光离子化检测器便携式气相色谱仪快速测定空气中苯系物

本文研究了使用光离子化检测器便携式气相色谱仪,直接测定空气中ｍｇ／ｍ３级苯系物（苯、甲苯、乙苯、邻、间、对位的二甲苯及异丙苯）的快速分析方法。方法的线性范围为０～１００ｍｇ／ｍ３,相关系数均在０．９９９以上,方法的变异系数分别为２．９～１２．５％（５ｍｇ／ｍ３）,３．４～７．９％（３０ｍｇ／ｍ３）,方法最低检测限达０．２～１．０ｍｇ／ｍ３。     

Artifact evidence in carbonyl compound sampling using the enclosure technique with cuvette system

Biogenic hydrocarbon emission rates from individual plant species have been estimated experimentally placing small plants or branches in enclosures and measuring the emission rates of the compounds. All-Teflon chambers (cuvettes) where air samples are drawn through tubes packed with adsorbents, have been commonly used for plant enclosure. Sampling of carbonyl compounds emitted from plants has been done using 2,4-dinitrophenylhydrazine coated particles and the derivative carbonyl compounds have been analyzed by HPLC-UV. In this work, the enclosure technique using a cuvette for measurements of carbonyl compound emissions from plants was evaluated. Blank measurements in an empty cuvette have revealed quite different results for experiments performed under laboratory and field conditions. Rigorous univariate statistical analysis of the data obtained indicate that the analytical procedure to determine carbonyl compounds at trace levels in emission samples using the cuvette may lead to positive artifacts during field sampling. This analysis applied to laboratory measurements showed no difference in the results for the cuvette and external lines. Multivariate statistical calculations point out that solar light intensity accounts for the high carbonyl compound levels, especially for acetaldehyde, in the empty cuvette.     

利用保留时间锁定软件对水中挥发性有机物进行气相色谱测定

使用保留时间锁定软件 (RTL) ,在气相色谱体系中建立了水质中 5 3种挥发性有机物的保留时间数据库 ,使原始的保留时间成为化合物定性的可靠参数 ,实现了未知样品在色谱仪上的定性 ,提高了分析效率。     

Development of a diffusive sampling method for determination of methyl isocyanate in air

A diffusive sampling method for determination of methyl isocyanate in air has been developed. A glass fibre filter impregnated with 1-(2-methoxyphenyl)piperazine in a commercially available diffusive sampling device was used to collect methyl isocyanate and the derivative formed was analysed with LC-MS/MS. The sampling rate was determined to be 15.6 ml min(-1), with a relative standard deviation of 7.3%. The sampler was validated for sampling periods from 15 min to 8 h, for relative humidities from 20% to 80% and for concentrations from I to 46 microg m(-3). A field validation was also made and the diffusive sampling results showed no difference compared to a pumped reference method. The impregnated filters have to be stored apart from the diffusive sampler housing and loaded into the sampler prior to each sampling.     

反相高效液相色谱分析空气和废气中己内酰胺的方法研究

研究了反相高效液相色谱分析空气和废气中己内酰胺的方法。该方法以VWD为检测器,检测波长为210nm,流动相为乙腈∶纯水=10∶90,流动相流速为1ml/min。在已选择色谱条件下,连续运行10次,己内酰胺平均出峰时间为4 2min,保留时间和峰面积的相对标准偏差分别为1 5%和3 5%,采样体积为90L时,检测下限为0 01mg/m3,上限为2 20mg/m3,回收率在105 2%-106 3%。     

An evaluation of a fast sampling procedure for the trace analysis of volatile organic compounds in ambient air

This study deals with the evaluation of a fast method for sampling of volatile organic compounds in ambient air. Special bags made of an inert material are used together with a large handpump which allows a sampling of one liter per second. After the sampling, the pollutants are concentrated by adsorption on Tenax and transfered by heat desorption, to a small capillary precolumn cooled with liquid nitrogen, or directly trapped on the precolumn. The suitability of this technique was evaluated by sampling complex synthetic mixtures of known concentration and composition, after which the samples were submitted to a series of operations such as transport, aging, changing of the humidity, heating and cooling, irradiation, etc. Changes in the original mixtures, caused by adsorption, diffusion, chemical or photochemical reactions were investigated by GC-MS analysis. The results of the study show that under certain conditions the samples can be preserved for a rather long period of time without noticeable changes in composition. However for certain compounds, severe quantitative losses occur after one day storage. Finally a practical application of this method is described in a recent case of strong odour annoyance by a chemical plant in the north of Belgium.     

