气相色谱表面发射火焰光度检测法测定汽油中的四乙基铅

本文介绍气相色谱表面发射漯焰光度法快速、简便地测定汽油中的四乙基铅，最小检测限为０．３ｎｇ。所得结果与气相色谱－原子吸收联用法基本一致。     

微柱高效液相色谱与火焰光度检测器联用研究

报道了微柱高效液相色谱（micro-column HPLC）与火焰光度检测器（FPD）在线联用系统的研究,目的是发展一种不经复杂前处理步骤即可直接测定有机锡化合物的方法。三丁基锡氯化物（TBT）等经HPLC微柱分离后,通过毛细管连接引入特制的燃烧头,通过火焰光度检测器进行检测,对系统有关参数进行了优化和讨论。所建方法可以直接测定各种水样中的三丁基锡氯化物。     

气相色谱法测定白术及其土壤中二嗪磷残留

本文建立了白术及其土壤中二嗪磷的气相色谱-火焰光度检测(GC-FPD)方法。样品经有机溶剂提取,土壤提取液直接浓缩至干;白术提取液浓缩后过活性炭-助滤剂(Celite545)柱净化,GC-FPD检测。结果表明:二嗪磷在0.01~10 mg/L范围内具有良好的线性关系(R2=0.999),白术及土壤中的最低检测浓度为0.01mg/kg,回收率在80.64%~99.54%之间,相对标准偏差(RSD)为1.25%~4.16%。     

固相微萃取-脉冲火焰光度法测定大气及水中的路易氏剂

建立了固相微萃取（SPME）与气相色谱/脉冲火焰光度检测器（GC／PFPD）联用测定大气和水中路易氏剂及其水解产物的方法。探讨了影响SPME萃取效率的萃取头类型、萃取时间、解吸时间等因素。优化了PFPD的条件参数、衍生化试剂及衍生条件。在优化的条件下，路易氏剂衍生产物的响应值与浓度有良好的线性关系。本方法对水中路易氏剂及其水解产物的检出限为0．1μg/L；气体中路易氏剂的检出限为10ng／m^3；水样的加标回收率为96．7％-102．1％；气体样品的加标回收率为94．9％-103．0％；RSD为2．06％。     

顶空固相微萃取-气相色谱表面发射火焰光度检测法测定底泥中的丁基锡化合物

固相微萃取可用于多种样品基体中挥发、半挥发性有机化合物的测定。将固相微萃取技术应用于底泥样品中丁基锡化合物的富集和萃取,以气相色谱分离结合表面发射火焰光度检测器检测,方法灵敏、快速,一丁、二丁、三丁基锡的检测限可达16.9、1.58和0.17ng/g。     

Comparative Response Characterization of a Universal Acoustic Flame Detector for Chromatography

The relative response towards a wide variety of hydrocarbons was measured simultaneously in both the acoustic flame detector (AFD) and the flame ionization detector (FID). The compounds examined included alkanes, aromatics, unsaturates, aldehydes, ketones, alcohols, carboxylic acids, and a number of hetero-atomic organic analytes. A very close linear correlation was found between AFD and FID response for these analytes with regression providing an r ² coefficient of 0.9103. The observed universal AFD response towards hydrocarbons was attributed to a reduction in flame burning velocity through the capture of key propagating species such as hydrogen radicals. While a few minor exceptions to this correlation were observed, the most notable differences occurred for organometallic compounds, which responded 2–3 orders of magnitude more strongly in the AFD than anticipated by their FID response alone. It was found that the metals present in such analytes are directly responsible for generating the greatly increased AFD response observed, which is attributed to their known radical scavenger properties. Results indicate that overall the AFD provides a uniform response towards most hydrocarbons that is qualitatively very similar to that of an FID. For those analytes containing metals or other moieties that may be capable of significantly altering flame burning velocity, an enhanced AFD response is to be anticipated.     

