离子色谱法检测高纯硅微粉中痕量铁和氧化铁杂质

建立了柱后衍生-紫外检测-离子色谱法同时测定高纯硅微粉中痕量铁和氧化铁杂质含量的方法。方法选用具有阴阳离子交换基团的高选择性Thermo Scientific Dionex^TM IonPac^TM CS5A色谱柱,选择与铁形成单一络合形态、中等络合能力的2,6-吡啶二羧酸（PDCA）为淋洗液,在线柱后添加普适性的4-2-吡啶偶氮苯二酚（PAR）金属显色剂,于530 nm波长下准确完成了二价和三价铁离子的分离测定。结果表明,本方法对二价铁离子和三价铁离子的检出限分别为0.013 mg/kg和0.006 mg/kg,线性相关系数r²均大于0.999,实际样品中二价铁和三价铁的加标回收率分别为79%~90%和92%~105%,具有较高的灵敏度、准确度和选择性。该方法可以准确测定高纯硅微粉中痕量二价铁和三价铁的含量,以此结果反馈高纯硅微粉产品中铁杂质含量的不同来源,为其生产工艺的持续优化和改进提供重要的参考数据。     

Determination of trace elements in iron by neutron-activation techniques

A systematic analytical procedure for the determination of some trace impurities in iron matrices was developed by employing both direct and destructive neutron-activation techniques. Irradiations in fast neutron fluxes, selective activation by epithermal neutrons and coincidence γ-spectrometry measurements were used in some cases, in order to improve the sensitivity for non-destructive analysis; for destructive methods, radiochemical separations based on ion exchange and solvent extraction were applied. Procedures are described, and some results of the determination of low concentrations of Al, Mn, Ti, V (non-destructive), P, S, Zn (destructive) and As, Co, Cr, Cu, Mo, Ni, Sc, W (both methods) in iron are reported and discussed.     

石墨炉原子吸收法测定高纯硒中痕量铁

研究了石墨炉原子吸收直接进样法和石墨炉内富集法测定高纯硒中痕量铁的条件,建立了石墨炉原子吸收法直接测定高纯硒中痕量铁的分析方法.直接进样法的检出限为0.008 μg/g,石墨炉内富集法的检出限为0.004 μg/g,相对标准偏差分别为:5.2%和4.6%,两种方法检测样品结果基本一致.测定含铁0.3 μg/g的高纯硒,测定值的RSD为4.6～5.2%.     

Determination of silicon in iron by thermal neutron activation

A new chemical separation procedure for the determination of silicon in iron after neutron activation was developed. It uses two separation steps, one on a cation exchange resin in HCl−HF-acetone medium, and the other on alumina at pH 9. The detection limit for silicon was 0.02 μg. This analytical procedure was applied to the control of the zone-melting purification of iron.     

高纯二氧化锗中痕量杂质的ICP-MS法测定

建立了高纯二氧化锗中痕量杂质Mg、Al、Ni、Cu、Zn、In、Pb的ICP-MS测定方法。选择了仪器最佳工作条件,研究了锗基体对被测元素的干扰,方法回收率为94％～114％,RSD为11．1％～57％。     

钼蓝分光光度法测定纯金中的硅

建立了钼蓝分光光度法测定纯金中硅量的方法。确定了基体的分离方法、分离条件、还原剂及其用量;考察了酸度,试剂等对测定的影响。在优化条件下对3个合成试样进行了测定,RSD10%。方法的回收率在97%~122%之间,满足测定的要求。方法适用于0.001%~0.005%的硅量的测定。     

Determination of trace amounts of iron by catalytic-adsorptive stripping voltammetry

A highly sensitive and selective voltammetric procedure is described for the determination of trace amounts of iron. The procedure is based on the adsorptive collection of an iron-thiocyanate-nitric oxide complex on a hanging mercury drop electrode. The adsorbed complex catalyzes the reduction of nitrite in solution, which gives a detection limit of 40 ppt iron (30 s accumulation). The stripping current increases linearly with iron concentration up to 80 ppb. The relative standard deviations are 4.2% and 1.6% at 0.5 ppb and 40 ppb respectively. Most of the common ions, except cobalt, do not interfere with the determination of iron. The procedure is applied to determine iron in biological samples, natural waters and analytical-grade chemicals.     

