火花放电原子发射光谱法测定镍基合金中12种元素

化学元素的含量及其变化影响镍基合金材料的各项性能.因此准确检测镍基合金化学成分并对其严格控制,对提高和保证镍基合金材料性能具有重要意义.通过对仪器分析条件进行优化,采用控制样品法,建立了用火花放电原子发射光谱法测定镍基合金中Al、C、Cr、Co、Cu、Fe、Nb、P、Si、S、W、Mo等12种元素含量的方法.采用优化的...     

火花放电原子发射光谱分析方法测定镍基合金中12种元素

化学元素的含量及其变化影响镍基合金材料的各项性能。因此准确检测镍基合金化学成分并对其严格控制,对提高和保证镍基合金材料性能具有重要意义。通过对仪器分析条件进行优化,采用控制样品法,建立了用火花放电原子发射光谱测定镍基合金中Al、C、Cr、Co、Cu、Fe、Nb、P、Si、S、W、Mo等12种元素含量的方法。优化的试验条件如下：①吹氩时间6 s;②预燃时间6 s;③积分时间8 s。应用此方法分析了三种常规镍基合金样品,测定值与现行国家标准分析方法结果一致。     

平台石墨炉原子吸收法直接测定镍基合金中铅和锑

平台石墨炉原子吸收法直接测定镍基合金中铅和锑谢文兵，姚金玉，胡庆兰（中国科学院长春应用化学研究所长春１３００２２）关键词石墨炉原子吸收，镍合金，铅，锑，基体改进剂石墨炉原子吸收法是测定痕量元素最有效的方法之一。但是铅和锑都是易挥发元素，为了增强灰化过...     

电感耦合等离子体原子发射光谱法测定镍基高温合金中铬、钛、铌、铝、铁、硼的含量

在对各元素的分析谱线的选择及基体元素镍对相关元素测定的干扰作了系统研究的基础上,提出用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定镍基高温合金中铬、钛、铌、铝、铁及硼6种合金元素的方法。上述6种元素的检出限(3s/k)在0.006 9~0.13 mg.L-1范围内。取GH 33镍基高温标准样品按所提出方法分析,测定值与标准值相互一致,测得相对标准偏差值(n=10)均小于1.5%。在基体镍溶液中加入各被测元素的标准溶液做回收试验,上述6种元素的回收率在98.3%~101.0%之间。为对此方法的准确性作进一步考核,对GH 4145高温镍基合金样品进行分析,各元素的测定值与国家标准方法的测定值相符合。     

氢化物原子吸收法测定镍基合金和钢铁中微量锡

拟定了氢化物原子吸收法测定镍基合金和钢铁中微量锡的方法。Cl~(6+)(1毫克),Al~(3+)(0.5毫克),Co~(2+)(1.2毫克),Cu~(2+)(1毫克),As~(3+)(5微克),Sb~(3+)(10微克)均可产生严重干扰(抑制信号约70—80%),因此,对于镍基合金要用氢氧化铍共沉淀分离法除去干扰元素,而钢铁试样不需分离就可直接用氢化物原子吸收测定。方法可测定低至0.0001%的锡。     

锆基合金中元素分析方法的研究进展

综述了近年来原子发射光谱法、原子吸收光谱法、分光光度法、滴定法、X射线荧光光谱法和质谱法等测定锆基合金中相关元素的分析方法及研究进展(引用文献64篇)。     

电感耦合等离子体原子发射光谱法测定哈氏合金中Cr、Fe、Mn、Mo、Ni的含量北大核心CSCD

哈氏合金（Hastelloy alloy）由Ni、Cr、Mo、Fe等元素组成,属于高等镍基合金,镍为面心立方结构,晶体学上的稳定性使得它能够比铁基合金容纳更多的合金元素[1]。哈氏合金作为高级镍基合金,在湿氧、亚硫酸、强氧化盐介质中都有优异的抗腐蚀性能[1],同时具有优良的强度、塑性、韧性、冶金稳定性、可加工性及可焊接性,已广泛应用于航空航天、核电及船舶等领域[2]。     

N4O2供体型环状席夫碱Ni(Ⅱ)配合物的合成、晶体结构、DFT计算及脲酶抑制活性(英文)

在镍(Ⅱ)离子存在的条件下,利用模板法以1,2-双(2-甲氧基-6-甲酰基苯氧基)乙烷与乙二胺按照1∶1的化学计量比[2+2]合成,得到N₄O₂型的二十八元大环席夫碱镍(Ⅱ)配合物[Ni(C₄₀H₄₄N₄O₈)]Cl₂·4CH₃OH。通过元素分析、红外光谱、粉末X射线衍射、单晶X射线衍射和密度泛函理论量化计算对镍(Ⅱ)配合物进行了分析和表征。结构分析表明,Ni(Ⅱ)离子与来自C=N基团的4个N原子和来自醚基团的2个O原子进行配位,形成扭曲的八面体几何构型。脲酶抑制活性及分子对接模拟研究表明,该镍(Ⅱ)配合物能较好地抑制脲酶活性。     

