Rapid determination of indium,nickel and copper in NBS standard reference material by substoichiometric radioactivation analysis

A method of rapid determination for indium, nickel and copper in Spinach (NBS; SRM-1570) by substoichiometric radioactivation analysis is described. The method is based on the principle that an equal amount of non-irradiated test sample is added to the irradiated standard sample and subsequent substoichiometric extraction for the irradiated test and standard samples is carried out. Indium is extracted as diethyldithiocarbamate into carbon tetrachloride, nickel as dimethylglyoximate into chloroform and copper as dithizonate into carbon tetrachloride. The radioactivities of these extracts are measured by NaI(Tl) or Ge(Li) detector coupled with pulse-height analyser. The analytical results obtained by the method were in good agreement with our published values and certified values by NBS.     

Determination of vanadium,cobalt, copper,zinc, and cadmium in biological materials by a combined anion-exchange-spectrophotometric method

Summary A preconcentration technique involving anion-exchange in thiocyanate media has been developed for the determination of traces of bio-significant and biofunctional elements. The procedure is applied to the analyses of NBS standard reference materials as well as environmental reference materials of NIES (The National Institute of Environmental Studies, Japan Environmental Agency). The results are quoted for vanadium, cobalt, copper, zinc, and cadmium.     

Comparison of standard materials for the establishment of calibration curves in solid sampling graphite furnace atomic absorption spectrometry. Direct determination of copper in powdered biological samples

Summary The selection of standard materials for the establishment of calibration curves is one of the most important problems in the direct analysis of biological samples by GFAAS. Three kinds of standard materials, NBS tomato leaves, coprecipitates with magnesium oxinate and Ni/DMG/PAN were investigated. It was found that it is possible to use both the NBS-SRM and the synthetic reference material prepared by coprecipitation with magnesium oxinate as standard materials for the direct determination of copper in several biological samples issued from NBS and NIES. However, too low results are obtained when the synthetic reference material prepared by coprecipitation with Ni/DMG/PAN is used. In order to clarify this, the effects of nickel and magnesium were examined and the role of magnesium was discussed.     

Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultra-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B&C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS.     

Application of standard materials and standard reference materials in the analysis of lead in blood

Summary Valuable information can be obtained at little expenses from quality control samples prepared in-house to monitor the determination of blood lead by atomic absorption spectrophotometry. Commercially manufactured control materials can also be used for this purpose. These materials are compared to standard reference materials which at present are available.The relative standard deviations for analysis of NBS standard reference materials were 15.4–2.8% (range 60–754 g/l) and in agreement with the relative standard deviation estimated for the analytical method. The corresponding figures for BCR control reference materials were lower: 1.1–1.4% (range 134–795 g/l).The average analytical bias demonstrated by analysis of NBS standard reference material and BCR control reference material were 3–6% (range 795–60 g/l) and in agreement with bias estimated by analysis of commercially manufactured and in-house prepared control materials.     

Simultaneous determination of silicon and phosphorus in biological standard materials with on-line column flow-injection spectrophotometry

Summary A simultaneous determination of silicon and phosphorus in biological standard materials with on-line column flow-injection spectrophotometry (FIA) is described. Biological materials are ashed, fused with a lithium carbonate-boric acid mixture, and dissolved in a hydrochloric acid solution. Interfering cations are removed by a simple cation-exchange column filtration. The acid effluent is evaporated to dryness, fused with a small amount of sodium carbonate for depolymerization, taken up in dilute EDTA solution, and analyzed for silica and phosphorus by FIA. For the simultaneous determination of these elements, TSK-gel SAX was used, and the eluent was 0.085 mol/l NaCl/0.01 mol/l NH₃/0.001 mol/l EDTA. Several standard reference materials [bovine liver (NBS), chlorella and pepperbush (NIES)] were analyzed for both elements. The results of phosphorus determination for bovine liver are in satisfactory agreement with the NBS certificated value. ICP measurements were applied to analyses of chlorella and pepperbush for silica and phosphorus. The agreement of the analytical results between FIA and ICP is satisfactory. Silica in bovine liver was determined in the present study for the first time.

