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dowex1×8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阴离子树脂分离和宙集化探样中的镉;F.Bea.Barredo和C.Polo polo曾用dowex1×8阴离子树脂分离硅酸盐岩石中的金、银和镉后,用无火焰原子吸收法测定。本工作参考了他人的工作,结合我们的工作情况,确定了实验条件。其绝对灵敏度银为1.5×10~(-11)克,镉为1×10~(-11)克。     

新显色剂—苯重氮氨基偶氮苯测定岩矿中的痕量镉

本文研究了新显色剂苯重氮氨基偶氮苯与镉(Ⅱ)在TritonX-100存在下的显色反应。实验表明,在pH10的硼砂—氢氧化钠缓冲溶液中显色剂同镉生成红色配合物,λ_(max)为525nm,ε=1.77×10~5L·mol~(-1)·cm~(-1),镉(Ⅱ)在0—10μg/25ml范围内服从比尔定律。采用D235大孔阴离子交换树脂分离富集,能够测定岩矿试样中的痕     

断续流动在线分离富集-蒸气发生原子荧光光谱法测定复杂环境样品中痕量镉

用D201阴离子交换树脂富集样品中的痕量Cd，使Cd与共存干扰元素Cu、Ni、Pb、Zn有效分离，消除了这些元素对镉蒸气发生的干扰，从而建立了断续流动在线分离富集-蒸气发生原子荧光光谱法测定复杂环境样品中痕量Cd的分析方法。方法的检出限为3ng／L（3σ）；测定精密度（RSD）为1．9％（对1μg/L Cd，n=11）。用该方法对国家一级标准物质（土壤、水系沉积物和岩石）中的痕量镉进行了测定，结果与标准值相符。     

醋酸丁酯萃取-无火焰原子吸收法测定化探样品中痕量金

在KBr存在下,用小体积醋酸丁酯萃取金后,用无火焰原子吸收法测定化探样品中痕量金的分析方法较化学富集光谱法具灵敏度高(检出下限可达0.05×10-9)、精度好、简便快速、成本低等优点.通过批量化探样的检验,证明该方法足已满足化探样品对金的测定要求.     

森林沼泽景观区化探找金技术方法——以黑龙江北部及内蒙古东北部为例

通过对黑龙江北部及内蒙古东北部森林沼泽景观区Au在水系沉积物和土壤中富集特征的研究,认为Au在水系沉积物中的迁移搬运距离为800～1400m,主要富集在-40目的中细粒级的粉砂和淤泥中,一般含量为0.6×10-9～1.2×10-9,大于3×10-9可形成异常.Au在土壤中的迁移搬运距离为60～100m,主要富集在-40目的B层粘土物质中,一般含量为1.1×10-9～2.0×10-9,大于6×10-9可形成异常.因此该区的化探工作适合用1∶10万水系沉积物测量工作圈定成矿有望地段,用1∶5万水系沉积物或土壤测量进行查证,在较好地段进行1∶2万(200m×40m)土壤测量工作,再于有望地段加密至100m×20m,并进行工程验证.     

痕量镉的光度分析法研究——Cd（Ⅱ）-TPPS4-CTMAB-抗坏血酸体系

本提出了用卟啉TPPS4[meso-四(4-磺酸基苯)卟啉]测定痕量镉的新方法。表观摩尔吸光系数为4．62×10^5L·mool^-1·cm^-1.镉含量0～8．0μg／25ml范围内呈良好线性关系．在萃取分离主要干扰元素之后．用于测定地质样品中痕量镉，分析结果满意。     

贵州都匀牛角塘富镉锌矿床中镉的分布及赋存状态探讨

对贵州都匀牛角塘富镉锌矿的研究发现该矿床高度富集镉 ,矿石中镉含量一般为 2 2 84× 1 0 -6～ 9850× 1 0 -6,最高为 1 3 4 0 0× 1 0 -6,比地壳克拉克值 ( 0 .2× 1 0 -6)高 5～ 6个数量级 ,比工业品位高n× 1 0～n×1 0 2 倍 ,且其储量达到大型矿床的规模 ,在世界上十分罕见。镉主要以类质同象存在于闪锌矿中 ,少量镉以硫镉矿等独立矿物形式存在于矿床的氧化带 ,是风化淋滤过程中形成的镉的次生矿物。     

石墨炉原子吸收光谱法测定地质样品中的痕量铂、钯

本文提出了用717阴离子交换树脂富集铂、钯的石墨炉原子吸收光谱分析方法。对富集铂、钯的条件,共存离子的干扰情况以及在GF-2000型石墨炉中测定铂、钯的最佳条件进行了研究。样品用王水分解后,在10％的王水介质中,用717阴离子交换树脂富集铂、钯,以热的硫脲溶液解脱,在拟定的工作条件下,于石墨炉原子吸收光谱仪上进行测定,大量的共存离子不干扰测定。方法简便快速,检出限分别为Pt8.8×10~(-9)g/ml,Pd3.4×10~(-9)g/ml,方法的相对标准偏差分别为Pt7.09％Pd11.48％,适用于地质样品中铂、钯的测定,结果令人满意。     

阴离子交换色谱分离和测定微量单矿物方铅矿和闪锌矿中铜、铅、锌、银、铋、镉、锰、钴和镍等元素

微量单矿物方铅矿和闪锌矿中主体元素和痕量元素的多项分析,作者根据金属元素在阴离子交换树脂上与在盐酸、氢溴酸、硝酸、硫酸溶液之间的行为差别,试验了用阴离子交换色谱分离的条件,选用不同浓度的盐酸溶液洗提铜、钴、镍、锰、铅和银;氢溴酸溶液洗提锌;硝酸溶液洗提镉;最后用硫酸溶液洗提铋。本文所拟定的分析流程简便,试用于微量单矿物方铅矿和闪锌矿中九个元素的测定,效果较好。     

