF THE IMPACTS OF SEA-LEVEL RISE SINCE THE LATEGLA-CIAL PERIOD ON THE CHANGJIANG(YANGTZE) RIVER, CHINA

Dramatic water stage rise and channel aggradation in the middle and lower reaches of the Changjiang (Yangtze) River have been recognized by previous studies. A further analysis of the data from geological, geomorphological, and paleohydrological surveys suggests that these changes might have resulted from sea-level rise since the Lateglacial period. So a mathematical model has been developed here, which reconstructs the processes of water-stage rise and channel aggradation of the Changjiang River as responses to sea-level rise since 12,100 a B.P.     

浅议基于《有机化合物命名原则2017》的复杂有机化合物

In order to promote and keep pace with the teaching of new nomenclature of organic compounds, some important revisions about teaching organic nomenclature suggested in Nomenclature of Organic Compounds 2017 were summarized. We proposed some concrete suggestions for using the new principles of the Nomenclature of Organic Compounds 2017 to name the complex organic compounds.     

固相萃取液相色谱-质谱/质谱联用测定河水中大环内酯类抗生素

应用固相萃取（SPE）及LC—MS／MS技术，建立了水中痕量大环内酯类抗生素即红霉素、脱水红霉素、罗红霉素的分析方法，优化了固相萃取、液相色谱-质谱／质谱等相关条件。水样经HLB固相萃取柱富集净化，以多反应检测方式（MRM）对待测物进行定性和定量分析。3种抗生素在10-2000ng／L范围内具有良好的线性。其定量下限为5ng／L（S／N〉10）。加标纯水和实际水样的回收率在71％-111％之间，相对标准偏差（RSD）在3．7％-8．6％之间。该方法灵敏度高、选择性好、准确度高，适合实际水样中痕量大环内酯类药物的检测。使用该方法测得珠江广州河段某水样中红霉素、脱水红霉素和罗红霉素质量浓度分别为164、291和134ng／L。