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Simultanbestimmung von Silicium und Phosphor in biologischen Standardmaterialien mit Hilfe von On-line Fließinjektions-Spektralphotometrie

     

Indium determination in different environmental materials by electrothermal atomic absorption spectrometry with Amberlite XAD-2 coated with 1-(2-pyridylazo)-2-naphthol

Methods were developed for indium (In) determination in complex ores by electrothermal atomization atomic absorption spectrometry using matrix modification after its separation with Amberlite XAD-2 coated with 1-(2-pyridylazo)-2-naphthol (PAN). Palladium-magnesium, nickel, and zinc nitrates were used as matrix modifiers and were compared in terms of maximum pyrolysis temperature, sensitivity and background signal. They have enhanced the absorption signals for indium, respectively eliminating the matrix interferences. The standard additions method was applied. The relative standard deviations for six replicate determinations were in the range 0.3-4.0% for indium in different ores samples for indium concentrations 7.6-209 μg g⁻¹. The recommended method was applied to the indium determination in real samples. The data obtained by this method were in good agreement with those obtained by ICP-AES.     

A highly selective diethyldithiocarbamate extraction system in activation analysis of copper,indium, manganese and zinc

A versatile separation system based on the extraction of dithiocarbamates and applicable to the determination of copper, managanese, zinc and indium in a wide selection of materials by activation analysis is described. After the dissolution of the sample and a few simple operations which eliminate specific interferences, depending upon the material (e. g. sodium and gold in the NBS Standard Reference Glasses), carbamates are extracted under specific conditions by addition of appropriate complexing agents and selective stripping. Extreme separation factors permit interference-free counting using a sodium iodide detector. For example, indium is separated from a hundred thousand fold excess of manganese in the determination of the two elements in Orchard Leaves. Results are also presented for all four elements in Bowen's Kale, NBS Bovine Liver, and for Cu, In and Mn in the 0.02 ppm and 1 ppm SRM glasses.     

辉光放电质谱法测定高纯材料中痕量硫杂质

准确测定并控制材料中杂质元素含量是发挥高纯材料性能不可或缺的环节。辉光放电质谱法(GDMS)是准确、快速、高灵敏分析高纯材料中痕量及超痕量硫的理想方法。对GDMS分析高纯铜和镍基高温合金中痕量硫的质谱干扰进行了讨论,优化了放电电流和放电电压,采用多种标准物质对硫的相对灵敏度因子(RSF)进行了校准和验证,并与二次离子质谱法(SIMS)进行分析结果比对,验证了GDMS定量分析结果的准确性和可靠性。     

A comparison of two separation techniques using NaI(Tl) and Ge(Li) spectrometry for trace element determination in biological materials by neutron activation analysis

A comparison of two group separation techniques using either NaI(Tl) or Ge(Li) spectrometry is presented for trace element determination in biological materials by neutron activation analysis. The capabilities of both procedures are described in terms of detection limits, precision and accuracy for the determination of the elements As, Cd, Co, Cr, Cu, Fe, Hg, Mo, Ni, Sb, Se, Sn, and Zn in various types of biological samples. For this purpose the (standard) reference materials NBS SRM-1577 Bovine Liver, Bowen's Kale, IAEA Pig Kidney H-7 and IAEA Milk Powder A-11 were analyzed. An attempt was also made to minimize blank values for several elements.     

Evaluation and Application of the Internal Standard Technique for the Direct Determination of Copper in Fruit Juices Employing Fast Sequential Flame Atomic Absorption Spectrometry

Abstract

The present paper describes the evaluation and application of internal standard for the determination of copper in fruit juices, employing Fast Sequential Flame Atomic Absorption Spectrometry (FS FAAS). The internal standards tested were indium, cobalt, and nickel using correlation graphs. However, indium was used, considering the composition of the samples. After this step, copper was determined in fruit juices using indium as internal standard. This method allows the determination of copper with a limit of quantification of 0.011 mg L^?1. The fruit juice samples selected for analysis were of grape, orange, pineapple, peach, cashew, and strawberry. The contents of copper in these samples varied from 0.02 to 0.42 mg L^?1. The analytical results were compared with the results obtained by analysis of these samples after complete mineralization using acid digestion and determination employing FS FAAS. The statistical comparison by a t-test (95% confidence level) showed no significant difference between the results. The relative standard deviations (RSD) with and without the use of the internal standard for a copper solution containing 0.4 mg L^?1 were of 0.62 and 1.94%, respectively. The use of indium as internal standard provided more accurate analytical results, as well as better analytical performance for the determination of copper in juice samples.     

