顶空气相色谱法测定工作场所空气中的乙酸乙酯

采用顶空气相色谱法测定工作场所空气中的乙酸乙酯。气态乙酸乙酯用活性炭管吸附,二氯甲烷解吸,顶空进样,HP–FFAP毛细管柱分离,FID检测器测定,峰面积定量。乙酸乙酯的质量浓度在1.76~880.0μg/m L范围内与色谱峰面积呈良好的线性,相关系数r=0.999 4。不同浓度样品批内测定结果的相对标准偏差为1.34%~3.61%(n=7),批间测定结果的相对标准偏差为1.04%~4.78%(n=7),加标回收率为91.02%~100.29%,方法检出限为0.32μg/m L,解吸效率为91.28%~95.19%。对于100 mg活性炭,乙酸乙酯的穿透容大于2.2 mg,当其浓度在17.6~17 600 mg/m3时,采样效率为91.23%~97.40%,常温下可以保存10 d。该方法各项指标均达到《工作场所空气中有毒物质检测方法研制规范》的要求,适用于工作场所空气中乙酸乙酯的现场监测。     

活性氧化铝柱-气相色谱法测定工作场所空气中“四烯”的方法研究

采用活性氧化铝柱-气相色谱法对作业场所空气中乙烯、丙烯、丁烯、丁二烯进行活性炭采样,热解吸后进样分析。活性炭管对"四烯"的吸附性良好,测定结果的相对标准偏差为0.37%～2.08%;乙烯、丙烯、丁烯、丁二烯检出限分别为0.0010、0.000520、.00083、0.0003 mg/L;样品的平均解吸效率为93.7%～98.59%;样品的平均采样效率为93.9%～99.1%;乙烯、丙烯、丁烯、丁二烯穿透容量分别为9.58、.87、.4、7.1 mg;样品在室温下放置7 d,其平均样品损失率不大于5.58%,在4～10℃环境放置10 d,其平均样品损失率不大于7.11%,空气中乙烷对本方法无干扰。该法可满足职业卫生检测的要求。     

Modern Analytical Methods for Monitoring Workplace Atmospheres

Abstract

Since measurements of exposure to hazardous substances were made obligatory in Germany under the Hazardous Material Regulation and Regulations for Accident Prevention there has been a need for widely-applicable, economic methods for determining airborne organic substance concentrations at workplaces. The relevant limits, which are based on toxicological and industrial hygiene data, are drawn up annually by the German Science Foundation and published as “Technische Regel für gefährliche Arbeitsstoffe” (TRgA 900) by the Ministry of Employment and Welfare.

Most organic substances, that have been assigned limits can be determined by gas liquid chromatography. The system described here is based on multicomponent GLC analysis. It has been used at BASF, the chemical-manufacturing company, where since 1979 approximately fifteen thousand workplaces have been evaluated. Hazardous substances have been detected at levels down to a few micrograms per cubic meter.

The standard system encompasses:

–-personal air samplers operating for 8 h;

–-adsorption by a solid sorbent;

–-desorption by solvent;

–-simultaneous GLC-separation on two different capillary columns;

–-computer correlation of the qualitative and quantitative data of the two chromatograms (plausibility check);

–-automatic print-out of the analytical report;

–-transfer of the results to a data bank for documentation.

Details are given of the method involving adsorption on activated charcoal and desorption with carbon disulfide. Benefits, cost advantages, and limitations are discussed.

Special sampling by means of other adsorbents (e.g. silica gel) in conjunction with special desorption, formation of derivatives, headspace analysis, and adsorption by liquids are techniques used to supplement the standard method of organic trace analysis in the field of industrial hygiene.     

Optical molecular fluorescence determination of ultra-trace beryllium in occupational and environmental samples using highly alkaline conditions

Exposures to beryllium (Be), even at extremely low levels, can cause severe health effects in a percentage of those exposed; consequently, occupational exposure limits (OELs) promulgated for this element are the lowest established for any element. This work describes the advantages of using highly alkaline dye solutions for determination of Be in occupational hygiene and environmental samples by means of an optical molecular fluorescence technique after sample extraction in 1–3% (w?w^?1) aqueous ammonium bifluoride (NH₄HF₂). Improved attributes include the ability to further enhance the detection limits of Be in extraction solutions of high acidity with minimal dilution, which is particularly beneficial when NH₄HF₂ solutions of higher concentration are used for extraction of Be from soil samples. Significant improvements in Be method detection limits (MDLs) are obtained at levels manyfold below those reported previously for this methodology. Notably, MDLs for Be of <0.01 ng L^?1 /0.1 ng per sample have been attained, which are superior to MDLs routinely reported for this element by means of the most widely used ultra-trace elemental measurement technique, inductively coupled plasma mass spectrometry (ICP-MS). Very low MDLs for Be are essential in consideration of reductions in OELs for this element in workplace air by health organisations and regulatory agencies in the USA and internationally. Applications of enhanced Be measurements to air filter samples, surface wipe samples, soils and newly designed occupational air sampler inserts are illustrated.     

