岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2014年
3期
312-320
,共9页
地球化学勘查样品%稀土矿%铌%钽%恒温电热板消解%碱熔%电感耦合等离子体质谱法%电感耦合等离子体发射光谱法
地毬化學勘查樣品%稀土礦%鈮%鐽%恆溫電熱闆消解%堿鎔%電感耦閤等離子體質譜法%電感耦閤等離子體髮射光譜法
지구화학감사양품%희토광%니%단%항온전열판소해%감용%전감우합등리자체질보법%전감우합등리자체발사광보법
geochemical exploration samples%rare earth ores%Nb%Ta%constant temperature-electric heating plate digestion%Na2 O2 fusion%Inductively Coupled Plasma-Mass Spectrometry%Inductively Coupled Plasma-Atomic Emission Spectrometry
针对目前铌钽分析中出现的样品溶解不完全、元素易水解及现有分析技术流程复杂的情况，本文对常用的混合酸恒温电热板溶解和过氧化钠碱熔两种样品前处理方式进行优化，运用电感耦合等离子体质谱法（ ICP-MS）、电感耦合等离子体发射光谱法（ ICP-AES）两种技术手段，建立了测定地球化学勘查样品及稀土矿石中不同含量水平的铌、钽两套分析方法。对于铌、钽含量较低且易于分解的样品，采用硝酸-氢氟酸-硫酸混合酸恒温电热板消解ICP-MS方法测定；对于铌、钽含量高且难溶的样品，采用过氧化钠高温熔融ICP-AES方法测定。ICP-MS用于分析低含量样品更具优势，而高含量样品更适合运用ICP-AES。通过分析土壤、水系沉积物、岩石、稀有稀土矿石系列国家标准物质，结果表明混合酸处理ICP-MS分析方法的线性范围为0~200 ng/mL；检出限为铌0.01μg/g，钽0.05μg/g；相对误差小于10%，精密度（ RSD）小于6%；碱熔处理ICP-AES分析方法的线性范围为0~30μg/mL，检出限为铌0.2μg/g，钽2.5μg/g，相对误差小于10%，精密度（ RSD）小于7%。这两套分析方法可以满足基体复杂、铌钽含量变化范围大、试样批量大的检测要求。
針對目前鈮鐽分析中齣現的樣品溶解不完全、元素易水解及現有分析技術流程複雜的情況，本文對常用的混閤痠恆溫電熱闆溶解和過氧化鈉堿鎔兩種樣品前處理方式進行優化，運用電感耦閤等離子體質譜法（ ICP-MS）、電感耦閤等離子體髮射光譜法（ ICP-AES）兩種技術手段，建立瞭測定地毬化學勘查樣品及稀土礦石中不同含量水平的鈮、鐽兩套分析方法。對于鈮、鐽含量較低且易于分解的樣品，採用硝痠-氫氟痠-硫痠混閤痠恆溫電熱闆消解ICP-MS方法測定；對于鈮、鐽含量高且難溶的樣品，採用過氧化鈉高溫鎔融ICP-AES方法測定。ICP-MS用于分析低含量樣品更具優勢，而高含量樣品更適閤運用ICP-AES。通過分析土壤、水繫沉積物、巖石、稀有稀土礦石繫列國傢標準物質，結果錶明混閤痠處理ICP-MS分析方法的線性範圍為0~200 ng/mL；檢齣限為鈮0.01μg/g，鐽0.05μg/g；相對誤差小于10%，精密度（ RSD）小于6%；堿鎔處理ICP-AES分析方法的線性範圍為0~30μg/mL，檢齣限為鈮0.2μg/g，鐽2.5μg/g，相對誤差小于10%，精密度（ RSD）小于7%。這兩套分析方法可以滿足基體複雜、鈮鐽含量變化範圍大、試樣批量大的檢測要求。
침대목전니단분석중출현적양품용해불완전、원소역수해급현유분석기술류정복잡적정황，본문대상용적혼합산항온전열판용해화과양화납감용량충양품전처리방식진행우화，운용전감우합등리자체질보법（ ICP-MS）、전감우합등리자체발사광보법（ ICP-AES）량충기술수단，건립료측정지구화학감사양품급희토광석중불동함량수평적니、단량투분석방법。대우니、단함량교저차역우분해적양품，채용초산-경불산-류산혼합산항온전열판소해ICP-MS방법측정；대우니、단함량고차난용적양품，채용과양화납고온용융ICP-AES방법측정。ICP-MS용우분석저함량양품경구우세，이고함량양품경괄합운용ICP-AES。통과분석토양、수계침적물、암석、희유희토광석계렬국가표준물질，결과표명혼합산처리ICP-MS분석방법적선성범위위0~200 ng/mL；검출한위니0.01μg/g，단0.05μg/g；상대오차소우10%，정밀도（ RSD）소우6%；감용처리ICP-AES분석방법적선성범위위0~30μg/mL，검출한위니0.2μg/g，단2.5μg/g，상대오차소우10%，정밀도（ RSD）소우7%。저량투분석방법가이만족기체복잡、니단함량변화범위대、시양비량대적검측요구。
A method to deal with the conditions of incomplete digestion of geological samples,and the complexity of the analysis for present technologies,along with the routine methods of wet digestion on constant temperature electric heating plate with mixed acids and Na2 O2 fusion pre-treatment method and to ease the hydrolysis of Nb and Ta are describe in this paper. Both Inductively Coupled Plasma-Mass Spectrometry( ICP-MS ) and Inductively Coupled Plasma-Atomic Emission Spectrometry( ICP-AES)were applied to establish two sets of analysis methods which can be used to detect the contents of Nb and Ta in geochemical exploration samples and rare earth ores. Wet digestion on constant temperature electric heating plate is suitable for low content and easy decomposition of samples with nitric acid-hydrofluoric acid-sulfuric acid by ICP-MS. Na2 O2 fusion pre-treatment method is suitable for high content and insoluble samples by using ICP-AES. Through the analysis of a series of national certified reference samples of soil,stream sediments,rocks and rare earth ores,the results show that mixed acid pre-treatment coupled with ICP-MS had a linear range of 0-200 ng/mL and detection limits of Nb and Ta were 0 . 01 μg/g and 0. 05 μg/g,respectively. The relative error was less than 10%,and the relative standard deviation( RSD)was less than 6%. The Na2 O2 fusion pre-treatment coupled with ICP-AES had a linear range of 0 -30 μg/mL, detection limits of Nb and Ta were 0. 2 μg/g and 2. 5 μg/g,respectively. The relative error was less than 10%, and the precision( RSD)was less than 7%. The two sets of analysis method satisfy the demand of analysis of Nb and Ta in samples with a complex matrix,a large range of content and large quantities of samples.