Grain-scale heterogeneities in the stable carbon and oxygen isotopic compositions of the international standard calcite materials (NBS 19, NBS 18, IAEA-CO-1, and IAEA-CO-8)

We determined grain-scale heterogeneities (from 6 to 88 microg) in the stable carbon and oxygen isotopic compositions (delta(13)C and delta(18)O) of the international standard calcite materials (NBS 19, NBS 18, IAEA-CO-1, and IAEA-CO-8) using a continuous-flow isotope ratio mass spectrometry (CF-IRMS) system that realizes a simultaneous determination of the delta(13)C and the delta(18)O values with standard deviations (S.D.) of less than 0.05 per thousand for CO(2) gas. Based on the S.D. of the delta(13)C and delta(18)O values determined for CO(2) gases evolved from the different grains of the same calcite material, we found that NBS 19, IAEA-CO-1, and IEAE-CO-8 were homogeneous for delta(13)C (less than 0.10 per thousand S.D.), and that only NBS 19 was homogeneous for delta(18)O (less than 0.14 per thousand S.D.). On the level of single grains, we found that both IAEA-CO-1 and IAEA-CO-8 were heterogeneous for delta(18)O (1.46 per thousand and 0.76 per thousand S.D., respectively), and that NBS 18 was heterogeneous for both delta(13)C and delta(18)O (0.34 per thousand and 0.54 per thousand S.D., respectively). Closer inspection of NBS 18 grains revealed that the highly deviated isotopic compositions were limited to the colored grains. By excluding such colored grains, we could also obtain the homogeneous delta(13)C and delta(18)O values (less than 0.18 per thousand and less than 0.16 per thousand S.D., respectively) for NBS 18. We conclude that NBS 19, IAEA-CO-1, or pure grains in NBS 18 are suitable to be used as the standard reference material for delta(13)C, and that either NBS 19 or pure grains in NBS 18 are suitable to be used as the reference material for delta(18)O during the grain-scale isotopic analyses of calcite.     

Determination of sulfur,nickel and vanadium in fuel and residual oils by x-ray fluorescence spectrometry

The determination of sulfur, nickel and vanadium in fuel and residual oils by wavelength-dispersive x-ray fluorescence spectrometry is reported. Calibration is initially established with matrix-matched synthetic standards, and maintained free of instrumental drift by daily normalization to a reference standard. An epoxy-cast reference standard pellet offers mechanical rigidity and chemical stability for at least nine months. Matrix effects of sulfur and carbon are studied and corrected. Results for NBS SRM oils fall within the NBS certified values, with imprecision (% RSD) for S, Ni, and V of 1.1, 1.5 and 1.0%, respectively. Detection limits (3 s.d.) are 20 μg g^?1 for sulfur and 0.8 μg g^?1 for Ni and for V.     

Determination of trace elements in reference materials by the k(0)-standardization method (INAA)

Instrumental neutron activation analysis was applied to four reference materials: NBS 1573 (Tomato Leaves), NBS 1645 (Citrus Leaves), NBS 1645 (River Sediment), and IAEA MA-A-2 (TM) (Fish Flesh). The k(0)-standardization method was used. The results are compared with (i) reference values (mostly non-certified) and (ii) published values obtained by other methods. Good agreement is found for most of the elements. For some elements, large discrepancies are observed.     

Distribution patterns of rare-earth elements in biological materials evaluated by radiochemical neutron activation analysis

This study deals with the quantitative determination of eight REE's viz, La, Ce, Nd, Sm, Eu, Tb, Yb, and Lu as an Integral part of a post-irradiation chemical separation scheme for the determination of 14 trace elements in biological materials. REE values are given for NBS Orchard Leaves SRM 1571, NBS Bovine Liver SRM 1577 and Bowen's Kale, as well as for some other biological (reference) materials of plant, animal and human origin. Chondritic-normalized REE patterns of these materials are discussed. It is shown that differentiations in REE-pattern between soil and plant may occur, and also that within the human body different modes of fractionation of REE's take place.     