金基合金中钯铁镍钒的原子吸收法测定

用化学法分析金基合金中钯、铁、镍、钒等元素需经繁杂的分离手续,耗用较昂贵的试剂,取样量多,一次只能测定一个元素。而采用原子吸收法测定时,取样量和试剂用量只有化学法的几分之一,特别是钯的分析从0.5％到5％都能得到满意的结果。少用试样,分析多个元素,基体全可以回收,这对贵重金属的分析尤为重要。本文参考有关文献,就金基合金中钯、铁、镍、钒的火焰原子吸收法测定进行了研究,并进行了合成试液的分析试验、结果对照和方法精密度考察。方法是在试样分解后分取部分试液,以亚硫酸还原金分离除去,再以铝为干扰抑制剂,同时测定     

关于新版GB/T 4336-2016标准的理解和实施建议

<正>火花放电原子发射光谱法具有分析快速、检出限低、精确度高、多元素同时检测等优点,目前商品化的仪器设备可用于分析钢铁、铝及铝合金、铜及铜合金、镍基合金、锌及锌合金、镁及镁合金、铅锡合金等材料。火花放电原子发射光谱法已成为金属冶炼、铸造及其他金属加工行业在线或临线分析必不可少的分析手段。钢铁冶金过程中在线或临线分析时,主要涉及的国家标准方法包括GB/T 4336-2016《碳素钢和     

Determination of bismuth, selenium and tellurium in nickel-based alloys and pure copper by flow-injection hydride generation atomic absorption spectrometry—with ascorbic acid prereduction and cupferron chelation-extraction

Diverse matrix effects on the determination of bismuth, selenium and tellurium (μg g⁻¹) in nickel-based alloys and pure copper by flow-injection hydride generation atomic absorption spectrometry (FIAS-HGAAS) were investigated. Sodium tetrahydroborate was used as the reductant. The separation of analytes from copper matrix was mandatory while the analytes were successfully determined without being separated from the alloy matrix. Hydrochloric acid was effective in the prereduction of bismuth and selenium, however, it did not give any satisfactory result for tellurium in nickel-based alloys. In this work, 5% (w/v) ascorbic acid was proved effective for the prereduction of tellurium.Successful determination of tellurium in copper was achieved when N-nitroso-N-phenylhydroxylamine (cupferron) chelation-extraction was employed for the separation of tellurium from copper matrix. Cupferron chelation-extraction was performed in phosphate buffer (a mixture of 0.2 mol l⁻¹ sodium phosphate and 0.1 mol l⁻¹ citric acid). Lanthanum hydroxide coprecipitation at pH 10.0±0.5 was effective for bismuth and selenium. Standard reference materials of nickel-based alloys and pure copper were analyzed using the proposed methods. The linear range for the calibration curves were 0.30-15 and 0.20-10 ng ml⁻¹ for BiH₃ and H₂Se, respectively, with a correlation coefficient of 0.9995. For H₂Te, the linear range for the calibration curves was 0.50-12 ng ml⁻¹ with the correlation coefficient of 0.9994. Good agreement was obtained between experimental values and certified values. Satisfactory recovery ranged from 91±1 to 106±2% was obtained from five replicate determinations.     

Determination of trace impurities in iron and nickel-base alloys by graphite furnace atomic absorption spectrometry

Five approaches to the determination of trace amounts of lead, bismuth, thallium, selenium, tellurium, and silver in iron and nickel-based alloys were investigated. While all procedures produced satisfactory results, direct techniques yielded a significant times advantage over separation schemes. Matrix effects made calibration curves an impractical approach. A spiking technique was used to generate data on a wide range of standard alloy samples.     

原子荧光光谱法测定铜合金中铋元素含量方法改进

基于原子荧光光谱法测定铋元素时检出限低、测定结果稳定且准确等优点,研究原子荧光光谱法测定铜合金中铋元素含量的方法。在标准系列中加入相近浓度的铜元素标准溶液,原子荧光光谱法测定铜合金中铋元素含量。称取0.1 g样品,加入10 mL硝酸溶解,10%硫脲-5%抗坏血酸溶液7.5 mL预处理样品。在20μg/L的铋标准溶液中加入6 mL浓度为1000μg/mL的铜元素标准溶液。结果表明:在0~20μg/L范围内,该方法线性关系良好,线性方程为I=138.1670c+43.8572,相关系数为0.9996,所测定的样品中铋元素含量的相对误差在-4.3%~7.7%之间,精密度在0.4%~4.7%之间。原子荧光光谱法可作为铜合金中铋元素含量测定的方法。     

Determination of mercury in bismuth by neutron activation analysis

A method has been developed for the determination of traces of mercury in bismuth by neutron activation analysis. After sample irradiation at a flux of 7 · 10¹³ n cm^-2 s^-1 for 20 min, mercury was separated from bismuth by addition of ammonium sulfide and re-dissolution of bismuth (matrix) sulfide with nitric acid, and filtration of sulfur containing mercury on a membrane filter. The activity of the 68- or 68–77-keV region, counted with a Ge(Li) or NaI(Tl) detector, was used for quantitative measurements. The method was applied to bismuth samples containing 0.1–100 p.p.m. of mercury.     

