电感耦合等离子体原子发射光谱（ICP-AES）法测定高纯氧化铟中7种杂质元素

采用电感耦合等离子体原子发射光谱(ICP-AES)法测定高纯氧化铟中杂质元素Al、Cd、Cu、Fe、Pb、Tl和Zn等的含量。使用盐酸(1+1)溶解高纯氧化铟试样,基体铟的干扰采用基体匹配法消除,被测元素之间没有光谱干扰。对方法进行加标回收实验和精密度实验,方法加标回收率在92.2%～110%,测得结果的相对标准偏差在0.57%～5.8%,可以满足高纯氧化铟中Al、Cd、Cu、Fe、Pb、Tl和Zn等杂质元素含量的测定要求。     

基体分离-电感耦合等离子体原子发射光谱(ICP-AES)法测定精铋中10种杂质元素

采用电感耦合等离子体原子发射光谱(ICP-AES)法测定精铋中Cd、Co、Cu、Fe、Mg、Mn、Ni、Pb、Ti、Zn等十种杂质元素,样品用优级纯硝酸溶解,往60℃左右的溶液中,滴加氨水(1+1),控制pH值在3.0～4.0.考察了温度、酸度、沉降时间对铋的去除率和对检测结果的影响.根据分析线的选择原则,结合待测元素...     

藏药材铁棒锤的微量元素含量分析

目的研究藏药材铁棒锤的微量元素含量。方法使用电感耦合等离子体质谱仪(ICPMS)测定藏药材铁棒锤药材中As、Hg、Pb、Cd含量,使用原子吸收光谱仪(火焰法、石墨炉法)测定药材中Zn、Mn、Cr、Fe、Ca、K、Cu元素的含量并进行分析。结果铁棒锤中有害元素As、Hg、Pb、Cd含量较低,Cu、Fe等有益元素含量较高。结论藏药材铁棒锤有丰富的微量元素,具有较高的开发利用价值。     

微波消解-ICP-MS法同时测定木薯淀粉中铅、铜、镉、砷、汞的含量

用硝酸-过氧化氢溶液(3+3)作为消解剂,微波消解法处理木薯淀粉等样品,采用电感耦合等离子体质谱法,选择适合的同位素元素,运用碰撞池技术(CCT)降低元素Cu、As的多原子离子干扰,测定样品溶液中Pb、Cu、Cd、As、Hg等元素的含量,各元素线性相关系数为0.9997 ～0.9999,元素的检出限(3sd)分别为pb...     

ICP-AES测定硫酸锌中痕量杂质铜铅铁锰镉镍

应用电感藕合等离子体和WSP-1光栅摄谱仪测定硫酸锌中痕量杂质元素Cu、Fe、Pb、Mn、Cd和Ni。对于Cu、Pb、Fe、Mn和Ni的检测限分别为1.7,16,1.8,0.46,12.7和11.8微克/克。没有光谱干扰。变异系数在4.1—17.6％的范围内。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K,Na,Ca,Mg,Zn,Fe,Cu,Mn,Se,Pb,Cd和Cr 12种元素。结果表明:方法简便、快速、准确;山药富含对人体有益的K,Ca,Fe,Mg,Zn,Mn,Se等矿物质元素,其肉质中重金属元素Pb,Cd,Cr含量均未超过国家食品卫生标准。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定锌精矿中杂质元素含量

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了锌精矿中Ca,Mg,Cu,Pb,Fe,As,Cd,Sb八种元素的含量。其测定范围:0.1%≤w(Ca,Mg,As,Cu,Pb)≤5.0%,0.05%≤w(Cd)≤2.0%,1.0%≤w(Fe)≤10.0%,0.03%≤w(Sb)≤0.5%。经加标回收实验,各元素的加标回收率为95%~104%(n=3),相对标准偏差RSD小于0.27%~4.7%(n=11)。方法快速,准确、可靠,适用于锌精矿中Fe,Cu,Pb,Cd,Ca,Mg,As,Sb含量的同时测定。     

电感耦合等离子体原子发射光谱（ICP-AES）法测定 高纯氧化铟中7种杂质元素

采用电感耦合等离子体原子发射光谱(ICP-AES)法测定高纯氧化铟中杂质元素Al、Cd、Cu 、Fe、Pb、Tl和Zn等的含量。使用盐酸(1+1)溶解高纯氧化铟试样,基体铟的干扰采用基体匹配法消除,被测元素之间没有光谱干扰。对方法进行加标回收实验和精密度实验,方法加标回收率在92.2%~110%之间,测得结果的相对标准偏差在0.57%~5.8%之间。     

