Determination of Selenium in Twenty-Eight Geological Reference Materials by Atomic Absorption Spectrometry

Twenty-eight geological reference samples have been analysed for selenium using atomic absorption spectrometry with hydride generation and quartz cell atomizer and/or with solvent extraction and carbon tube atomizer. Data are presented for 5 CCRMP, 6 USGS, 3 NBS, 6 NIM and 8 GSJ reference materials.     

地质样品中超痕量铂族元素的中子活化分析

文章概述了中子活化分析的基本原理和地质样品中超痕量铂族元素的中子活化分析方法。其中除介绍了样品的制备方法、照射和测量条件之外，还对地质样品中铂族元素放射化学分离方法进行了说细的讨论和评述。引用文献２４篇。     

悬浮液原子荧光光谱法测定化探样品中的痕量汞

拟定了将悬浮液技术与汞蒸气原子荧光光谱法相结合测定化探样品中痕量Ｈｇ的分析方法。控制悬浮液中试样粒度在２００目,试样质量浓度１５ｇ／Ｌ,用电磁搅拌和载气搅拌保证悬浮液分散稳定,水溶液标准作校正曲线,方法的检出限为６ｎｇ／ｇＨｇ。对水系沉积物国家标准物质中痕量Ｈｇ进行测定,结果与标准值相符,对含Ｈｇ０１０μｇ／ｇ的ＧＢＷ０７３０５（ＧＳＤ ５）测定１１次,ｘ为０１０５μｇ／ｇ,ＲＳＤ为５４％。     

Determination of Beryllium in Eighty Geological Reference Samples by Atomic Absorption Spectrometry

The beryllium content of eighty geological reference samples has been determined by atomic absorption spectrometry using a nitrous oxide-acetylene flame or a carbon tube atomizer, after extraction of beryllium as acetylacetonate with methylisobutylketone (MIBK). The agreement between the present results and published data is generally good.     

双通道-原子荧光光谱和固体进样-冷原子吸收光谱测定岩石中痕量汞

岩石中的痕量汞检测往往因内部晶胞结构复杂,使得热水浴酸解提取不彻底、挥发损失以及接触污染等引起结果偏差和不稳定.本文在前人研究的基础上,采用中国研制的双通道-原子荧光光谱仪和固体进样-冷原子吸收光谱仪分析岩石中的痕量汞,以探索最佳检测方案.双通道-原子荧光光谱分析中,优化的实验条件为:以80％王水溶液对样品沸水浴提取5...     

Fractional Determination of Gold in Twenty Six Geological Reference Materials by Sequential Extraction with Graphite Furnace Atomic Absorption Spectrometry

A method is described to estimate the chemical form of gold (Au) in a variety of geological reference samples, combining a sequential extraction scheme with graphite furnace atomic absorption spectrometry, after extraction of Au as iodide or chloride with methyl isobutyl ketone. The fractions dissolved by sequential extraction are empirically defined as the exchangeable, amorphous, metallic, aqua regia-soluble and residual fractions. The amounts of Au in the amorphous fraction have been derived mainly from oxide or amorphous phases, and the chemical forms of Au are considered to be mostly amorphous and partly metallic. The metallic fraction of Au is likely to exist as submicroscopic grains of native metal which are relatively free from the rock-forming minerals, whereas the aqua regia-soluble or residual fraction of Au may be bound more intimately perhaps as inclusions or solid solutions of either native metal or electrum in most cases. Satisfactory agreement was observed between the sum of the Au values from exchangeable to residual fractions and the reported total Au values, except for a few samples which contained a large amount of reducing materials. Analytical results of Au for twenty six geological reference materials are tabulated, and geochemical and mineralogical features are discussed.     

