Ono-Ogasawara M, Furuse M, Matsumura Y
National Institute of Industrial Health, Kawasaki, Japan.
Ind Health. 1990;28(4):175-84. doi: 10.2486/indhealth.28.175.
A method for determining phosphine was developed using adsorption sampling followed by colorimetric measurement. Two types of adsorbent used in this study were prepared from silica gel by impregnation with potassium permanganate (1% w/w) or (mercury(II) chloride and sodium chloride) (0.2 + 0.2% w/w). Each adsorbent (150 mg) packed in a glass tube had the capacity to adsorb 0.3 ppm of phosphine in 3 l of test gas passing through at a rate of 300 ml/min without breakthrough. The adsorbed phosphine was desorbed into solutions as phosphate and the recovered phosphate was determined by ICP-AES or by one of two kinds of colorimetric methods for phosphate based on the molybdenum blue method, i.e., the colorimetric method following JIS K 0102 and that following the NIOSH Manual of analytical method, No. S 332. When 0.01 ppm of phosphine in 3 l of test gas was adsorbed on the potassium permanganate adsorbent and determined by the JIS method, 93.8% of the phosphine was recovered as phosphate with a CV of 12.9% (n = 3). This method was applicable to field surveys of phosphine in workplaces. The other method with the mercury(II) chloride adsorbent followed by the NIOSH method resulted in lower recovery of phosphate in low phosphine concentration range. ICP-AES was less sensitive than the colorimetries. The effect of coexistent arsenite or silicate on the colorimetry of phosphate was assessed.
建立了一种采用吸附采样后比色测定来测定磷化氢的方法。本研究中使用的两种吸附剂是通过用高锰酸钾（1%重量/重量）或（氯化汞和氯化钠）（0.2 + 0.2%重量/重量）浸渍硅胶制备的。每个装在玻璃管中的吸附剂（150毫克）能够在以300毫升/分钟的流速通过的3升测试气体中吸附0.3 ppm的磷化氢而不会出现穿透。吸附的磷化氢以磷酸盐的形式解吸到溶液中，回收的磷酸盐通过电感耦合等离子体发射光谱法（ICP - AES）或基于钼蓝法的两种磷酸盐比色法之一进行测定，即遵循JIS K 0102的比色法和遵循美国国家职业安全与健康研究所（NIOSH）分析方法手册第S 332号的比色法。当3升测试气体中0.01 ppm的磷化氢吸附在高锰酸钾吸附剂上并通过JIS方法测定时，93.8%的磷化氢作为磷酸盐被回收，变异系数为12.9%（n = 3）。该方法适用于工作场所磷化氢的现场调查。另一种使用氯化汞吸附剂并采用NIOSH方法的方法在低磷化氢浓度范围内导致磷酸盐的回收率较低。ICP - AES的灵敏度低于比色法。评估了共存的亚砷酸盐或硅酸盐对磷酸盐比色法的影响。
