工作场所空气中异丙胺测定方法研究

发布时间：2018-06-23 17:20

  本文选题：异丙胺 + 气相色谱　； 参考：《首都经济贸易大学》2013年硕士论文

【摘要】：异丙胺属有毒物质，吸入异丙胺蒸气或雾，对皮肤有中等刺激性，对眼部有严重刺激性，对粘膜中等刺激性。摄取和黏膜吸收有中等毒性。工人暴露在异丙胺环境中，被发现会出现短暂的视觉干扰，还会造成角膜水肿，液体或雾严重损害眼睛，重者可致失明对呼吸道有刺激性；持续高浓度吸入引起肺水肿。可致皮肤灼伤。口服灼伤消化道，大量口服可引起死亡。而异丙胺作为一种重要的精细化工中间体，其用途主要用作溶剂、有机合成、乳化剂、橡胶硫化促进剂、杀虫剂、脱毛剂、表面活性剂、2，4-D的增溶剂等。我国对工作场所空气中异丙胺接触限值做了规定，GBZ2.1-2007《工作场所有害因素职业接触限值》中规定时间加权平均容许浓度（PC-TWA）为12mg/m~3,短时间接触容许浓度（PC-STEL）为24mg/m~3，但是没有相应的标准检测方法。 目的建立工作场所空气中异丙胺测定方法，为职业卫生领域该物质测定提供方法支持。 方法对比气相色谱法和液相色谱法，采用实验室静态配齐的试验方法，对仪器测定条件进行优化和改进，采用气相色谱法，以保留时间定性，以已知标准系列浓度为横坐标，测得的峰面积为纵坐标建立标准曲线进行定量，对方法的各项性能指标进行评估。 结果方法采用气相色谱法，该方法灵敏度较高，色谱峰形尖锐，检出限（LOD）为0.688μg/mL。定量下限（LOQ）为2.30μg/mL，在采样20L的条件下，该方法的最低检出浓度为0.12mg/m~3。配置浓度为0、6.88μg/mL、13.76μg/mL、27.52μg/mL、55.04μg/mL、110.08μg/mL、220.16μg/mL、550.40μg/mL的标准系列，以浓度为横坐标，测得峰面积为纵坐标，得回归方程Y=1671.316X-3186.64,相关系数r=0.9994,线性范围在6.88～550.4μg/mL。该方法批内精密度为2.3%～4.4%，批间精密度为1.4%～5.0%，解析效率为91.8%～98.2%，样品于4℃冰箱条件下保存至少可存放七天。 结论本方法灵敏度较高，峰形较好，，适用于职业卫生领域空气中异丙胺浓度测定。
[Abstract]:Isopropylamine is a toxic substance, inhaling isopropylamine vapor or fog, has moderate irritation to the skin, serious irritation to the eyes, and middle irritation to the mucous membrane. Uptake and mucosal absorption are moderately toxic. Workers exposed to isopropylamine are found to have transient visual disturbances, corneal edema, fluid or fog serious damage to the eye, severe blindness, irritation to the respiratory tract, and persistent high concentrations of inhalation to cause pulmonary edema. Can cause skin burns. Oral burns the digestive tract, a large number of oral can cause death. As an important fine chemical intermediate, isopropylamine is mainly used as solvent, organic synthesis, emulsifier, rubber vulcanizing accelerator, insecticide, hair remover, surfactant and so on. The limit of exposure to isopropylamine in workplace air has been stipulated in GBZ2.1-2007 (Occupational exposure limit for harmful factors in the Workplace). The time-weighted mean allowable concentration (PC-TWA) is 12 mg / m-1, and the allowable concentration of short time exposure (PC-STEL) is 24 mg / m ~ (3), but there is no phase. The standard test method should be used. Objective to establish a method for the determination of isopropylamine in workplace air. Methods by comparing gas chromatography with liquid chromatography, the test method of static matching in laboratory was used to optimize and improve the measuring conditions of the instrument. The determination conditions were determined by gas chromatography with the retention time and the known standard series concentration as the horizontal coordinate. The measured peak area is measured by establishing a standard curve in the ordinate to evaluate the performance of the method. Results Gas chromatography was used. The sensitivity of the method was high, the peak shape was sharp, and the detection limit (LOD) was 0.688 渭 g / mL. The low limit of quantification (LOQ) is 2.30 渭 g / mL. Under the condition of 20 L sampling, the lowest detection concentration of this method is 0.12 mg / mL. The standard series of 0.6.88 渭 g / mLN 13.76 渭 g / mL 27.52 渭 g / mL 55.04 渭 g / mL 110.08 渭 g / mL 220.16 渭 g / mL 550.40 渭 g / mL, with the concentration as the horizontal coordinate and the peak area measured as the vertical coordinate, the regression equation Y _ (1671.316X-3186.64) is obtained, the correlation coefficient is 0.9994, and the linear range is 6.88 ~ 550.4 渭 g / mL-1 / mL, and the linear range is 6.880.550.4 渭 g / mL-1 / mL, and the regression equation is Y _ (1671.316X-3186.64), the correlation coefficient is 0.9994, and the linear range is 6.88 ~ 550.4 渭 g 路mL ~ (-1). The precision of the method is 2.3and 4.4, and the precision between batches is 1.40.The analytical efficiency is 91.8and 98.2.The sample can be stored for at least seven days under the condition of 4 鈩

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