Development of a sampling method for the simultaneous monitoring of straight-chain alkanes, straight-chain saturated carbonyl compounds and monoterpenes in remote areas

Studies have shown that biogenic compounds, long chain secondary compounds and long lifetime anthropogenic compounds are involved in the formation of organic aerosols in both polluted areas and remote places. This work aims at developing an active sampling method to monitor these compounds (i.e. 6 straight-chain saturated aldehydes from C6 to C11; 8 straight-chain alkanes from C9 to C16; 6 monoterpenes: α-pinene, β-pinene, camphene, limonene, α-terpinene, & γ-terpinene; and 5 aromatic compounds: toluene, ethylbenzene, meta-, para- and ortho-xylenes) in remote areas. Samples are collected onto multi-bed sorbent cartridges at 200 mL min(-1) flow rate, using the automatic sampler SyPAC (TERA-Environnement, Crolles, France). No breakthrough was observed for sampling volumes up to 120 L (standard mixture at ambient temperature, with a relative humidity of 75%). As ozone has been shown to alter the samples (losses of 90% of aldehydes and up to 95% of terpenes were observed), the addition of a conditioned manganese dioxide (MnO(2)) scrubber to the system has been validated (full recovery of the affected compounds for a standard mixture at 50% relative humidity--RH). Samples are first thermodesorbed and then analysed by GC/FID/MS. This method allows suitable detection limits (from 2 ppt for camphene to 13 ppt for octanal--36 L sampled), and reproducibility (from 1% for toluene to 22% for heptanal). It has been successfully used to determine the diurnal variation of the target compounds (six 3 h samples a day) during winter and summer measurement campaigns at a remote site in the south of France.     

填充柱气相色谱法测定空气和废气中的乙酸

在用蒸馏水吸收空气或废气中的乙酸后,采用5%PEG20M+0.5%H3PO4chromo-sorbHP80～100目2m×2mm玻璃填充柱,GC直接进样测定蒸馏水中的乙酸,方法简便、快捷,变异系数为2%～5%,加标回收率为85%～106%,最低检出浓度为0.16mg/m3。     

Colorimetric determination of formaldehyde in air using a hanging drop of chromotropic acid

A simple and sensitive method to determine parts per billion (ppb) of atmospheric formaldehyde in situ, using chromotropic acid, is described. A colorimetric sensor, coupled to a droplet of 15.5 microL chromotropic acid, was constructed and used to sample and quantify formaldehyde. The sensor was set up with two optical fibers, a light emitting diode (LED) and two photodiodes. The reference and transmitted light were measured by a photodetection arrangement that converts the signals into units of absorbance. Air was sampled around the chromotropic acid droplet. A purple product was formed and measured after the sampling terminated (typically 7 min). The response is proportional to the sampling period, analyte concentration and sample flow rate. The detection limit is approximately 2 ppb and can be improved by using longer sampling times and/or a sampling flow rate higher than that used in this work, 200 mL min-1. The present technique affords a simple, inexpensive near real-time measurement with very little reagent consumption. The method is selective and highly sensitive. This sensor could be used either for outdoor or indoor atmospheres.     

TEA(三乙醇胺)挂片测定空气中NO2的滤膜制备方法

介绍了一种用于TEA挂片测定NO2的滤膜制备方法,解决了原方法中存在的滤膜空白值偏高且不稳定的问题.实验结果表明,该方法可用于大面积、多点位同步监侧中大批量滤膜的制备.     

The role of hydrodynamics, matrix and sampling duration in passive sampling of polar compounds with Empore SDB-RPS disks