气相色谱法测定工作场所空气中正己烷、丙酮、丁酮和乙酸丁酯的含量

用气相色谱法对空气中正己烷、丙酮、丁酮和乙酸丁酯的含量进行测定。采用活性炭管采集了空气中的正己烷、丙酮、丁酮和乙酸丁酯,采用二硫化碳进行解吸,用Agilent 19091N-216HP-INNOWAX Polyethylene Glycol毛细管色谱柱分离,氢焰离子化检测器检测。正己烷、丙酮、丁酮和乙酸丁酯的检出限(3S/N)为0.43,0.30,0.44,1.7mg.L-1。方法的解吸率在86.7%～100.3%之间,相对标准偏差(n=6)在1.97%～3.89%之间。     

A Novel Method for Inhalation Control of Workplace Anthropogenic Pollutant Particles

This in vitro study investigated electrically charging effect on the deposition of inhaled workplace anthropogenic pollutant particles (APP) in a hollow throat cast model. Many occupational lung diseases are associated with exposure to workplace dust particles and other pollutants. Since the human throat is an effective filter, this study devised a novel idea of charging particles, and studying their deposition in the throat. Simulated workplace aerosol particles were generated from a commercially available nebulizer, and charged by a corona charger. Charged and uncharged particles were allowed to pass through a polyester resin cast of cadaver based throat, a replicate of a human oropharyngeal region. The aerosol particles' size and charge distribution were characterized by an Electronic Single Particle Aerodynamic Relaxation Time (ESPART) analyzer before and after passing the throat cast. The ESPART operates on the principle of Laser Doppler Velocimetry to measure simultaneously aerodynamic diameter and electrostatic charge on a single particle basis and in real time. The study results revealed that electrically charging increased agglomeration of smaller particles and increased deposition. Deposition of charged particles increased with increasing particle size which can be explained as the effect of inertial impaction.     

Improved sampling and analytical method for airborne carbon disulfide measurement in the workplace

Summary An improved sampling and analytical method for airborne carbon disulfide (CS₂) both in the laboratory and in a rayon viscose manufacturing plant is described. A tube-type diffusive sampler (ATD) packed with solid Spherocarb was used for airborne CS₂ collection. The ATD was then thermally desorbed and analyzed by (GC-MS). A standard curve range of 0.69 to 103.4 μg was established with correlation coefficient (r)>0.998. Desorption efficiency was 100% mean recovery 97.8% and coefficient of variation<10%. The limit of detection (LOD) was 0.21 μg and limit of quantitation (LOQ) 0.69 μg. Temperature and humidity effects were not significant. There was no influence from tube direction to exposure gas stream. The uptake rate was stable over an 8h period. Even after 90 repeated usages, the uptake rate still remained quite stable. ATD samples were stable at <4°C for at least 2 weeks. Field validation data showed a strong linear correlation (r>0.97) between the proposed method and the current method for fixed-point samples. The proposed method can provide a specific, sensitive, convenient, and reliable tool for assessment of occupational exposure to CS₂. Using this method to assess CS₂ exposures gives findings comparable to those of the traditional method with respect to accuracy, precision, and effects of environmental interference.     

Systematic errors in the readings of track etch neutron dosemeters caused by the energy dependence of response

A study has been performed to assess the extent to which variations in the energy dependence of response of neutron personal dosemeters can cause systematic errors in readings obtained in workplace fields. This involved a detailed determination of the response functions of personal dosemeters used in the UK. These response functions were folded with workplace spectra to ascertain the under- or over-response in workplace fields.     

基于混合方法的工作乐趣分类模型构建及其效用的实证研究

本文采用混合研究的方法,分析目前两岸企业工作乐趣的开展类型和效果。在构建类型学概念模型基础上,修订中华工作乐趣测量量表并检验不同乐趣活动对员工的绩效影响差异。数据分析结果表明社交型、放松型、辅助型和福利型乐趣的四类结构信效度良好,但不同类型乐趣对员工满意度、任务绩效和组织公民行为的影响存在明显差异。     

气相色谱法测定工作场所空气中的毒死蜱

建立气相色谱测定工作场所空气中毒死蜱的方法。采用硅胶管采集空气样品,丙酮溶剂解吸,用气相色谱工作曲线法测定毒死蜱的含量。在采样体积为4.5 L,解吸体积为1.0 m L的条件下,空气中毒死蜱的含量在0.022~2.2μg/L范围内与色谱峰面积呈良好的线性关系,线性相关系数为0.999 5,检出限为0.002μg/L。加标回收率为99.4%~97.3%,测定结果的相对标准偏差为4.6%~6.0%(n=6)。该方法适合测定工作场所空气中的毒死蜱。