Shimadzu GC2010工作场所空气有毒物质黄磷测定岛津硬质玻璃柱3%SE30+2%QF-1/CWA

本标准规定了监测工作场所空气中无机含磷化合物浓度的方法。
       本标准适用于工作场所空气中无机含磷化合物浓度的测定。


黄磷的吸收液采集－气相色谱法
8.1 原理
空气中黄磷用吸收液采集，直接进样，经SE-30和QF-1 混合柱分离，用火焰光度检测器检测，以保留时间定性，峰面积定量。
8.2 仪器
8.2.1 多孔玻板吸收管。
8.2.2 空气采样器，流量0～3L/min。
8.2.3 具塞比色管，10ml。
8.2.4 微量注射器，1ml，10ml。
8.2.5 气相色谱仪，火焰光度检测器（磷滤光片，526nm）。
仪器操作参考条件
色谱柱：1.5m×3mm 玻璃柱，SE-30:QF-1:Chromosorb WAW DMCS = 3:2:100；
柱温：70℃；
汽化室温度：190℃；
检测室温度：200℃；
载气（氮气）流量：30ml/min。
8.3 试剂
8.3.1 吸收液：100ml 苯和150ml 无水乙醇混合。
8.3.2 SE-30和QF-1：色谱固定液。
8.3.3 Chromosorb WAW DMCS：色谱担体，60～80目。
8.3.4 标准溶液：于25ml 容量瓶中，加入10ml 苯（优级纯），准确称量后，加入一粒经滤纸吸干水份的黄磷，再准确称量，用苯（优级纯）定容。由2次称量之差计算溶液中黄磷的浓度。此溶液为标准贮备液。置于冰箱内保存。临用前，用吸收液稀释成1.0μg/ml 黄磷标准溶液。或用国家认可的标准溶液配制。

 
This standard specifies the method for monitoring the concentration of inorganic phosphorus containing compounds in the air of the workplace.
This standard is applicable to the determination of the concentration of inorganic phosphorus containing compounds in the air of the workplace.
Collection of yellow phosphorus absorption solution - gas chromatography method
8.1 Principle
Yellow phosphorus in the air is collected using absorption solution, directly injected, separated by SE-30 and QF-1 mixed columns, detected by flame photometric detector, qualitatively determined by retention time, and quantitatively determined by peak area.
8.2 Instruments
8.2.1 Porous glass absorption tube.
8.2.2 Air sampler, flow rate 0-3L/min.
8.2.3 Color tube with stopper, 10ml.
8.2.4 Microinjector, 1ml, 10ml.
8.2.5 Gas chromatograph, flame photometric detector (phosphorus filter, 526nm).
Reference conditions for instrument operation
Chromatography column: 1.5m × 3mm glass column, SE-30:QF-1:Chromosorb WAW DMCS = 3:2:100；
Column temperature: 70 ℃;
Vaporization chamber temperature: 190 ℃;
Testing room temperature: 200 ℃;
Carrier gas (nitrogen) flow rate: 30ml/min.
8.3 Reagents
8.3.1 Absorption solution: Mix 100ml of benzene and 150ml of anhydrous ethanol.
8.3.2 SE-30 and QF-1: Chromatographic fixatives.
8.3.3 Chromosorb WAW DMCS: chromatographic support, 60-80 mesh.
8.3.4 Standard solution: In a 25ml volumetric flask, add 10ml of benzene (high-purity), weigh accurately, add a piece of yellow phosphorus that has been dried with filter paper, weigh accurately, and make up to volume with benzene (high-purity). Calculate the concentration of yellow phosphorus in the solution based on the difference between two weighings. This solution is a standard stock solution. Store in the refrigerator. Before use, dilute with absorption solution to a standard solution of 1.0 μ g/ml yellow phosphorus. Or prepare with nationally recognized standard solutions.