阴离子树脂-活性炭分离富集等离子体发射光谱法测定富钴锰结壳中的痕量金银铂钯

采用717阴离子树脂活性炭联合交换分离富集技术,电感耦合等离子体发射光谱法同时测定富钴锰结壳中痕量金、银、铂、钯。方法检出限四元素分别为:Au1. 3、Ag0. 4、Pd0. 6、Pt4. 8ng/g。样品加标回收率在89. 0% ~110. 3%,相对标准偏差3. 5% ~7. 8% (n=4)。方法已用于富钴锰结壳中痕量金银铂钯的测定。     

Silver, Cadmium and Lead Contents of Some Rock Reference Samples

A series of rock reference samples have been analyzed for Ag, Cd and Pb. All elements were determined from a single digest using a method involving solvent extraction and flameless atomic absorption spectrophotometry.     

Analysis of Sulfides for Gold and Associated Trace Metals by Direct Neutron Activation With a Low-Flux Reactor

A routine method for the direct determination of Au and associated trace metals in sulfides has been developed for use with a low-flux nuclear reactor (SLOWPOKE II Reactor Facility, University of Toronto). Small samples (100–200 mg) are analysed simultaneously for Au, Ag, As, Sb, Mo, Co, Se, Cd, Fe, and Zn. Sulfides containing finely divided gold can be analysed with a high degree of precision and yield results which agree closely with commercial fire assay-atomic absorption analyses for Au. Favourable comparisons with other analytical techniques (flameless atomic absorption and emission spectrometry) are also indicated for Ag, As, and Sb. Neutron activation has the advantage of providing precise and accurate results for these elements without chemical separation or preconcentration. Analyses of 10 sulfide-bearing reference materials from CANMET, Ottawa are compared with published best values for selected trace metals including Au.     

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。     

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%.     

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.     

石墨炉原子吸收光谱法测定地质样品中微量银

对石墨炉原子吸收光谱法测定地质样品中微量银进行了研究。样品经四酸溶解,在3mol/L的HCl介质中以EDTA-抗坏血酸溶液作为基体干扰改进剂,用石墨炉原子吸收光谱法测定地质样品中微量银。方法检出限为0.051ng/mL,精密度(RSD,N=11)5.91%~12.83%。能满足地质样品中w(Ag)/10-6=0.03~5范围内银测定的准确度和精密度的要求。     

Correction of matrix effects in the analysis of stream waters by flameless atomic absorption spectrophotometry

Direct injection techniques to measure trace metal concentrations by flameless atomic absorption were applied to fresh water samples of low to moderate matrix content. Many samples exhibited high non-atomic absorption which was decreased considerably by HNO₃ digestion within the furnace. The remaining background absorption could not be reduced by selective volatilization prior to atomization. It was taken into account where necessary by background measurements at nearby non-absorbable wavelengths.Other interference problems applying especially to Cd, Pb and Zn were eliminated by operating at higher than usual atomization temperatures. The method of standard additions to calibrate concentrations seemed to be adequate for these particular samples.Using the method recommended, precision tests to measure “within batch” and “between batch” variations were carried out for four elements in a typical sample.     

NK8310螯合树脂分离富集地质样品中痕量金银铂钯及其测定

研究了硫脲螯合树脂（NK8310）分类富集地质样品中痕量Au、Ag、Pt和Pd的实验条件。在φ=10％的王水介质中，[AuCI4]^-、[AgCI2]^-、[PtCI6]^2-和[PdCI4]^2-定量吸附于树脂上并与大量贱金属分离；用5g/L硫脲－0.12mol/L HCI溶液洗脱Au、Ag、Pt和Pd，回收率为97％－104％。用硫镍矿管理样以及国家一级标准物质进行分析验证，分析结果与推荐值及标准值吻合，表明NK8310螯合树脂适用于地质样品中Au、Ag、Pt和Pd的分离富集。     

The effect of filtration on analyses of surface water samples. A study from the Salars of Coipasa and Uyuni,Bolivian Altiplano

Analyses by inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and cold vapour atomic absorption (for Hg, CVAA) of a wide range of elements in some 300 surface water samples from the Salar de Uyuni and Salar de Coipasa catchments of the Bolivian Altiplano have been undertaken. Comparison of analyses of acidified aliquots of unfiltered sample water with water filtered at 0.45 μm reveals that the following elements are not affected significantly by filtration in this high-pH environment: B, Ca, Li, Mg, K, Si, Na, Sr, S. The following elements appear to experience significantly elevated concentrations in unfiltered samples, relative to filtered: Al, (As to a minor extent), Ba, Be, Cd, Cr, Co, Cu, Fe, Pb, Mn, Hg, Ni, P, Ag, Tl, Ti, V. The effect appears to be related to the presence, and subsequent dissolution in acid preservative, of Fe-, Al-or Mn-oxyhydroxide flocs (or coatings on silicate particles) in unfiltered samples, and their retention or precipitation on filters.     

Comprehensive Analysis of Precious Metals in some Geological Standards by Flameless A.A. Spectroscopy

Precious metals (Ag, Au, Pt, Pd, Rh) were determined by flameless absorption atomic spectrornetry. Aqua regia sample decomposition followed by Te coprecipitation was employed to preconcentrate the precious metals in geological materials. With 5 g sample take-up, the limits of determination were 1-2 ppb for Au, Pd and Rh, 5 ppb for Ag and 10-20 ppb for Pt. These elements were determined in some geochemical standards.