冷阱温度和激活电压对气相色谱分析痕量磷化氢的影响

磷化氢是一种有芥子气味的无色剧毒气体,磷化氢浓度在1．0～10μ/L内可使人眩晕、头疼、恶心、呕吐,当其浓度进一步增加时会导致肺水肿甚至昏迷死亡。常用的磷化氢分析方法主要有铝蓝比色法和气相色谱法,本实验室牛晓君等采用柱前两次低温冷阱富集和气相色谱／氮磷检测器联用技术（GC-NPD）分析了痕量磷化氢,在这一方法中,冷阱温度是影响磷化氢富集率的重要因素,检测器激活电压则是影响磷化氢响应值的重要因素。本文分别考察了这两个因素对磷化氢定量的影响。     

甲醇在Pt-Sn/GC上的电催化氧化

直接甲醇燃料电池（DMFC）以环境友好的甲醇为燃料,具有广泛的应用前景。目前使用的阳极催化剂主要是铂族贵金属,成本高,寿命和活性较差,因此,研究出高活性催化剂仍是目前的热点。通常方法是向Pt中添加一种或多种亲氧金属如Ru或Sn等,制成二元或多元铂合金。本文采用循环伏安法在玻碳电极上修饰铂锡合金,金属用量少,操作方便,相比Pt／GC,对甲醇的氧化呈现了较高的催化活性。     

水中挥发性有机有害物质分析的痕量富集研究──疏水富集效果的评价

用通过容量（ＱＢ）作为疏水富集效果的评价指标，ＱＢ可根据反相液相色谱的保留体积或容量因子来求得。本文列出了若干水中典型有机有害物质在反相色谱填料上的通过容量，并与从前沿色谱得到的数据进行了比较和讨论。     

浙产山鸡椒挥发油成分的GC/MS分析

山鸡椒Litsea cubeba系樟科木姜子属植物,民间亦名山苍子、木姜子等,广布于我国南部省区,具有温中散寒、行气止痛等功效[1].     

水中超痕量汞的富集与测定

利用合成的巯基含量为2.2～2.5%的高巯基粉状巯基棉,对水中超痕量汞进行富集测定。流速可达100mL·min~(-1),检出限为0.5×10~(-12),加标回收率为90～104%。     

食品中痕量稀土元素微型高效富集器离子交换预富集-ICP-AES-联用分析方法的研究

本文研究了食品中痕量稀土元素的离子交换预富集-ICP-AES在线分析方法；筛选出4种对各稀土元素具有较好富集性能，并适于微型富集器使用的高效树脂（包括离子交换树脂、鳌合树脂和螯合纤维树脂），该分析系统可用于矿泉水、贻贝、牡蛎、茶叶等食品标样中ng／ml及μg／g级痕量稀土元素测定。所得结果与推荐值相吻合。该分析系统测定精密度符合痕量分析要求，富集倍数可达17—30倍，检出限为0．08—5．5ng／ml     

Pt-Ru/GC电极对甲醇电催化氧化的研究

利用循环伏安法制备了Pt-Ru/GC电极并用于对甲醇的电催化氧化研究,考察了Pt、Ru原子比、沉积电位下限和沉积量对电极催化性能的影响,研究了电极催化性能的稳定性。结果表明Ru的加入对电极催化性能具有明显的改善作用,对甲醇的氧化电位范围明显变宽,氧化电流明显增大,电极的稳定性明显高于Pt/GC电极。在Pt、Ru原子比为1:1、沉积电位下限为-0.2V、沉积量为40r的条件下,Pt-Ru/GC电极对甲醇电催化氧化的性能最好。     

柚皮蒸馏产物的GC/MS分析

用水蒸气蒸馏法对柚皮外果皮进行了挥发性成分提取。用GC/MS分析法进行了分离鉴定,初步分离出50余个峰,鉴定了44种物质,用面积归一法测定其质量分数。在被测物质中,烃类化合物有13种和含氧有机化合物有31种,主要物质为柠檬烯(75.09%),α 蒎烯(0.84%),β 月桂烯(6.71%),芳樟醇(1 08%),芳樟酯(1.43%),萘酮(4.89%)。     

W/O型微乳状液迁移和富集痕量金属离子Cd2+、Cr3+的研究

利用各种分离技术分离和富集金属离子,无论是在环境保护还是在湿法冶金方面都具有重要的意义.油包水型微乳状液因具有独特的物理化学性质,已越来越广泛地应用于金属离子的萃取分离上.     

我国环境中有机污染物分析方法及痕量富集技术的进展

对有机污染物分析在近年进展作了评述。其主要内容涉及试样的预处理技术（如顶空法,吹扫-捕集法,固相萃取,半透膜等技术）,各化合物的适用及有效的分析方法或仪器（如GC,HPLC及GC／MS等）以及各种技术及方法的联用技术等（引述文献37篇）。     

气相色谱/氢火焰检测器快速检测海洛因毒品及其来源推测

建立一种海洛因样本的快速检测和来源推测的方法。采用气相色谱/氢火焰检测器(GC/FID)和主成分分析(PCA)的方法对675份云南、新疆两地海洛因样本进行了检测,实现了云南、新疆两地缴获海洛因毒品的特征性划分,阳性率达到83.5%以上。采用GC/FID技术和主成分分析的方法可以实现海洛因样本地理来源区分。     

Simplification of determination method for standard materials using post-column reaction GC/FID

For the simple and fast preparation of highly reliable standard materials, a post-column reaction GC/FID system was developed and evaluated on the mixture of oxygen-containing organic compounds. The oxygen-containing organic compounds mixing solution were determined with the post-column reaction GC/FID system using n-dodecane as an internal calibration standard. Required value of relative expanded uncertainty as an original source of SI-traceable standard materials was within 1% and it aimed at this value as accuracy of the quantitative analysis. The results showed good agreement between the prepared concentrations and analytical values using post-column reaction GC/FID system. These results indicated that the post-column reaction GC/FID system would be used for getting SI-traceable values.     