Determination of Butyltins in Sea Water by Gas Chromatography with Flame Photometric Detection

Use of a gas chromatograph with a flame-photometric detector (GC-FPD) is described to determine butyltin compounds in sea water. The butyltins in an acidified water sample (pH 3.0) are first complexed with tropolone, followed by solid-phase extraction (SPE) with a tropolone-treated C₁₈ cartridge. HCI at a small concentration is then added to the concentrated SPE eluate before GC analysis. This procedure is simple and off-column derivatization of analytes is not required. The organotins, viz. mono-, di- and tributyltin, are separated as their respective chlorides on a capillary column (HP-1) and are detected with a flame-photometric detector and an interference filter at 610 nm. Recoveries of the three butyltin species are quantitative (> 90%). Based on a sea water sample 200-mL, the detection limits for mono-, di- and tributyltin are 6,4 and 3 ng tin L^?1, respectively. This method is applied to analysis of trace butyltins in various samples of sea water.     

The Performance of a Dual Alkali Aerosol Flame Ionization Detector for Gas Chromatography

Abstract

The described alkali flame ionization detector (AFID) differs from other designs by introducing the alkali salt into the detector in the form of an aerosol. The preheated, desolvated alkali aerosol salt is introduced into a dual hydrogen gas flame assembly. This detector shows no evidence of fatigue due to the constant delivery of salt into the detector, compared to the fixed alkali supply found in other versions, which can be depleted by vaporization and become easily contaminated. This AFID design also allows for operation as an FID by implementing a simple pneumatic procedure. This paper deals with the performance and optimization of the detector using a dual alkali salt aerosol flame design for organonitrogen and organophosphorus compounds. Detection limits were 23.5 pgN/sec for alachlor, 185 pgN/sec for dinoseb, and 4.83 pgP/sec to 10.1 pgP/sec for various pesticides studied. Selectivity ratios are tunable to 6.6 × 10⁶ gP/gC, 4.0 × 10⁴ gN/gC and 2.3 × 10³ gP/gN by establishing the appropriate detector gas flow rates.     

Determination of Volatile Sulfur Compounds in Beverage and Coffee Samples by Purge-and-Trap On-Line Coupling with a Gas Chromatography-Flame Photometric Detector

A sensitive and fast analytical method using purge-and-trap on-line coupling with gas chromatography was developed for the determination of trace volatile sulfur compounds including dimethyl sulfide (DMS), ethyl-methyl sulfide (EMS), and dimethyl disulfide (DMDS) in beverage and coffee samples. The analytes were purged for 12min from the sample by high purity nitrogen at a flow rate of 35KPa and preconcentrated in the cooled fused-silica capillary trap at –75°C. The NaCl content in the samples was maintained at 10%. The volatile sulfur compounds were separated with an Agilent-6890 gas chromatograph by a suitable temperature program and detected by means of a flame photometric detector (FPD). The detection limits were 80ngL^–1 for DMS, 80ngL^–1 for EMS, and 100ngL^–1 for DMDS, respectively. This method was successfully applied to the determination of volatile sulfur compounds in different beverage and coffee samples.     

用毛细管气相色谱脉冲火焰光度检测器测定汽油中的含硫化合物

采用毛细管气相色谱／脉冲火焰光度检测器（GC／PFPD）对催化裂化汽油中大部分硫化物做了定量和定性研究。在此基础上,考察了降硫助剂与平衡剂掺混后的使用性能,并采用GC／PFPI）对产物FCC汽油中硫化合物进行了分析测定,结果表明降硫助剂的加入使FCC汽油硫含量显著下降。     

The Gas Chromatographic Separation of Volatile Fluorides Using a Hydrogen Diffusion Flame as Detector

Abstract

An account is given of the preparation, separation and detection of volatile fluorides. These fluorides are formed by the reaction of chlorine trifluoride with the elements in a specially designed PTFE reaction vessel enclosed in an HF coil. A comparison is also made of a spectroscopic detector with a katharometer for the detection of the fluorides.