Neutron activation analysis of biological materials by the monostandard method

Instrumental neutron activation analysis by the monostandard method has been applied to the analyses of biological NBS standard reference materials; 1571 Orchard Leaves and 1577 Bovine Liver. Aluminum foils containing 0.100% gold or 2.00% cobalt were used as the monostandards. The gamma-ray spectral data were recorded on punched paper tape and were analyzed by a computer assisted data processing. The following 25 elements were determined: Al, Ca, Cl Cu, Mg, Mn, V (by short period irradiation), As, Ba, Br, Co, Cr, Cs, Eu, Fe, Hg, K, La, Na, Rb, Sb, Sc, Se, Sm and Zn (by long period irradiation). The results were compared with the certified values by NBS and the reported values in literatures to prove the reliability and accuracy of the monostandard method.     

离子交换分离石墨炉原子吸收光谱法测定高纯铟中痕量铜

高纯铟样品经盐酸溶解、以阳离子交换树脂分离出痕量铜后,用石墨炉原子吸收光谱法测定铜。研究了溶样方法、离子交换分离和测定铜的条件:用8mL浓盐酸将1g样品溶解;以0.6mol/L盐酸作为淋洗液进行离子交换,可把绝大部分铟基体及样品中痕量的银、砷、镉、硅分离除去,随后用2.0mol/L盐酸把铜洗出并收集之。铝、铁、镁、镍、铅、锡、铊、锌与小于10μg的铟不能与铜分离,但对测定无影响。当称样量为1g,进样量为50μL时,方法线性范围为1~4ng/mL,检出限为0.1ng/mL,测定下限为0.001μg/g,比行业标准方法 YS/T 230.1—2011的0.1μg/g低两个数量级。方法用于实际样品分析,结果与电感耦合等离子体质谱法(ICP-MS)相符,相对标准偏差(RSD,n=8)为1.7%~18.5%,加标回收率为94.8%~115.0%。     

流动注射在线柱预富集-电感耦合等离子体原子发射光谱测定痕量金属元素

本文报道了流动注射在线柱预富集ICP光谱测定痕量金属的方法,以meso-四(4-磺基苯)卟啉为柱前衍生试剂,硅胶作固定相和盐酸作洗脱液,对痕量金属离子Cu、Mn、Ni、Fe、Pb、Cd进行在线预富集检测。在给定实验条件下,方法的富集倍数为9.3～11.3,检出限和测定的相对标准偏差(n=6)分别在0.32～26.8ng/ml和1.3％～3.0％范围内。方法用于小牛肝和西红柿叶样品分析,结果与参考值吻合。     

H-point standard addition method for the selective simultaneous determination of nickel and copper using 1-(2-pyridylazo)-2-naphthol in Tween 80 micellar media.

The H-point standard addition method (HPSAM) has been applied for the simultaneous determination of nickel and copper in trace levels, using 1-(2-pyridylazo)-2-naphthol (PAN) as a chromogenic reagent in aqueous Tween 80 micellar media. Under the optimum condition, the simultaneous determinations of nickel and copper by HPSAM were performed. The absorbances at one pair of wavelengths, 548 and 579 nm, were monitored with the addition of standard solutions of copper. The method is able to accurately determine copper-to-nickel ratios of 15:1 to 1:10 (Wt/Wt). The effects of diverse ions on the determination of nickel and copper to investigate the selectivity of the method were also studied. The recommended procedure was successfully applied to some water and alloy samples.     

Simultaneous third-derivative spectrophotometric determination of copper and nickel in iron alloys and aluminium alloy

A method is proposed for the simultaneous determination of copper and nickel by third-derivative spectrophotometry based on the absorption spectra of their complexes with cyanide ion in the ultraviolet range. The method allows the determination of 0.55-5.8 mug/ml of copper and 0.55-6.8 mug/ml of nickel. The relative standard deviation for 11 determinations of 1.5 mul/ml of copper and nickel were 0.78 and 0.72%, respectively. The detection limits were 0.10,mug/ml for nickel and 0.13 mug/ml for copper. The method has been applied to direct determination of copper and nickel in iron alloys and an aluminium alloy without any separation.