There is an increasing need to monitor concentrations of polar organic contaminants in the aquatic environment. Integrative passive samplers can be used to assess time weighted average aqueous concentrations, provided calibration data are available and sampling rates are known. The sampling rate depends on environmental factors, such as temperature and water flow rate. Here we introduce an apparatus to investigate the sampling properties of passive samplers using river-like flow conditions and ambient environmental matrices: river water and treated sewage effluent. As a model sampler we selected Empore SDB-RPS disks in a Chemcatcher housing. The disks were exposed for 1 to 8 days at flow rates between 0.03 and 0.4 m s(-1). Samples were analysed using a bioassay for estrogenic activity and by LC-MS-MS target analysis of the pharmaceuticals sulfamethoxazole, carbamazepine and clarithromycin. In order to assess sampling rates of SDB disks, we also measured aqueous concentrations of the pharmaceuticals. Sampling rates increased with increasing flow rate and this relationship was not affected by the environmental matrix. However, SDB disks were only sampling in the integrative mode at low flow rates <0.1 m s(-1) and/or for short sampling times. The duration of linear uptake was particularly short for sulfamethoxazole (1 day) and longer for clarithromycin (5 days). At 0.03 m s(-1) and 12-14 degrees C, the sampling rate of SDB disks was 0.09 L day(-1) for clarithromycin, 0.14 L day(-1) for sulfamethoxazole and 0.25 L day(-1) for carbamazepine. The results show that under controlled conditions, SDB disks can be effectively used as passive sampling devices.     

A diffusive sampling device for the determination of formaldehyde in air using N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) as reagent

A new method utilizing the diffusive sampling of formaldehyde in air has been developed. Formaldehyde is sampled with the use of a glass fiber filter impregnated with N-methyl-4-hydrazino-7-nitrobenzofurazan (MNBDH) and phosphoric acid. The formaldehyde hydrazone formed is desorbed from the filter with acetonitrile and determined by high-performance liquid chromatography (HPLC) with UV/visible detection at 474 nm. The sampling rate was determined to be 24.7 mL min-1 with a relative standard deviation of 7% for 48 experiments. The measured sampling rates were not dependent on the formaldehyde concentration (0.1-1.0 mg m-3), sampling time (15-482 min) or relative humidity (20-85%). The detection limit was 70 micrograms m-3 for a 15 min sampling period and 2 micrograms m-3 for an 8 h sampling period.     

Performances and application of a passive sampling method for the simultaneous determination of nitrogen dioxide and sulfur dioxide in ambient air

The performances and applicability of a diffusion tubesampler for the simultaneous measurements of NO₂ andSO₂ in ambient air were evaluated. SO₂ andNO₂are collected by the passive sampler using triethanolamine astrapping agent and are determined as sulphate and nitrite withion chromatography. The detection limit (2.3 g m^-3 ofNO₂ and 4.2 g m^-3 of SO₂ for two weekssampling) is adequate for the determination of concentrationsin urban and industrial areas. Precision of the method as RSDis in mean 5% for NO₂ and 12% for SO₂ at theconcentration levels in urban areas. Calibration of the methodwas performed in the field conditions by comparison between theresponses of sampler and the concentrations measured by thecontinuous monitors. High degree of linearity (correlationcoefficients > 0.8) is found between the passive sampler tubeand the continuous monitor data for both NO₂ and SO₂.To reduce the wind velocity influence on passive sampling ofdiffusion tubes, a protective shelter was tested in this study.The overall uncertainty of one measure for the optimised methodis estimated at 5 g m^-3 for NO₂ and 6g m^-3 for SO₂. Suitability of this passivesampling method for air pollution monitoring in urban areas wasdemonstrated by the results shown in this paper on a campaigncarried out in the French agglomeration.     

膜分离紫外光度法连续测定二氧化氯的应用

利用 Cl O2 能透过微孔性聚四氟乙烯膜 (PTFE)而制成 Cl O2 连续流动分离装置 ,建立了膜分离紫外光度法连续测定二氧化氯的测试方法。用此方法测定江苏某水厂净水流程线上各采样点的二氧化氯浓度 ,并对测定结果进行显著性检验 ,确定当水中二氧化氯浓度大于或等于 0 .0 8mg/ L时 ,此方法与美国 Vulcan公司推荐的连续碘量法无显著性差异     

Application of portable gas chromatography-photo ionization detector combined with headspace sampling for field analysis of benzene, toluene, ethylbenzene, and xylene in soils