Determination of silicon in cast iron by 14 MeV neutron activation

Silicon in cast iron was analyzed by 14 MeV neutron activation—high-resolution γ-ray spectrometry. Silicon was detected as²⁸Al, the product of the²⁸Si(n, p)²⁸Al reaction. Interference of⁵⁶Mn was separated using a Ge(Li) detector and a biased amplifying system. The 1. 81 MeV gamma-radiation of⁵⁶Mn, which is the product of the⁵⁶Fe(n, p)⁵⁶Mn reaction of the matrix of cast iron, was used as an internal standard and for correction of the self-absorption of the 1. 78 MeV gamma-radiation of²⁸Al by the sample. The interferences of aluminum, phosphorus and manganese could be neglected according to the results calculated from their nuclear properties and contents in the cast iron of this experiment. The results of this method agreed well with the results of the usual chemical method, with errors less than 5% of the results, and the precision of the method was satisfactory with a C. V. of less than almost 6% for rapid analysis of silicon in cast iron. The analytical line through the origin with a slope of the mean value of the repetition experiments could be used as the analytical line with almost the same precision and accuracy of the results as for the analytical line calculated by the least squares method.     

Determination of trace elements in a silicon single crystal

Instrumental neutron activation analysis was applied to the determination of trace impurity elements in a silicon single crystal. Impurity concentrations in polysilicon melt were compared with those in a single crystal. Impurity concentrations in artificial quartz were also compared with those in natural quartz. Segregation coefficients in Au, Ir and Sb were determined at different concentrations. The segregation coefficient of an element in a silicon single crystal is constant over a critical concentration, it becomes larger gradually under the critical one, and at last it becomes larger than 1.     

Determination of trace element in a silicon single crystal

Neutron activation analysis was applied to the determination of trace impurity elements in a silicon ingot. Detection limits of 36 elements were calculated semi — empirically and compared with minimum concentrations detected in a silicon single crystal. The sources of the impurities were estimated from element concentrations detected in polycrystalline silicon and a quartz crucible. Segregation coefficients were determined from the concentration curves in a single crystal and discussed by comparing with reported values.     

Determination of trace amounts of permanent gases in ultra pure hydrogen by gas chromatography

Summary A HP-5880A gas Chromatograph equipped with TCD and FID has been used to determine trace amounts of O₂+Ar, N₂, CO, CH₄ and CO₂ in pure and ultra pure hydrogen. Utilizing the preconcentration technique, the minimum detectability with a 10-liter sample is around 0.2 ppb (v/v) for O₂+Ar, 0.4 ppb (v/v) for N₂, 0.05 ppb (v/v) for CO, 0.2 ppb (v/v) for CH₄ and 0.3 ppb (v/v) for CO₂. Calculation of results in trace gas analysis is discussed and a calculation method is proposed for the concentration of impurities in the sample calculated from the difference of successive sampling volumes and peak areas.

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Spurenbestimmung von permanenten Gasen in hochreinem Wasserstoff mit Hilfe der Gas-Chromatographie

     

双波长双指示剂催化动力学光度法测定痕量铁

铁是人体健康所必须的微量元素,它对人体的生理功能有一定影响.如果体内可利用的铁不能满足血红蛋白正常合成的需要,致使红细胞增殖能力下降,就会造成缺铁性贫血.相反,体内铁含量过高,又易产生癌症~([1]).     

