Determination of Arsenic and Antimony in Eighty-Five Geochemical Reference Samples by Automated Hydride Generation and Electrothermal Atomic Absorption Spectrometry

The arsenic and antimony contents of 85 geochemical reference samples have been determined by atomic absorption spectrometry with hydride generation and heated quartz cell atomizer. The sample is decomposed with a mixture of perchloric, nitric and hydrofluoric acids and potassium permanganate solution; interferences are eliminated by addition of potassium iodide, aluminium chloride and ascorbic acid. The agreement between the present results and published data is fairly good.     

Determination of Selenium in Fifty Two Geochemical Reference Materials by Hydride Generation Atomic Absorption Spectrometry

The selenium content of fifty two geochemical reference samples, issued by several reference material producers (ANRT, GIT-IWG, USGS, NIST and GSJ) has been determined by continuous hydride generation and atomic absorption spectrometry. Selenium(VI) in the digested solutions was pre-reduced to selenium(IV) by heating in 6 mol l⁻¹ HCl solution. The limit of detection was 3 ng g⁻¹ selenium in common geological samples. Some samples which contain a large amount of heavy metals were analysed by the standard addition technique. The agreement between the reported results and published data is satisfactory.     

Determination of Selenium in Thirty-Two Geochemical Reference Materials by Continuous - Flow Hydride Generation Atomic Absorption Spectrophotometry

A continuous-flow hydride atomic absorption spectrophotometric method has been applied to 32 geochemical reference materials for the determination of selenium. The sample is decomposed with a mixture of nitric, perchloric and hydrofluoric acids. Selenium values obtained in this study are in general agreement with literature values and provide additional certification for these reference materials. The precision of the method is generally better than 5% relative standard deviation. The lower limit of determination of selenium in the sample is 12 ppb.     

氢化物发生-双道原子荧光光谱法测定化探样品中砷锑铋

介绍了氢化物发生-双道原子荧光光谱法测定地质化探样品中砷、锑、铋的分析方法。通过一系列方法实验及讨论,确立了较合理的测试条件,准确度及检出限大大改进;通过加入硫脲、抗坏血酸固体粉末,一定程度上减小了稀释倍数,提高了灵敏度;通过实验,砷、锑、铋的负高压/灯电流分别选取280 V/40 mA、280 V/60 mA、280 V/60 mA。方法操作快速、高效、准确,并大大降低了分析成本。     

Analysis of Geochemical Reference Materials Using Simultaneous Multi-Element Atomic Absorption Spectrometry

Analytical data are presented for the determination of Ag, Bi, Cd, Co, Cu, Mn, Ni, Pb, Zn in 60 geochemical reference samples by simultaneous multi-element atomic absorption spectrometry with flame atomization. The samples include rocks, sediments, coal ash, Mn nodules and ores. Accuracy and precision of the analysis are evaluated statistically.     

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.     

氢化物发生原子荧光光谱法测定土壤中络合态锑

采用酒石酸作提取剂，氢化物发生原子荧光光谱法测定土壤中络合态Sb(Ⅲ）和Sb(Ⅴ）。研究了氢化物发生原子荧光光谱测定土壤中络合态Sb(Ⅲ）和Sb(Ⅴ）的浸提和还原条件及对测定结果的影响。Sb(Ⅲ）和总Sb检出限分别为0.11μg/L和0.09μg/L。相对标准偏差（RSD，n=11)分别为5.4%和6.1%，加标回收率在82.5%-101.9%。     

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.     

碱性体系在线氢化物发生原子荧光光谱法测定铜矿石中痕量砷锑铋

建立了一个碱性体系在线氢化物发生原子荧光光谱法测定铜矿石中痕量砷、锑、铋的分析方法。设计了在线氢化物发生流路及操作程序。选择了碱性体系氢化物发生的各项最佳条件,避免了Ｃｕ、Ｆｅ等大量基体元素的干扰。方法检出限为Ａｓ０．６μｇ／Ｌ,Ｓｂ０．４μｇ／Ｌ,Ｂｉ０．９μｇ／Ｌ,Ａｓ、Ｓｂ、Ｂｉ的工作曲线均在０～４００μｇ／Ｌ内呈良好的线性,经铜矿石国家一级标准物质分析验证,砷锑铋的测定结果与标准值吻合,相对标准偏差（ＲＳＤ,ｎ＝５）在４．２％～８．８％。     

