Abstract
The present work is aimed to evaluate the conditions of the hydride generation (HG) for germanium analysis by inductively coupled plasma (ICP)-atomic emission spectrometry (AES). Twelve different kinds of acids were used such as phosphoric, hydrochloric, nitric, sulfuric, perchloric, boric, tartaric, malic, oxalic, tannic, citric, and acetic acid. It was found that phosphoric acid yielded the maximum efficiency of hydride generation. Also, efficient hydride generation was obtined with the buffer solutions containing phosphate ions over a wide range of pH. In addition, in the presence of phosphoric acid the interference caused by metals was suppressed in the hydride generation of germanium. As the concentrations of a reducing agent and a stabilizing increased the hydride generation efficiency and the acid concentration proviaing the maximum intensity were increased. By using an analytical method developed in this study, the contents of germanium in water and rock samples were determined. The detection limit of germanium in the presence of phosphoric acid was $0.03{\mu}g/L$.
수소화물생성법-유도결합플라스마-원자방출분광법으로 게르마늄을 분석할 때 보조산으로 phosphoric acid의 사용은 nitric acid, hydrochloric acid, sulfuric acid, perchloric acid, boric acid, tartaric acid, malic acid, oxalic acid, acetic acid, tannic acid, citric acid의 사용보다 높은 수소화물 생성효율을 보였고, 같은 pH영역이라도 phosphate ion이 존재하는 buffer의 사용이 더 높은 생성효율을 보였다. 또한, 2.5M phosphoric acid를 이용한 결과, 시료용액 내에 잔류하는 산이나 공존원소의 영향이 감소하였다. 환원제와 안정제의 농도가 증가할수록 수소화물 생성효율은 증가되었으며, 최대방출세기를 나타내는 산의 세기는 높은 쪽으로 이동했고 농도영역은 넓어졌다. 인산 존재 하에서의 게르마늄의 검출한계는 $0.03{\mu}g/L$이었다.
