Determination of lead content in the plastic by ICP and AAS using HI reduction - PbSO4 dissolution method

HI 환원-PbSO4용해법을 이용한 ICP와 AAS에 의한 플라스틱 중의 납 정량 방법

  • Lee, Hyun-Ja (Materials & Components Standards Division Agency for Technology and Standards) ;
  • Kim, Sang-Kyung (Materials & Components Standards Division Agency for Technology and Standards) ;
  • Lee, Se-Jin (Materials & Components Standards Division Agency for Technology and Standards) ;
  • Lee, Hyun-A (Materials & Components Standards Division Agency for Technology and Standards)
  • 이현자 (산업자원부 기술표준원 기간산업기술표준부 소재부품과) ;
  • 김상경 (산업자원부 기술표준원 기간산업기술표준부 소재부품과) ;
  • 이세진 (산업자원부 기술표준원 기간산업기술표준부 소재부품과) ;
  • 이현아 (산업자원부 기술표준원 기간산업기술표준부 소재부품과)
  • Received : 2004.03.25
  • Accepted : 2004.08.09
  • Published : 2004.10.25

Abstract

Plastic was decomposed with nitric acid after being carbonized by sulfuric acid. Then excess sulfuric acid and nitric acid was removed by evaporating and drying. Precipitated $SO{_4}^{-2}$ ion of $PbSO_4$ was resolved itself into $H_2S$ by HI in hydrochloric acid and was volatilized. Then $Pb^{+2}$ was dissolved and was measured by AAS and ICP. The test for reproducibility using PVC-Pb standard material (690-34610mg/kg) was conducted and the accuracy was more than 99.9% compared with the estimated concentration. The precision by AAS was 99.8% and that of ICP was 99.9%.

플라스틱을 황산으로 탄화시키고 질산으로 산화 분해한 후 과잉의 황산과 질산을 증발 건조에 의해 제거한다. 이때 침전된 납화합물 ($PbSO_4$)의 $SO{_4}^{-2}$ 이온을 염산산성에서 HI에 의해 $H_2S$로 환원하여 휘발시킨 다음 납을 용해한후 AAS와 ICP로 측정하였다. PVC-Pb 표준시료 (690~34610mg/kg)를 이용하여 재현성 실험을 하였으며 예상농도에 대비하여 99.9% 이상의 정확성을 보였다. 정밀성은 AAS는 99.8%, ICP는 99.9%로 비슷하였다.

Keywords

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