Identification of organic residues in tertiary effluents by GC/EI-MS,GC/CI-MS and GC/TSQ-MS

A method was developed for the analysis of non-volatile dissolved organic residues in tertiary treated wastewater effluents. This method involved concentration of samples by rotary evaporation, propylation using propanol/formic acid/acetyl chloride, and separation, detection and quantitation by capillary GC/EI and CI-MS and GC/TSQ-MS analysis. Ethylenediamine tetraacetic acid (EDTA) was the most prominent compound found in both granular activated carbon (GAC) and chlorinated GAC effluents (110 and 140 μg/L, respectively). Other compounds identified included nitrilotriacetic acid (NTA), carboxyalkylphenoxy ethoxy carboxylates, poly(propoxy), poly(ethoxy) or poly(ethoxy)(propoxy) compounds, small aliphatic dicarboxylic acids and aldehydes, all at lg/L levels. Approximately 80% of all chromatographically separated compounds were positively or tentatively identified. The identified compounds are estimated to account for approximately 10% of the dissolved organic carbon. Received: 8 August 1994/Revised: 14 February 1995/Accepted: 16 February 1995 Correspondence to: W.-H. Ding     

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。     

Identification of Dinocap in water using GC/IR and GC/MS

The determination of Dinocap, one of the most often used acaricides and contact fungicides, is complicated by the fact that it consists of several isomeric alkyldinitro-phenyl-crotonates. In a first step, GC/IR and GC/MS has been used to separate the mixture, to determine the chromatographic behaviour and to fully characterize the six different isomeric compounds. The structures of additional impurities in the commerical preparation were shown to be the correlating phenols. An extraction/preconcentration method has been devised based on Carbopack B, yielding recoveries between 75 and 98%. A qualified estimation of the total Dinocap content of drinking water can be made by this approach for concentrations well below the limits set by the European drinking water regulations. The development of a complete analytical procedure based on these results appears to be feasible.Dedicated to Professor Dr. Dr. h.c. mult J. F. K. Huber on the occasion of his 70th birthday     

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％。     

GC/IMS and GC/MS analysis of pre-concentrated medical and biological samples

Ion mobility spectrometry (IMS) is a well-known analytical method for the detection of CWAs and explosives since many years. Coupling IMS to GC pre-separation, new application fields in medicine and biology could be opened, dealing with complex and humid mixtures. However, identification of unknowns in such a complex sample is challenging and can only be achieved by parallel GC/MS analysis, thus obtaining a proposal for the responsible compound for validation via reference substances by GC/IMS again. The available adsorption tools for such accompanying GC/MS analysis have their particular drawbacks (e.g. problematic quantification for SPME, high sample volumes for adsorption tubes). Therefore miniaturised adsorption needles (NeedleTrap) were applied to both GC/IMS and GC/MS for validation of their reproducibility. It could be demonstrated that the needles can even be used for appropriate quantification when the adsorbent and the sample volume are adapted properly to the concentration range, the compounds of interest and humidity of the sample. The method is very flexible with regard to the concentration range by variation of the sample volume (e.g. 20 mL for ppt_V, 10 mL for lower ppb_V or 1 mL for ppm_V) and with regard to the compounds of interest by application of common adsorption materials optimised for the relevant substance group. Such materials are available commercially in a broad variability. Therefore, the miniaturised adsorption needles are a helpful complementary sampling method for any GC/MS or GC/IMS investigations.     

气相色谱和气相色谱/质谱法分析高级脂肪伯醇混合物的化学组分

多廿醇是从制糖滤泥中分离得到的一种高级脂肪伯醇天然混合物,其化学组成分析未见报道。本文采用气相色谱法（GC）和气相色谱／质谱法（GC／MS）,对其组分和结构进行了分析和鉴定。     

Archaeological wood characterisation by PY/GC/MS, GC/MS, NMR and GPC techniques

The chemical characterisation of waterlogged archaeological wood is of paramount importance in terms of understanding not only the degradation processes of wood in artistic and archaeological objects but also the development of consolidation and conservation procedures. The two different types of archaeological waterlogged wood were characterized using several analytical techniques. The analytical protocol consists in using PY/GC/MS with in situ derivatisation with hexamethyldisilazane, GC/MS of the extractives, ¹H, ¹³C and ³¹P NMR analysis, and GPC. The main results showed that one of the ancient samples was a gymnosperm wood from the Pinaceae family, whereas the other type of wood was an angiosperm. Lignin from the angiosperm was oxidised in a benzylic position of β-O-4 to give oxo functional groups, in primary alcohol moiety to give carboxylic groups. In addition, the formation of a new intermonomeric bond 5-O-4 was observed.     