苦安酸偶氮变色酸褪色光度法测定硅铁中钙

在pH 11.0的氨水-NH4Cl介质中,研究了显色剂苦安酸偶氮变色酸与钙的褪色反应,建立了测定硅铁中钙的褪色光度分析方法.讨论了吸收光谱、酸度、试剂用量、干扰离子等因素的影响,确定了反应的最佳条件.在25 mL的溶液中,钙量在8～90 μg范围内符合比尔定律,该方法表观摩尔吸光系数为1.26×104 L·mol-1·cm-1,可用于硅铁中钙的测定.其RSD在1.4%～2.1%之间.     

Determination of silicon in Japanese iron reference standard materials by reactor fast neutron activation analysis combined with a simple pre-concentration

A reactor fast neutron activation analysis was used in combinationwith a simple pre-concentration procedure for determining silicon in someiron reference standard materials of Japan Iron and Steel Federation. Thesamples were dissolved with aqua regia and digested with perchloric or sulfuricacid. The precipitated silica was collected on a filter paper and irradiatedin a cadmium case with reactor fast neutrons. Silicon can be determined intool steel SKD6, low-alloy steel Nos 2 and 4 and silico-manganese samplesby a present method measuring 1,273.4 keV rays from 6.63-minute ²⁹Alproduced by ²⁹Si(n,p)²⁹ Al reaction.     

微波消解-双波长双指示剂动力学光度法测定人发中的痕量铁

研究了微波消解人发的最佳条件,同时研究了在HNO3介质中,痕量铁(Ⅲ)催化H2O2氧化甲基紫和亚甲基蓝褪色的指反应,建立了双波长双指示剂催化动力学光度法测定痕量铁的新方法。方法的线性范围为0.005~0.05μg/mL,检出限为1.02×10-4μg/mL。该方法可用于人发中痕量铁的测定。     

Functionalization of silicon nanowires by iron oxide and copper for degradation of phenol

Research on Chemical Intermediates - Iron oxide (Fe3O4) and copper-functionalized silicon nanowires (SiNWs) from silicon powder mesh?<?500 with a spherical structure have been...     

Determination of trace elements in uranium oxide by Total Reflection X-ray Fluorescence spectrometry

A study on the applicability of Total Reflection X-ray Fluorescence for the determination of multielements in trace amounts in U₃O₈ matrix has been made. The calibration of the Total Reflection X-ray Fluorescence spectrometer and the validation of the method were done using multielement standards. The trace elements present in U₃O₈ standards and samples were determined after separating the U matrix by solvent extraction using tri-n-butyl phosphate and trioctyl phosphine oxide as extractants. From the aqueous phase the elements K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, Br, Rb, Sr, Y, Zr, Pb and Ba, etc., were determined by Total Reflection X-ray Fluorescence using Ga as an internal standard. An intercomparison of the Total Reflection X-ray Fluorescence determined concentrations of the trace elements specific to nuclear fuel, e.g. Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn in U₃O₈ standards/samples with certified concentrations for these elements in U₃O₈ standards and Inductively Coupled Plasma Atomic Emission Spectroscopy determined concentrations in real U₃O₈ samples was also made. The method shows a precision and accuracy better than 5% (1σ) for most elements in concentration range of ng/mL with a sample size of 10 μL.     

High photocurrent in silicon photoanodes catalyzed by iron oxide thin films for water oxidation

Silicon splits: The application of silicon to water oxidation is limited due to unfavorable interface properties. However, these can be circumvented by using a high-performance silicon photoanode with a catalytically active iron oxide thin film (see picture). This approach results in photocurrents as high as 17?mA?cm(-2) under 1?sun and zero overpotential conditions.     

Nanoengineering of iron oxide and iron oxide/silica hollow spheres by sequential layering combined with a sol-gel process

Fe2O3 and Fe2O3/SiO2 hollow spheres with tailored dimensions and compositions were created by consecutively coating polystyrene (PS) latices either with Fe3+ alternately adsorbed with Nafion or combining a sol-gel process based on the hydrolysis of tetraethoxysilane (TEOS), and subsequently removing the cores upon pyrolysis.