岩矿测试
巖礦測試
암광측시
Rock and Mineral Analysis
2015年
5期
533-538
,共6页
土壤%水系沉积物%砷锑铋%氢化物发生%电感耦合等离子体发射光谱法
土壤%水繫沉積物%砷銻鉍%氫化物髮生%電感耦閤等離子體髮射光譜法
토양%수계침적물%신제필%경화물발생%전감우합등리자체발사광보법
soil%stream sediment%As-Sb-Bi%Hydride Generation%Inductively Coupled Plasma-Optical Emission Spectrometry
氢化物发生法-电感耦合等离子体发射光谱（ ICP-OES）联用可以提高仪器测定的灵敏度，但氢化物发生的化学反应过程不稳定，导致检测精密度变差。本文设计了一套简易氢化物发生系统，将样品进样管内径由0.32 mm扩大为0.76 mm，与还原剂（硼氢化钾）管路通过三通混合，混合后反应管内径由0.76 mm扩大为1.14 mm，反应管长度由30 cm延长至50 cm，显著增加了待测元素氢化反应的空间和时间，使氢化反应达到平衡态从而提高了氢化物的稳定性。土壤和水系沉积物样品用盐酸-硝酸水浴浸提、硫脲-抗坏血酸预还原后利用此套系统与ICP-OES联用测定了砷锑铋的含量。砷锑铋的检出限分别为0.35μg/g、0.33μg/g、0.25μg/g，测定范围分别为1.1~300μg/g、1.0~100μg/g、0.75~100μg/g，均满足了相关分析要求。
氫化物髮生法-電感耦閤等離子體髮射光譜（ ICP-OES）聯用可以提高儀器測定的靈敏度，但氫化物髮生的化學反應過程不穩定，導緻檢測精密度變差。本文設計瞭一套簡易氫化物髮生繫統，將樣品進樣管內徑由0.32 mm擴大為0.76 mm，與還原劑（硼氫化鉀）管路通過三通混閤，混閤後反應管內徑由0.76 mm擴大為1.14 mm，反應管長度由30 cm延長至50 cm，顯著增加瞭待測元素氫化反應的空間和時間，使氫化反應達到平衡態從而提高瞭氫化物的穩定性。土壤和水繫沉積物樣品用鹽痠-硝痠水浴浸提、硫脲-抗壞血痠預還原後利用此套繫統與ICP-OES聯用測定瞭砷銻鉍的含量。砷銻鉍的檢齣限分彆為0.35μg/g、0.33μg/g、0.25μg/g，測定範圍分彆為1.1~300μg/g、1.0~100μg/g、0.75~100μg/g，均滿足瞭相關分析要求。
경화물발생법-전감우합등리자체발사광보（ ICP-OES）련용가이제고의기측정적령민도，단경화물발생적화학반응과정불은정，도치검측정밀도변차。본문설계료일투간역경화물발생계통，장양품진양관내경유0.32 mm확대위0.76 mm，여환원제（붕경화갑）관로통과삼통혼합，혼합후반응관내경유0.76 mm확대위1.14 mm，반응관장도유30 cm연장지50 cm，현저증가료대측원소경화반응적공간화시간，사경화반응체도평형태종이제고료경화물적은정성。토양화수계침적물양품용염산-초산수욕침제、류뇨-항배혈산예환원후이용차투계통여ICP-OES련용측정료신제필적함량。신제필적검출한분별위0.35μg/g、0.33μg/g、0.25μg/g，측정범위분별위1.1~300μg/g、1.0~100μg/g、0.75~100μg/g，균만족료상관분석요구。
Hydride Generation( HG)combined with Inductively Coupled Plasma-Optical Emission Spectrometry ( ICP-OES ) has excellent analytical sensitivity. However,the instable chemical reactions of HG may cause unsatisfactory analytical precision. In this study,a novel and self-made HG system coupled with ICP-OES was developed for measurement of As,Sb and Bi in geological samples. Inner diameter( i. d. )of introduction tube changed from 0. 32 mm to 0. 76 mm. Inner diameter(i. d. )of reaction tube changed from 0. 76 mm to 1. 14 mm and length increased from 30 cm to 50 cm. These changes significantly improve the stability of HG reaction by increasing space and time of chemical reactions to reach reaction equilibrium. Arsenic,Sb and Bi were firstly leached from soil and stream sediment using HCl-HNO3 water bath,pre-reduced by thiocarbamide-ascorbic acid mixture,and were finally determined by the modified HG-ICP-OES. The detection limits of this method are 0. 35μg/g,0. 33 μg/g and 0. 25 μg/g for As,Sb and Bi,respectively. The linear ranges are 1. 1-300 μg/g for As, 1. 0-100 μg/g for Sb and 0. 75-100 μg/g for Bi,which is sufficient for the measurement of As,Sb and Bi in geological samples.