氢化物—原子荧光法测定大洋沉积物中的砷

试验了常用酸及还原剂用量对测定Ａｓ的影响,选择了仪器的最佳工作条件,考察了大洋沉积物中主量及常见元素对测定的干扰情况,并给出了这些元素不干扰测定的允许存在量。方法用于测定海底沉积物标准样品,结果与标准值吻合,相对标准偏差（ｎ＝１２）小于５％。     

Determination of Silver in Seventy-Three Geochemical Reference Samples by Atomic Absorption Spectrometry

The silver content of seventy-three geochemical reference samples has been determined by atomic absorption spectrometry using an air-acetylene flame or a graphite furnace atomizer, after extraction of silver as iodide with methyl isobutyl ketone (MIBK). A comparison with published data shows clearly the need for much more data on most reference samples.     

Determination of Bismuth in Eighty-Three Geochemical Reference Samples by Atomic Absorption Spectrometry

The bismuth content of eighty-three geochemical reference samples has been determined by atomic absorption spectrometry using either a hydride generation and heated quartz cell atomizer or a solvent extraction and carbon tube atomizer. The agreement between the present results and published data is generally good.     

Determination of Thallium in Eighty-Seven Geochemical Reference Samples by Atomic Absorption Spectrometry

The thallium content of eighty-seven geochemical reference samples has been determined by atomic absorption spectrometry using an air-acetylene flame or a graphite furnace atomizer, after extraction of thallium as chloride with methylisobutylketone (MIBK). A comparison with published data show clearly the need for much more data on most reference samples.     

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     

Determination of Gold in Twenty Geochemical Reference Samples by Flameless Atomic Absorption Spectrometry

After acid digestion, gold is extracted with MIBK and determinated by flameless atomic absorption spectrometry. The results for six USGS reference samples and fourteen French geochemical standards are presented and discussed. The agreement with working values for these standards is in the range of pm 5%.     

Determination of Gold in Sixty Geochemical Reference Samples by Flameless Atomic Absorption Spectrometry

The gold content of sixty geochemical reference samples has been determined by atomic absorption spectrometry using a graphite furnace atomizer after digestion of sample with aqua regia and extraction of gold as chloride by methylisobutylketone. A comparison with published data shows clearly the need for much more data on most samples before consensus values could be assigned.
La teneur en or dans soixante échantillons géochimiques de référence a été déterminée par le spectromètre d'absorption atomique équipé d'un four à graphite. L'échantillon a été mis en solution avec de l'eau régale et l'or extrait avec du methylisobutylketone. Un examen des données publiées sur l'or montre qu'il faut davantage de résultats pour fixer des valeurs de consensus dans la plupart des échantillons.     

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.     

Determination of Selenium in Geochemical Reference Samples Using Flameless Atomic Absorption Spectrometry

Sixteen international and six inter-laboratory geochemical reference samples have been analysed for their selenium content. No previous Sedata are available for thirteen of them. Selenium has been separated from silicate matrix by volatilization and was determined with flameless atomic absorption spectrometry. An outline of the procedure is given. The limit of detection is 10 ng Se per 1 g of sample. Time required for one full analysis is 1.2 to 2.5 hours depending on amount of sample to be volatilized.     

Determination of Platinum and Palladium in Sixty-Eight Geochemical Reference Samples by Flameless Atomic Absorption Spectrometry

Platinum and palladium contents of sixty-eight geochemical reference samples have been determined by graphite furnace atomic absorption spectrometry after digestion of sample with aqua regia and hydrofluoric acid and extraction of platinum and palladium as iodides by methylisobutylketone (MIBK). The data are compared with those from other studies and crustal abundances.     

Accurate Determination of Nickel in South African Primary and Secondary Geochemical Reference Materials by Cation Exchange Chromatography and Atomic Absorption Spectrometry

Nickel in the six SA primary (NIMROCS) and fourteen secondary reference materials as well as in a phosphate rock has been determined accurately by means of atomic absorption spectrometry. A selective and quantitative twocolumn ion exchange separation procedure, using AG50W-X4 cation exchange resin, is employed for the separation of nickel from all other elements. The accuracy and precision of the described method are demonstrated by the analysis of synthetic rock solutions containing various amounts of nickel.