掺氧空气—乙炔火焰原子吸收光谱法测定地质样品中微量钡

提出掺氧空气－乙炔火焰原子吸收光谱法测定地质样品中微量钡的新方法。使用磺基水杨酸作保护剂消除铝对钡的挥发原子化干扰，KCl作消电离剂消除钡的电离干扰。方法的检出限（K＝3）为0.04mg/L。方法已应用于测定地质标准样品中的微量钡，结果与标准值相符，对GBW07103试样测定6次，RSD为5.4%。     

流动注射-火焰原子吸收光谱法测定地质样品中的常量金

样品经室温烧至650℃高温后灼烧保持1.5 h,用浓王水溶解。用泡塑分两次吸附富集样品中的常量金,将富集同一样品中金的两块泡塑置于盛有10 mL 10 g/L硫脲溶液的玻璃试管中,沸水浴保持20 min,使金释放出来,所得溶液应用原子吸收分光光度计采用流动注射测定。对仪器的测定条件进行了优化比较。方法检出限(3σ)为0.022μg/g,精密度(RSD,n=11)小于8.0%,测定范围为0.05～60μg/g。经国家金矿石分析标准物质验证,其测定值与标准值基本一致。     

Determination of Indium and Tellurium in Fifty Nine Geological Reference Materials by Solvent Extraction and Graphite Furnace Atomic Absorption Spectrometry

The indium (In) and tellurium (Te) contents of fifty nine geological reference materials, issued by several reference material producers (USGS, CRPG, ANRT, GIT-IWG and GSJ) have been determined by graphite furnace atomic absorption spectrometry, after aqua regia and HF digestion, and extraction of iodide complexes with trioctylmethylammonium (TOMA) - metyl isobutyl ketone (MIBK). Although the interferences from most elements can be minimised by the addition of palladium solution as the matrix modifier, large concentrations of Bi, Cu, Pb or Sn suppress the absorbance of In and/or Te. Samples for analysis were therefore restricted to those in which the concentrations of these interfering elements did not cause a significant interference. The limit of detection was 0.2 ng g⁻¹ In and Te for 1 g test portions. The agreement between the reported results and published data is satisfactory.     

微型氢化物发生装置在冷原子吸收分光光度法测汞中的应用

采用微型氢化物发生装置-冷原子吸收分光光度法测定了焊锡料及纽扣电池中的汞.在酸性介质中,用硼氢化钾将汞离子还原为汞原子,用载气将汞蒸气导入石英管,原子吸收分光光度计在波长253.7 nm处进行测定.选择了实验条件,对共存离子的干扰等进行了考察.方法的检出限为0.34 ng/mL,11次测定的相对标准偏差(RSD)小于6%,加标回收率为94.4%～104.7%.     

氢化物－原子荧光光谱法直接测定地质物料中痕量锗

采用特种空心阴极灯作激发光源和具有氩氢火焰低温自动点燃装置的原子荧光仪，氢化法直接测定地质物料中痕量锗，方法的测定下限为０．０２μｇ／ｇ，线性范围１～４００μｇ／Ｌ，精密度（ＲＳＤ，ｎ＝１１，１１６μｇ／ｇＧｅ）为１．７９％，加标回收率９７．８％。经标样和大批量样品分析验证，方法可靠实用     

三乙醇胺增敏火焰原子吸收光谱法测定地质样品中的钼

样品经王水分解,加入适量的三乙醇胺增敏,用空气-乙炔火焰原子吸收光谱法测定地质样品中的钼。选择了三乙醇胺的最佳用量;比较了钼在盐酸-磷酸-铝盐、盐酸-三乙醇胺、盐酸-三乙醇胺-磷酸、盐酸-三乙醇胺-磷酸-铝盐等4种不同介质中的特征浓度。结果表明,在盐酸-三乙醇胺-磷酸-铝盐介质中,钼的质量浓度≤40 mg/L内线性良好,方法检出限为0.2 mg/L,相对标准偏差为5.2%(n=6),加标回收率为96%~102%。对国家一级标准物质进行测定,结果与标准值相符。     