红景天挥发油的GC／MS／DS和GC／IR／DS研究

红景天挥发油的ＧＣ／ＭＳ／ＤＳ和ＧＣ／ＩＲ／ＤＳ研究阎吉昌，张宏徐少敏卫永弟，阎雪（东北师范大学测试中心，长春，１３００２４）（吉林省石油化工研究院，白求恩医科大学）关键词红景天，色谱／质谱，色谱／红外，复杂有机混合物应用色谱／质谱／计算机（ＧＣ／Ｍ...     

Field-portable, high-speed GC/TOFMS

This work is focused on developing a fast gas chromatograph, time-of-flight mass spectrometer (GC/TOFMS) for man-portable field use. The goal is to achieve a total system solution for meeting performance, size, weight, power, cost, and ruggedness requirements for a laboratory in the field. The core technology will also be adaptable to specific applications including real-time point detection for hazardous chemical releases (e.g., chemical weapons), for biological agent signature identification, and for mobile monitoring platforms (e.g., air, ship, truck). Previously we presented results of a feasibility demonstration for a 30-lb field-portable TOFMS system. In this work we present recent progress in integrating a low-power, high-speed GC and show the capability for accurately recording fast GC transients for targeted compound detection using a quadrupole ion trap, time-of-flight instrument (QitTof).     

Polycyclic aromatic hydrocarbons in C8 isomer aromatic feed: analysis by GC, GC/MS, and GC/FTIR techniques

Polycyclic aromatic hydrocarbons (PAHs), apart from their carcinogenic and mutagenic nature, create many problems in the petrochemical industry due to their tendency toward carbonization. Compounds in C8 aromatic isomer feed are analyzed by means of sample concentration, followed by separation of individual compounds by gas chromatography on a stainless steel OV-101 phase capillary column and identification by gas chromatography/mass spectrometry and gas chromatography/Fourier transform infrared spectroscopy. Various compounds belonging to different classes (mainly monocyclic, dicyclic, and tricyclic aromatics), oxygenated aromatics, and aliphatic saturates are quantified in the concentrated hydrocarbon residue of C8 isomer feed. Both unsubstituted and alkyl substituted ring type compounds are present. Concentrations obtained for PAH compounds in the C8 isomer feed range from 0.2 to 0.42 micrograms/mL.     

GC和GC／MS分析脱硫细菌代谢二苯并噻吩的产物

从茂名炼油厂周围土壤中分离得到一株可脱除二苯并噻吩（DBT）的细菌YC－LI－1用GC／MS方法定性鉴定了该细菌脱除DBT的代谢的有机产物为2－羟基联苯（1－OHBP）,此外试验还证明了DBT中的硫原子代谢为水溶性的硫酸盐,用GC方法测定了该菌种将DBT代谢为2－羟基联苯的转化率,分析结果表明该菌种可有效代谢DBT,转化率达90％以上。     

Adsorption of Oil Substances by Carbon Monolith and Their Subsequent Determination by GC/GC/MS

Moscow University Chemistry Bulletin - A monolith based on foamed graphite is used for the sorption of hydrocarbons (alkanes, cycloalkanes, arenes) as markers of oil pollution. This material is...     

固相微萃取/气相色谱/质谱联用技术在农药残留物分析中的应用

综述了固相微萃取／气相色谱／质谱（SPME／GC／MS）在各种环境水、土壤等样品中农药残留分析中的应用和发展。SPME／GC／MS联用技术具有快速、简便、准确等优点。     

Ru-P/MWCNTs-DHP/GC电极的电化学特性

应用循环伏安法、微分脉冲伏安法、紫外-可见和荧光光谱研究了一种新型钌化卟啉[Ru(phen)2(MPyTMPP)Cl]+(phen=1,10-邻菲咯啉,MPyTMPP=5-(3-吡啶)-10,15,20-三-(4-甲苯基)-卟啉)在多壁碳纳米管(MWCNTs)修饰的玻碳(GC)电极表面的电化学特性及其与电极上和溶液中双十六烷基磷酸盐(DHP)的作用.结果表明:[Ru(phen)2(MPyTMPP)Cl]+能强吸附在MWCNTs-DHP/GC电极表面,并呈现一对由表面过程控制的氧化还原峰;适量DHP有利于该配合物的吸附固定;[Ru(phen)2(MPyTMPP)Cl]+能与溶液中的DHP形成结合体,导致配合物中心离子反应电位负移.