Binary modifiers for the determination of zinc in pure copper and nickel-based alloy by longitudinal Zeeman electrothermal atomic absorption spectrometry

The determination of zinc in pure copper and nickel-based alloy was successfully accomplished with a longitudinal Zeeman-effect correction and end-capped transversely heated graphite atomizer. Since aqua regia (an acid mixture of nitric acid and hydrochloric acid, 1:3, v/v) was used as the dissolving reagent, volatile ZnCl₂ was formed. Consequently, less Zn was found in the sample. EDTA could improve the atomic absorption profiles. Binary modifiers, EDTA + Pd(NO₃)₂ and EDTA + Mg(NO₃)₂, were effective for eliminating the chloride interference and the spectral interference from Cu I 213.853 nm. The experimental results obtained with and without the modifiers were compared. Increase of 200 °C in the pyrolysis temperature resulted from the addition of binary modifiers for both pure copper and nickel-based alloys. For pure copper, the atomization temperature increased from 1400 to 1600 °C whereas the atomization temperature increased from 1100 to 1600 °C for nickel-based alloys. The analytical performance of the proposed method was evaluated. Zinc contents in the pure copper and nickel-based alloy standards determined with both binary modifiers agreed closely with the certified values. The recovery ranged from 93 ± 2 to 104 ± 6% at 95% confidence level. The detection limits obtained by the binary modifiers of EDTA + Pd(NO₃)₂ and EDTA + Mg(NO₃)₂ were 0.77 and 0.31 pg, respectively.     

Determination of bismuth by electrochemical stripping analysis; elimination of interferences by using a mercury film electrode modified with tri-n-octylphosphine oxide, and application to copper alloys

A mercury film electrode modified with a film consisting of tri-n-octylphosphinc oxide in a poly(vinyl chloride) matrix is used for a galvanostatic stripping determination of bismuth in copper and copper alloys. The method can be used to determine from 0.002 to 0.5% of bismuth. It is very selective, simple and rapid. The precision and accuracy are good and the only serious interference is caused by tin(IV).     

Determination of trace impurities in nickel-based alloy using neutron activation analysis

A radiochemical neutron activation analysis procedure has been applied to investigate 40 major, minor, and trace impurities in nickel-based alloy. The extensive use of these alloys in the electronic industry, telecommunications, manufacturing of aircraft engine turbine blades and chemical equipments desires for their precise characterization. The concentration of nickel in the nickel-based alloy was found to be 56.8%, whereas Fe, Cr, Ca, Mg, Ce, Mn, Na and V were the major components of the alloy, which constituted to more than 26%. The rest of the elements was present in minor or trace levels. Most of the rare earth elements except Ce were also present in trace amounts. Neutron activation analysis technique was preferably used because of its good sensitivity and multielement determination capabilities for the characterization of high purity materials. The comparison of RNAA and INAA indicated improvement in the detection limits utilizing radiochemical separation procedures developed in the present work.     

Extraction,Separation and Spectrophotometric Determination of Bismuth(III) Using 1(4′-Bromophenyl) 4,4,6-Trimethyl (1H,4H)-Pyrimidine-2-Thiol

Abstract

The operating conditions for the spectrophotometric determination of bismuth(III) with 1-(4′-bromophenyl)-4,4,6-trimethyl-(1H,4H)-pyrimidine-2-thiol (4′bromo PTPT) as a ligand by a liquid-liquid extraction technique are presented. In acidic conditions bismuth(III) forms a yellow complex with the ligand which can be extracted in chloroform with an absorption maxima at 410 nm. The molar absorptivity is 1.5×10⁴ l mole^?1 cm^?1 and Sandell's sensitivity is 14.3 ng cm^?2. The difference in the absorbance between the chloroform blank and bismuth(III) sample increases linearly in the concentration range 2-14 ppm at 0.3 M hydrochloric acid. The proposed method is extremely sensitive, rapid, reproducible and has been satisfactorily applied to the determination of trace amounts of bismuth(III) in synthetic mixtures, alloys and pharmaceutical formulations and also provides binary separation of bismuth(III) from selenium, tellurium, lead, antimony, copper and gold. The overall process of extraction and determination takes about 15 to 20 min.     

Behaviour of trace impurities during chemical dissolution of a metal: Platinum elements in aluminium and nickel

In order to study the behaviour of trace impurities during aqueous dissolution of a sample, aluminium and nickel-based alloys containing 10⁻⁴−1% Ir, Os or Ru were used. Yields of chemical separations such as distillation and ion-exchange were chosen as dissolution criteria. Dissolution of aluminium samples leads to precipitation of the three impurities. The Os and Ru precipitates can afterwards be dissolved by an oxidation procedure, in contrast to commercial powders of these elements. This behaviour may be explained in terms of the small grain-size of the precipitates. The indium precipitates cannot be dissolved, which prevents quantitative separation of this element from an aluminium matrix. In the case of nickel alloys, these three impurities are dissolved and can be quantitatively separated.