富氧空气-乙炔火焰原子吸收光谱法测定地质样品中的钒

利用测试液中当铝离子浓度超过钒离子浓度两倍以上，铝对钒的吸收信号增感基本恒定，且能较好地克服其它元素的化学干扰，建立了富氧空气-乙炔火焰原子吸收光谱法测定地质样品中痕量钒的方法。方法的检出限LD为0．33mg／L。应用于国家一级地质标准物质中痕量钒的测定，结果与标准值相符。对GBW 07303水系沉积物样品测定6次，ω^-(V)=119．0μg/g，RSD为4．5％。     

Determination of Cadmium and Lead in Seventy-seven Geological Reference Samples by Atomic Absorption Spectrometry

The cadmium and lead contents of seventy-seven geological reference samples have been determined by atomic absorption spectrometry using an air-acetylene flame or a carbon tube atomizer, after extraction of cadmium and lead as iodides with methylisobutylketone (MIBK). The agreement between the present results and published data is generally good.     

化学蒸气发生-无色散原子荧光光谱法测定地质样品中微量和痕量金

试样用王水分解,采用特定的金化学发生增敏试剂使金在硼氢化物-酸体系中产生挥发物质,将其导入原子荧光光谱检测系统,检测金的原子荧光信号。通过对仪器工作参数和化学蒸气发生参数的优化,使金的可检测信号同比提高20倍以上,同时降低共存离子对金的化学蒸气发生的干扰。对微量和痕量金的测定方法具有灵敏度高、检出限低、基体干扰少等优点。方法检出限为0.23 ng/g,准确度(ΔlgC,n=12)为-0.004~0.02,精密度(RSD,n=12)为2.62%~8.79%。经国家一级标准物质分析验证,测定值与标准值相符。     

Determination of Molybdenum in Fifty Three Geochemical Reference Materials by Flameless Atomic Absorption Spectrometry

The molybdenum (Mo) contents of fifty three geochemical reference materials issued by ANRT, GIT-IWG, NIST and GSJ, have been determined by atomic absorption spectrometry, using a graphite furnace atomiser, after extraction of Mo dithiol with isoamyl acetate. Detection limits for this method (0.01 μg g⁻¹) are ten times smaller than for most classical methods. The agreement between the present results and published data is satisfactory.     

石墨炉原子吸收法测定地质样品中痕量银

本文介绍了采用硝酸、氢氟酸、高氯酸溶解试样，在５％的盐酸介质中，不经分离，直接测定地质样品中痕量银。银的检出限为５ｎｇ／ｇ，方法灵敏度２．０×１０－１２，相对标准偏差为４％，回收率９５％－１１５％。     

流动注射在线萃取-火焰原子吸收光谱法测定地质试样中痕量银

研究了在线萃取系统流程中最佳参数,提出一个流动注射在线萃取-火焰原子吸收光谱法测定地质试样中痕量Ag的分析方法。检出限为0.54ng/ml,对于含Ag 20ng/ml试样测定10次,精密度(RSD)为1.64％,分析速度可达20～30N/h,经地质标样分析验证结果可靠。     

Flameless Atomic Absorption Determination of Gold and Palladium in Geological Reference Samples

Gold and palladium have been determined in 42 geological reference samples with graphite furnace AAS after aqua regia digestion and SnCl₂-Hg extraction. A brief discussion on the quality of these analyses also is presented.     

快速程序升温-石墨炉原子吸收光谱法测定地质样品中痕量镉

建立了快速程序升温-石墨炉原子吸收光谱测定地质样品中痕量镉的分析方法.样品用硝酸-氢氟酸-高氯酸进行前处理,为提高分析效率,改进了石墨炉升温程序,省去了常规方法中的灰化步骤,使测定镉的程序升温时间由常规的90～100 s降至24 s,工作效率显著提高.方法检出限为0.011 μg/g,加标回收率为93.5%～106.0...