The separation of volatile fluorides has been reported to be partially successful on perfluorinated materials such as Kel-F oils or waxes on PTFE supports.^1–3 The present communication describes a more detailed investigation of these separations and also compares the performance of a newly developed spectroscopic detector⁴ with a conventional katharometer detector.     

气相色谱–火焰光度法测定进口天然气中4种形态硫

建立气相色谱–火焰光度法测定进口液化天然气中4种形态硫的方法。探讨了色谱柱、进样口温度、分流比、柱流速、升温程序和FPD检测器等对测定结果的影响。在优化的实验条件下,评价了方法的可靠性。4种形态硫化物的质量浓度在10.0~200.0μg/L范围内,其对数与峰面积对数呈良好的线性关系,线性相关系数r在0.983 3~0.999 2之间,检出限为1.7~7.7μg/L,测定结果的相对标准偏差为0.56%~0.68%(n=5)。用该法测定天然气形态硫标准气体,测定值与标准值相比,相对误差为–1.6%~–1.2%。该方法具有较高的准确度,可应用于进口天然气中4种形态硫的分析。     

顶空固相微萃取气相色谱-火焰光度法测定废水中烷基硫醇化合物

建立了顶空固相微萃取(HS-SPME)-气相色谱法测定人工湿地废水中烷基硫醇化合物的分析方法.详细研究了萃取参数如萃取涂层、萃取时间、萃取温度、样品体积、盐效应及样品pH值等对HS-SPME萃取乙硫醇(EtSH)、2-甲基-2-丙硫醇(Me-PrSH)、1-丙硫醇(1-PrSH)、2-丙硫醇(2-PrSH)、1-丁硫醇(1-BuSH)及环戊硫醇(CycloPeSH)(内标)的影响.富集的硫醇化合物经DB-VRX毛细管色谱柱分离,FPD检测.在优化的实验条件下,测定乙硫醇、2-甲基-2-丙硫醇、1-丙硫醇、2-丙硫醇、1-丁硫醇的线性范围介于0.12～16.21 μg/L之间; 检出限(3σ)介于0.97～22.11 ng/L之间.以环戊硫醇为内标物质,将本法用于废水中硫醇化合物的测定,获得满意结果.     

气相色谱法同时测定过氧化氢异丙苯中异丙苯和苯乙酮

建立了气相色谱-氢火焰离子化检测器同时测定过氧化氢异丙苯中异丙苯和苯乙酮含量的方法。样品用正己烷稀释,直接进样1.0μL,经DB-1柱分离后,用氢火焰离子化检测器检测,以保留时间定性,峰面积外标法定量。异丙苯、苯乙酮浓度分别在5.15～721μg/mL、5.8～812μg/mL范围内与峰面积呈良好线性关系,相关系数r分别为0.9997、0.9993。样品加标回收率在96.31%～101.2%之间,相对标准偏差在1.04%～2.17%之间。该法简便、快速,可用于过氧化氢异丙苯产品的质量控制。     

全二维气相色谱-飞行时间质谱/氢火焰离子化检测器对煤直接液化循环溶剂的定性与定量分析

建立了全二维气相色谱-飞行时间质谱/氢火焰离子化检测器(GC×GC-TOF MS/FID)对煤直接液化循环溶剂(CDLRS)定性定量的分析方法。采用TOF MS和FID两种检测器同时采集数据,并结合谱库检索、标准物质保留值对照、谱图解析、标准质谱图对照、全二维谱图特征以及提取化合物分子离子等定性方法,将TOF MS检测数据定性,然后将定性的烃类化合物以z值分类法分为18类;应用Chroma TOF数据处理软件将TOF MS数据的定性分类结果应用到FID的检测数据中,对TOF MS和FID采集的数据色谱峰面积归一化处理,实现CDLRS的半定量分析。GC×GC/FID定量结果显示:煤直接液化循环溶剂中饱和烃和芳烃分别占45.805%、53.938%,其中饱和烃主要为二环烷烃及三环烷烃,含量依次为14.644%、18.021%;芳烃主要为一环烷苯和二环烷苯,含量依次为19.759%、16.528%。该方法为CDLRS的定性定量提供了一种有效的分析方法。     

Combustion of Inert-Gas-Diluted Volatile Organic Compounds Using a Fuel-Rich Pilot Flame and Rotating Arc Plasma

Plasma Chemistry and Plasma Processing - This report proposes a method that uses plasma in combination with combustion to remove very low concentrations of volatile organic compounds (VOCs) that...     

