Ono-Ogasawara M, Furuse M, Matsumura Y, Yokota K, Naito K
National Institute of Industrial Health, Kawasaki, Japan.
Ind Health. 1992;30(1):35-45. doi: 10.2486/indhealth.30.35.
A method for determining atmospheric diborane in concentrations higher than 1/10 of TLV, i.e., 0.01 ppm, has been developed using the adsorption sampling method. Silica gel impregnated with potassium permanganate, synthetic resin activated carbon impregnated with or without mercury(II) chloride and activated carbon impregnated with chromate salt showed adsorption capacities larger than 18 l of 3 ppm diborane test gas when the test gas was drawn at 300 ml/min. Complete desorption of the adsorbed diborane was possible only from silica gel impregnated with potassium permanganate into a hydroxylamine hydrochloride solution. As methods for determining the desorbed boron, both the chromotropic acid-HPLC method and ICP-AES were applied. The former was more sensitive, but the latter was less influenced by coexistent substances. The most sensitive and reproducible procedure for diborane determination was as follows: diborane is collected with silica gel impregnated with potassium permanganate (0.05% (w/w)) and desorbed into hydroxylamine hydrochloride solution (400 micrograms/ml) followed by the determination of boron by the chromotropic acid-HPLC method. When diborane in 3 l of 0.1 ppm test gas was collected, the desorption efficiency was 105.3% with an RSD of 13.5%. The limit of quantitation of this method was 0.0026 ppm in 3 l air. Much lower concentrations can be determined by sampling larger amounts of air.
已开发出一种使用吸附采样法测定大气中浓度高于阈限值（TLV）十分之一（即0.01 ppm）的乙硼烷的方法。当以300 ml/min的流速抽取测试气体时，浸渍有高锰酸钾的硅胶、浸渍或未浸渍氯化汞（II）的合成树脂活性炭以及浸渍有铬酸盐的活性炭对3 ppm乙硼烷测试气体的吸附容量均大于18 l。仅从浸渍有高锰酸钾的硅胶中能将吸附的乙硼烷完全解吸至盐酸羟胺溶液中。作为测定解吸硼的方法，采用了变色酸-HPLC法和ICP-AES法。前者更灵敏，但后者受共存物质的影响较小。测定乙硼烷最灵敏且可重复的步骤如下：用浸渍有高锰酸钾（0.05%（w/w））的硅胶收集乙硼烷，并解吸至盐酸羟胺溶液（400微克/毫升）中，然后用变色酸-HPLC法测定硼。当收集3 l 0.1 ppm测试气体中的乙硼烷时，解吸效率为105.3%，相对标准偏差为13.5%。该方法在3 l空气中的定量限为0.0026 ppm。通过采集更多量的空气可测定更低的浓度。
