A comparative study on the contents of vitamins in the natural and the cultured prawn

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重油凝胶色谱制备样品中痕量镍的分析研究

研究表明微波密闭消解法对重油凝肢色谱制各样品的前处理，不造成易挥发有机金属化合物的损失，对样品无污染。采用消解前定容，配合石墨炉二次进样富集样品，可以测定样品中低至10^—9级的镍。方法应用于镍在渣油中随相对分子质量分布分析中，标准样品对照数据吻合好，相对标准偏差(RSD，n＝11)为8％。     

N1923-DA201大孔吸附树脂反相分配色层分离、偶氮胂Ⅲ比色测定矿石中钍

用N1923-二甲苯作固定相,AD201大孔聚二乙烯苯吸附树脂作裁体,研究了钍在硫酸介质中的反相分配色层分离条件。拟定了矿石中微量钍的测定方法。     

Determination of nitrophenols,diaminotoluenes, and chloroaromatics in ammunition wastewater

Methods for the determination of three compound classes, i. e. diaminotoluenes, nitrophenols, and chloroaromatics in groundwater of a former ammunition plant are reported. Diaminotoluenes were extracted by discontinuous liquid/liquid-, nitrophenols by continuous liquid/liquid-extraction using dichloromethane, and chloroaromatics by solid-phase extraction. These compound classes may be analyzed by gas chromatography (GC) or gas chromatography coupled to mass spectrometry (GC/MS) without derivatization or after derivatization with N-methyl-bis(trifluoroacetamide) (MBTFA) or heptafluorobutyric anhydride (HFBA) in the case of diaminotoluenes and HFBA or acetic anhydride in the case of nitrophenols. An atomic emission detector (AED) coupled to a gas chromatograph may be employed for the analysis of chloroaromatics. High selectivity can be achieved using the characteristic wavelengths of chlorine. A variety of these compounds were identified and quantified in a groundwater sample from the former ammunition plant Elsnig (Saxony, Germany). Concentrations were in the lower ppb range. Thus, dichlorobenzenes which may have been used as substituents at the end of World War II could be identified in groundwater samples at this site.     

Trace analysis of quaternary aminoalcohols as degradation products from softeners in wastewater

The sensitive and selective determination of polyalcohols without chromophores or fluorophores in the lower ppb-level is still an analytical task of high interest, especially in the field of environmental investigations. This paper describes a cation-exchange HPLC procedure for the separation and fluorescence detection of two quaternary ammonium compounds with polyalcoholic groups (degradation products of fabric softener) after derivatization with 9-fluorenylmethyl chloroformate (FMOC). Detailed experiments were carried out to determine optimum reaction conditions (pH, reaction time, temperature), linear range, detection limits, and kinetics of the reaction. The HPLC separation on a cation-exchange column includes a gradient program which provides complete separation from neutral compounds also reacting with FMOC and its hydrolysis products formed during the reaction in alkaline medium. High specificity for both investigated ammonium compounds with detection limits in the range of 1 ppb could be achieved.     

Characterization of industrial wastewaters using gel-permeation chromatography with multicomponent detection

The gel-permeation chromatography system with multicomponent detection of organic carbon, organic nitrogen, organic halogen, and UV/vis absorption measurement is shown to be a useful tool for characterization of industrial wastewaters and wastewater treatment processes. The proposed system was used to investigate biologically treated wastewater from chemical industry, whereby one branch stream was identified to be the main source of persistent halogenated organics. Various treatment processes of pulp mill wastewater were also evaluated revealing that precipitation with aluminium is very effective for the removal of the high molecular fraction whereas the biological treatment is generally less selective. In the biological treatment of tannery wastewaters, it has been shown that the aerobic treatment, in contrast to anaerobic step, causes evident alterations of the composition of the polar DOC fraction. The nitrogen containing compounds are also better decomposed in the aerobic step compared to the anaerobic one.     