Speciation Analysis of Butyltin Species in Water by Gas Chromatography with Flame Photometric Detection Using Quartz Surface-induced Tin Emission

A flame photometric detector using quartz surface-induced tin emission was designed and evaluated for quantification analysis of butyltin species. It has been demonstrated that this quartz surface-induced tin emission, centred at 390 nm, is more sensitive than the commonly used gas-phase emission at 610 nm. The dependence of detector response on quartz enclosure was studied. The operational variables such as hydrogen–air flow rate, carrier-gas flow rate and purge-gas flow rate were optimized. An analytical procedure for speciation analysis of butyltin species in water using simultaneous hydride generation with sodium borohydride and extraction into dichloromethane was established. The detection limits (defined as the signals that equal three times the deviations of the noise) were 0.3 pg of Sn for tetrabutyltin (TeBT), 5 pg of Sn for monobutyltin (MBT), 18 pg of Sn for dibutyltin (DBT) and 2 pg of Sn for tributyltin (TBT), which are approximately 10- to 30-fold better than those reported for using more commonly used gas-phase emission centred at 610 nm.     

光度法测定苦味酸的一种新显色体系

苦味酸的测定，在环境检测、药物分析、生化测定等方面都有重要意义。常见的测定方法有光度法、离子选择性电极法、荧光猝灭法等。以往的分析方法大部分存在着不同程度的重现性问题。近年来，有关苦味酸的高灵敏度高选择性和稳定性的测定方法报道较少。在文献[4]基础上，通过试验     

Determination of Camphor and Borneol in Traditional Chinese Medicines by Microwave-assisted Extraction and Gas Chromatography with Flame Ionization Detector

Abstract

In this work, microwave-assisted extraction (MAE) followed by gas chromatography with flame ionization detector (GC–FID) was developed for the rapid determination of camphor and borneol in three traditional Chinese medicines (TCM): Chrysanthemi indici, Flos Chrysanthemi indici and Amomum villosum lour. The optimal MAE conditions obtained were: acetone for solvent, with solvent having sample ratio of 12:1 (v/w); microwave power of 380 W, and an irradiation time of 4 min. Method validations were also studied. To demonstrate the proposed method, ultrasonic-assisted extraction (UAE) and steam distillation (SD), followed by GC-FID, were used to analyze camphor and borneol in thethree TCMs. The close results were obtained by the three methods. The results showed that the proposed MAE–GC–FID is a simple, rapid, and reliable method for quantitative analysis of camphor and borneol in TCM, and is also a potential tool for TCM quality assessment.     

新试剂偶氮胂HCS用于海产品中微量钍的测定

研究了新试剂 2 (2 胂酸基苯偶氮 ) 7 (2 羟基 3 羧基 磺酸苯偶氮 ) 1,8 二羟基 3,6 萘二磺酸 (简写作偶氮胂HCS)与钍的显色反应 ,建立了一种测定海产品中微量钍的光度法。在3 0mol·L-1硝酸介质中 ,钍与偶氮胂HCS发生灵敏的显色反应 ,生成 1∶2的绿色配合物。该配合物的吸收峰位于 676nm ,表观摩尔吸光系数为 8.5 4× 10 4 L·mol-1·cm-1。钍含量在 0～ 30 μg 2 5ml符合比耳定律。由于偶氮胂HCS水溶性非常好 ,可在高酸性条件下反应 ,使显色反应有极佳的选择性 ,大量的常见金属离子以及铀、稀土不干扰微量钍的测定 ,用于海产品中钍的分析时可不经分离而直接进行