Metrological effectiveness of an analytical method for volatile organic compounds standard materials using post-column reaction GC/FID system

The metrological effectiveness of an analytical method using the post-column reaction GC/FID system was evaluated. The SI-traceable certified reference material (CRM), the eight ester phthalates mixture standard solution, was used as a sample. We assigned specific value to n-eicosane and it was used as an internal standard. A known quantity of n-eicosane was added to the CRM, and the mixture was measured with the post-column reaction GC/FID system. Six phthalate esters were chromatographically separated and determined. The assigned values by our system are in good agreement with the certified values of the CRM, and the combined uncertainties of the measurements by the present system were better than those of the CRM. Our method is classified as a primary ratio method and the specific values of many organic compounds can be assigned very precisely by using a small number of reference materials. Also, the method can make it possible to avoid the purity determination of raw materials and directly to assign their specific values after the preparation of the standard mixture. Conclusively, this post-column reaction GC/FID system is very effective for the chemical metrology.     

棒状薄层色谱/氢火焰检测法在石油重质油烃组成分析上的应用

在石油重质油的烃组成分析中,液固色谱,质谱和高效液相色谱等已被广泛采用。但是,这些方法均存在着一些缺点,如分析时间长、定量困难等。棒状薄层色谱/氢火焰检测(TLC/FID)法则较好地克服了上述缺点。本文扼要叙述了TLC/FID法的分析原理、试验技术和在石油重质油烃组成分析中的应用实例,并对该技术的发展前景提出了看法。     

Identification and Linkage of Tarballs from the Coasts of Vancouver Island and Northern California Using GC/MS and Isotopic Techniques

During January and February 1996, a significant number of tarball/patty incidents occurred along the coasts of Vancouver Island, Washington, Oregon, and California. Samples of the tarballs were collected from the affected beaches and analyzed by gas chromatography/mass spectrometry (GC/MS) and gas chromatography/flame ionization detector (GC/FID) using a tiered analytical approach developed for determining the origin of oils. Selected samples were further analyzed using a carbon isotopic technique. Also, the relative abundances of a large number of “source-specific marker” compounds, in particular alkylated series of polycyclic aromatic hydrocarbons within the same alkylation isomeric groups, were compared. Results of the analysis revealed that (1) California/Oregon samples were chemically similar and consistent with the same source. They were identified to be bunker type fuel; (2) The tarball samples collected from British Columbia and Ocean Shores, Washington were chemically similar and consistent with the same source (also bunker type fuel). They were found to be similar to but may have a source different than the California/Oregon samples; (3) The source of the tarball/patty samples was neither Alaska North Slope oil nor California Monterrey Miocene oil; (4) The spilled oil samples have been highly weathered since release, and the California samples were more heavily weathered than the British Columbia samples.     

乙酰乙酸乙酯烯醇式与酮式GC/MS和GC/IR分析

采用ＧＣ／ＭＳ对乙酸乙酯烯醇式在不同离子源温度,接口温度,进样器温度,柱温等条件下的气相色谱行为进行了研究,用重氢交换法和高分辨质谱法对烯醇式和酮式的质谱进行了解析,并通过ＧＣ／ＩＲ研究了烯醇式和酮式的红外光谱。     

甲酯化气相色谱法检测化妆品中防腐剂十一烯酸及其锌盐

采用硫酸催化甲酯化法检测了化妆品中的十一烯酸及其锌盐,并对甲酯化试剂、硫酸浓度、反应体系含水量、甲酯化温度、反应时间等条件进行了优化,发现反应体系的含水量对产率影响较明显。以5%硫酸甲醇溶液为甲酯化试剂,65℃水浴中反应1 h,正己烷为提取溶剂,采用GC/FID色谱法测定,外标法定量。十一烯酸甲酯产率达95%以上,该方法在0.05～1.0 mg范围内线性良好(r>0.999),检出限和定量下限分别为0.001 2%和0.004%。膏霜、乳液、化妆水和洗手液中十一烯酸的平均回收率为93%～104%,相对标准偏差为0.39%～5.1%。     

生物样品中苯丙胺类毒品的小体积液相萃取及GC/MS分析

小体积液相萃取;苯丙胺毒品;唾液;毛发;GC/MS     

吹洗和捕集色/质联机法定量分析水中挥发性有机物

本文详细地介绍了利用吹洗和捕集色/质联机法定量分析水中挥发性有机物的原理、过程和实验中应注意的问题。该方法在严格的质量保证和质量控制(QA/QC)下,定量分析水中挥发性有机物,得到了满意的结果。     

调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用

报道了调味品中氯丙醇的衍生化气相色谱(GC／ECD)和衍生化气相色谱双串联质谱法(GC／MS／MS)测定。GC／ECD测定酱油中3—氯—1，2—丙二醇(3—MCPD)的检出限达到0．01mg／kg，回收率为91％～104％，变异系数为2．27％～7．96％；GC／MS／MS同时测定酱油中1，3—二氯—2—丙醇、2，3—二氯—1—丙醇和3—氯—1，2—丙二醇，1，3—二氯—2—丙醇、2，3—二氯—1—丙醇的检出限为0．02mg／kg，3—氯—1，2—丙二醇的检出限为0．01mg／kg，回收率在92％～106％，变异系数为3．51％～13．33％。