用离子色谱法测定金矿区水样中常规无机离子

利用DX－120离子色谱仪进行阴阳离子的精密度和准确度测定，100mg/L时相对标准偏差范围为1．00％－3．80％，回收经95．83％－105．00％；5mg／L时相对标准偏差范围为1．18％－4．57％，回收率92．40％－103．20％，完全达到实际要求。用该离子色谱仪测定甘肃阳山金矿山水样中常规无机离子，数据表明该区域水质较好，所测离子浓度都未超过饮用水标准。     

Zur Bildung von Artefakten und deren Vermeidung bei der Bestimmung leichtflüchtiger Halogenkohlenwasserstoffe in Wasser mittels Headspace-Gaschromatographie unter den Bedingungen der DIN 38407 Teil 5 (DEV-F5). Teil II: Überhöhte Trihalogenmethanbefunde in gechlortem Schwimmbeckenwasser

Formation of Artefacts and its Suppression during the Determination of Volatile Halogenated Hydrocarbons in Water by Means of Headspace Gas Chromatography under the Standard Conditions of DIN 38407-F5. Part II: Increased Trihalomethane Formation in Chlorinated Swimming-pool Water A comparison of two analytical standard procedures for the determination of trihalomethanes (THM) in water (headspace gas chromatography and pentane extraction/gas chromatography) yielded strongly differing results. Under the conditions recommended by the German Standard Method DIN 38407-F5 (60…80°C for at least 60 min) degradation of thermo-labile chlorination products occurs resulting in elevated THM concentrations. The reactions involved are partly pH-dependant, and these can be suppressed by sample acidification. The degradation of trihalogen acetic acids, however, can only be influenced by minimizing the equilibration time and temperature. Other intermediate chlorination products (haloacetonitriles) are also degraded to THM after preceding hydrolysis to the corresponding carboxylic acids. Comparative results obtained with a purge and trap method at ambient temperature, i.e. without thermal stress during the enrichtment step, are lower than with static headspace GC but still high in comparison to the pentane extraction method. Presumably volatile THM-precursors are also trapped and subsequently decomposed upon thermal desorption from the trap. As the static headspace GC is the most rational method of LHKW determination available, the recommended experimental sample handling conditions should be modified in a way that deterioration reactions are reduced as far as possible.     

Gas Chromatography for Determination of Pesticides in Aquatic Systems — Analytical Basis Gaschromatographie zur Bestimmung von Pestiziden in aquatischen Systemen — Analytische Grundlagen

High resolution gas chromatography (HRGC) with ECD, NFID and MSD is a very efficient determination method for pesticides in water. Because of their relatively low concentrations in aquatic systems enrichment and preconcentration procedures are essential. Some examples for pesticide determination by GC methods are given. Potentials and limitations of HRGC for pesticide analysis are also discussed. An extensive pesticide analysis in water has to include different methods like HRGC, HPLC and GC/MS.     

华北平原冬麦田土壤CH4的吸收特征研究

利用静态箱/气相色谱(GC)法,对华北平原冬小麦拔节-成熟期间麦田土壤CH₄气体通量进行了测定,得出华北平原典型冬麦田土壤是大气CH₄的弱吸收汇。试验期间土壤CH₄通量存在明显的季节变化和日变化,麦田拔节-成熟期间土壤CH₄通量日平均值为-18.3μg·m^-2·h^-1,波动范围为-4.3-24.4μg·m^-2·h^-1;在土壤CH₄通量的日变化中,观测到麦田土壤在午间和夜间都有一个吸收峰,峰值出现的时间因生育期不同而有所不同。试验期间CH₄通量日平均值与土壤温度关系不明显,而与土壤水分呈负相关(α=0.01);日变化中土壤CH₄通量与地表温度的相关性较差,而与5cm地温相关密切。麦田拔节-成熟期间土壤CH₄通量日平均值随NH4+-N施用量的增加呈递减规律,农田秸秆还田后不利于土壤对CH₄的吸收。