Determination of Total Carbon and Sulfur in Forty-Two Geochemical Reference Samples By Combustion and Infrared Spectrometry

Total carbon and sulfur were determined on a variety of geochemical reference samples such as rocks, sediments, minerals and ores by a method of infrared absorption following combustion in a high-frequency induction furnace. The sample was burned with an accelerator of iron powder and tungsten chips, and the carbon and sulfur dioxide in the evolved gases have been determined directly by a simultaneous infrared analyzer. The agreement between present results and other data is generally good.     

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 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.     

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 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 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 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.     

Determination of Trace Amounts of Tin in Seventy-Three Geochemical Reference Samples by Atomic Absorption Spectrometry

The tin contents of 73 geochemical reference samples have been determined by atomic absorption spectrometry using an argon-hydrogen flame after extraction of tin (IV) as iodide with benzene. The agreement between the present results and published data is generally good.     

酸溶-电感耦合等离子体发射光谱法和燃烧-红外吸收法测定不同类型地球化学样品中的硫

测试地质样品中的硫含量,以电感耦合等离子体发射光谱法(ICP-OES)和燃烧-红外吸收光谱法应用最为广泛。ICP-OES法灵敏度高、稳定性好,但受样品预处理和基体干扰的影响较大;燃烧-红外吸收光谱法便捷高效,但受结晶水红外吸收干扰,分析硫含量低的样品稳定性较差。本文采用5种酸溶方式处理样品ICP-OES测定硫含量,同时采用燃烧-红外吸收光谱法测定低中高含量的硫,综合比较了两类方法的检出限、检测范围、精密度和准确度、分析效率等,明确了各方法的适用范围。实验中确定了燃烧-红外吸收光谱法最佳测试条件为：称样量0.0500g,燃烧时间25s,分析时间40s,氧气流量4.0L/min;通过标准物质验证,该方法检出限为10×10-6,检测范围为10×10-6~470000×10-6,相对标准偏差(RSD) < 6%(n=12),相对误差绝对值小于8%。实验结果表明,ICP-OES分析效率高,但是样品处理时间长,检测范围不如燃烧-红外吸收光谱法宽;燃烧-红外吸收光谱法采用固体直接进样,成本低,用高氯酸镁作为干燥剂可解决结晶水红外吸收干扰问题。总体上,ICP-OES法适用于分析硫含量低的样品或作为测试结果佐证的手段,可实现多元素联测;批量样品或基体类型复杂的样品宜采用燃烧-红外吸收光谱法测试,更加便捷。     

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 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.     

石墨炉原子吸收光谱法测定地球化学样品中微量铬

应用ZEEnit 600型石墨炉原子吸收分光光度计测定地球化学样品中微量铬.在分解样品过程中,加入高氯酸,使Cr(Ⅱ)、Cr(Ⅲ)同时被氧化为Cr(Ⅵ),避免了Cr(Ⅲ)和Cr(Ⅵ)的吸光度不同而造成的分析误差.采用最大功率升温和纵向加热石墨管技术,测定铬的原子化温度降低至2100℃,以抗坏血酸作基体改进剂,测定灵敏度...     

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.     

Determination of Cesium in Sixty - Three Geochemical Reference Samples by Flame Emission Spectrometry

The cesium contents of 63 geochemical reference samples have been determined by flame emission spectrometry using an air-acetylene flame. The agreement between the present results and published data is generally good.     

Determination of Carbonate Carbon in 41 International Geochemical Reference Samples by Coulometric Method

The carbonate-carbon (CO₂) content of forty-one geochemical reference samples has been determined by coulometric method following acid treatment of the sample for releasing CO₂. The method is superior to the conventional methods in speed, accuracy, sensitivity, specificity, and the coverage of CO₂ range. The results on NBS limestone samples agree well with the certified values. The precision of the method is 0.5 % r.s.d., and the practical detection limit is 10 ppm C.     

Determination of Fluorine and Total Water in Thirty-Three International Geochemical Reference Samples

Thirty-three reference samples from the United States Geological Survey (USGS), Centre de Recherches Pétrographiques et Géochimiques (CRPG, France), Association Rationale de la Recherche Technique (ANRT, France), National Institute for Metallurgy (NIM, South Africa), Geotechnic Institute (GI, Austria), Mineralogical Institute of Basel and Bern (Switzerland), Zentrales Geolo-gisahes Institut (ZG1, DDR) and from the For-chungeinstitut der Zementinduatrie (Düsseldorf, GDF) were analysed for their fluorine and total water content. Fluorine was determined, after pyrohydrolysis, with an ion-selective electrode. Total water was determined, after pyrolysis, by Karl-Fischer titration. Our values, five determinations on each sample, are compared with the preferred values.     

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.     

无火焰原子吸收法测定化探样中痕量银和镉

化探样中的痕量银和镉(0.0xppm)不经分离直接用无火焰原子吸收法测定银和镉是困难的。宫本益夫曾用dowex 1×8阴离子树脂分离和富集电解铜中的银;辽宁地质局中心实验室曾用717阴离子树脂分离和富集化探样中的镉,F.Bea.Barredo和c.Polo polo曾用dowex1×8阴离子树     

电感耦合等离子体发射光谱法和火焰原子吸收光谱法连续测定化探样品中12个元素

建立了地质化探样品中不同含量和检出限要求的12个元素的连续测定方法。样品经一次取样,用盐酸-氢氟酸-硝酸-高氯酸溶样,电感耦合等离子体发射光谱法测定铜、铅、锌、钴、镍、镉、锶、钡、钒、锰后,加碘化钾-甲基异丁基甲酮萃取分离,火焰原子吸收光谱法测定银、镉。银、镉的相对标准偏差(RSD,n=12)分别为6.5%、4.7%。与现行分析方法相比,建立的方法灵敏度和精密度高、准确度好,降低了生产成本,缩短了检测时间,尤其适合大量化探样品的测定。