A method based on headspace (HS) sampling coupling with portable gas chromatography (GC) with photo ionization detector (PID) was developed for rapid determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in soils. Optimal conditions for HS gas sampling procedure were determined, and the influence of soil organic matter on the recovery of BTEX from soil was investigated using five representative Chinese soils. The results showed that the HS-portable-GC-PID method could be effectively operated at ambient temperature, and the addition of 15 ml of saturated NaCl solution in a 40-ml sampling vial and 60 s of shaking time for sample solution were optimum for the HS gas sampling procedure. The recoveries of each BTEX in soils ranged from 87.2 to 105.1 %, with relative standard deviations varying from 5.3 to 7.8 %. Good linearity was obtained for all BTEX compounds, and the detection limits were in the 0.1 to 0.8 μg kg^?1 range. Soil organic matter was identified as one of the principal elements that affect the HS gas sampling of BTEX in soils. The HS-portable-GC-PID method was successfully applied for field determination of benzene and toluene in soils of a former chemical plant in Jilin City, northeast China. Considering its satisfactory repeatability and reproducibility and particular suitability to be operated in ambient environment, HS sampling coupling with portable GC-PID is, therefore, recommended to be a suitable screening tool for rapid on-site determination of BTEX in soils.     

Determination of 14 amines in air samples using midget impingers sampling followed by analysis with ion chromatography in tandem with mass spectrometry

An Ion Chromatography-Mass Spectrometry (IC-MS) method was developed for the simultaneous quantification of 14 volatile amines in air. The method includes collection of compounds into two midget impingers in a row filled with 15 ml of ultrapure water. The analytical performances with mass spectrometry detection were compared to those obtained with classical conductivity detection. The use of mass spectrometry detection (in SIM mode) overcomes most of the coelutions encountered with conductivity detection. Although the linearity domain of calibrations is reduced for the MS detection as compared with the CD detection, the detection limits in MS detection are highly lowered allowing the quantification of amines at the levels of μg m(-3) in air with a good accuracy for most compounds (RSD of less than 10%). This method was successfully applied to the analysis of amines released from polyurethane foams. Seven amines were identified and some in high concentrations, like dimethylaminoethanol, NIAX and TEDA.     

某乡镇大气中毒害挥发性有机物的研究

对经济较发达的某乡镇大气的毒害挥发性有机化合物研究表明,该镇城区及其较发达的乡村已受到一定程度的有机污染,大气中主要存在苯系物、萘、氯代烃等毒害挥发性有机化合物.个别样品的苯乙烯含量高达14.50μg/m3,此值已超过中国居住区最高容许浓度.     

Erroneous mass transit system and its tended relationship with motor vehicular air pollution (An integrated approach for reduction of urban air pollution in Lahore)

Air pollution is threat to the lives of people living in big cities of Pakistan. In Lahore 1,250 people die annually because of air pollution.Mass transit system that can be put forth as solution to urban air pollution is contingent with right choice of system and its affiliation with motorized vehicles and nature of urban air pollution.Existing mass transit system in Lahore due to untrue operation causes surfeit discharge of motor vehicular carbon monoxide. Tended relationships of mass transit system with motorized vehicles and urban air pollution are quite noteworthy. The growing motor vehicles (a consequence of flawed public mass transit system) are potential source of urban air pollution. This paper attempts to highlight correlations and regression curves of existing mass transit system. Further it recommends a two facet approach for reduction of motor vehicular air pollution in Lahore.     

The use of semipermeable membrane devices as passive samplers to determine persistent organic compounds in indoor air

In the study reported here semipermeable membrane devices (SPMDs) were used to sample 28 PAHs and 19 PCBs in the gas phase in 15 single-family houses located in an area where domestic wood burning is widespread. Eight of the households used wood burning appliances whereas the others used other systems for residential heating. Most of the studied compounds were found in the houses: the PAHs at levels that were similar to or slightly higher than published SPMD-sampled levels for background or urban sites in Sweden, and the PCBs at levels that were somewhat lower than those recently found in both indoor and outdoor urban locations. A principal component analysis revealed that wood-burning heating systems may contribute to PAHs in indoor air. The sources may be emissions indoors or penetration from outdoors. The convenience of SPMD technology facilitates its use for semi-quantitative screening and monitoring of various persistent organic compounds indoors in dwellings and working environments.     

Passive sampling in combination with thermal desorption and gas chromatography as a tool for self-assessment of chemical exposure

Diffusive samplers for monitoring of air quality are user-friendly devices that can normally be operated by the user himself. Hence these samplers are suitable for self-assessment. Practical and work organisational aspects of self-assessment of chemical exposure were studied in different occupational settings. It was found that the diffusive sampler used in these studies, the Perkin-Elmer tube in combination with thermal desorption, worked well for the purpose and could be correctly handled by the individuals using it. The results from self-assessments agreed well with expert measurements carried out by an occupational hygienist. However, in order to obtain a sustainable system of self-assessment strong organizational support is needed.