电感耦合等离子体原子发射光谱法测定粗锑中的As、Bi、Cd、Cu、Fe、Pb和Se元素

通过样品处理、谱线选择、准确度和精密度测定、加标回收实验及与其他测定方法的比对实验,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定粗锑中As、Bi、Cd 、Cu、Fe、Pb、Se 7种元素的定量分析方法。实验结果表明,该方法准确度高,稳定可靠,相对标准偏差(RSD,n=6)均小于3%,方法的加标回收率在95~105%之间,分析结果与分光光度法、原子吸收光谱法(AAS)及原子荧光光谱法(AFS)分析结果相吻合,能够满足日常对粗锑中杂质元素含量测定的要求。     

电感耦合等离子体质谱法测定镁合金中的多种元素

用电感耦合等离子体质谱(ICP-MS)法测定了镁合金中的Be、Al、Ca、Fe、Mn、Ni、Cu、Zn、Ag、Cd、Sn、La、Ce、Pb14种元素,进行了稳定性实验以及Cu、Zn、Ni、Mg、Al基体实验,考察了共存元素的干扰.镁合金标准物质测定值与参考值符合较好,方法检出限为0.0002～0.3346 μg/g,相对标准偏差RSD＜10%.     

Improved separation of cadmium from indium,zinc, gallium and other elements by anion-exchange chromatography in hydrobromic nitric acid mixtures

The separation of cadmium from indium, zinc and many other elements is considerably improved by eluting these elements with 0.1 M hydrobromic–0.5 M nitric acid solution from a column of AG1-X8 resin. Cadmium is retained very strongly and can be eluted with 2 M nitric acid or 1 M ammonia–0.2 M ammonium nitrate solution. Separations are sharp and quantitative and from microgram amounts up to 2 g of indium and zinc are separated from amounts of cadmium ranging from micrograms up to 100 mg on a 2-g (4.6 ml) resin column. Ga(II), Fe(III). Mn(II), Co(II), U(VI) and Ni(II) can be separated quantitatively from cadmium in the same way. The behaviour of numerous elements is discussed, with special attention to lead, and relevant elution curves and results from the analysis of synthetic mixtures are presented.     

Improved separation of cadmium-109 from silver cyclotron targets by anion-exchange chromatography in nitric acid—hydrobromic acid mixtures

A method is presented for improved separation of ¹⁰⁹Cd from silver cyclotron targets. After dissolution of the target material in nitric acid and removal of silver by precipitation with copper metal, at pH 5, the cadmium is separated from zinc, copper and other elements by anion exchange chromatography. The solution in 0.5 M nitric acid plus 0.1 M hydrobromic acid is percolated through a column containing 4 ml of AG1-X8 anion-exchange resin (100–200 mesh), equilibrated with the same acid mixture. Zinc, copper(II) and other elements are eluted with 50 ml of this mixture. Cadmium is retained and finally eluted with 50 ml of 3 M nitric acid. The cadmium is retained much more strongly from the hydrobromic acid mixture than from the 0.02 M hydrochloric acid used for such separations previously; the presence of the strongly absorbed nitrate anion in fairly high concentration completely eliminates the tailing of zinc observed in 0.02 M hydrochloric acid. A typical elution curve and results of quantitative separations are presented.     

EDTA滴定法连续测定铅精矿中铅和锌

建立了EDTA滴定法连续测定铅精矿中铅和锌的方法。试样用盐酸、硝酸、硫酸和氯酸钾分解。铅通过硫酸铅沉淀与其他干扰元素分离,沉淀溶解于乙酸-乙酸钠溶液中。在滤液中加入氨水、氟化钾使铁等干扰元素沉淀并与锌溶液分离。用二甲酚橙作指示剂,EDTA分别滴定溶液中的铅和锌。研究中测定了能力验证NILPT(2010)-0211铅精矿样品10-1和10-2中铅和锌,结果满意。     

Hexaacetato calix(6)arene as the novel extractant for palladium

A novel method is proposed for the solvent extraction of palladium. A superamolecular compound, hexaacetato calix(6)arene in low concentration in toluene quantitatively extracts microgram concentration of palladium at pH 7.5. It can be stripped from the organic phase with 2 M nitric acid and determined spectrophotometrically as its stannous chloride complex at 635 nm. The probable composition of the extracted species is Pd(HR)(2)Cl. As low as 1x10(-3) M of extractant is adequate for quantitative extraction. Toluene was the best diluent. With nitric and perchloric acid (1.5-3 M) the stripping was complete. Palladium was separated in large ratios from alkali and alkaline earths (1:50). The main group elements were tolerated in higher ratios (1:25), but ions like zinc, cadmium, iron, nickel, platinium, thorium, vanadium and molydenum were tolerated at low concentrations (1:1). The ions showing strong interference were copper, chromium. The relative standard deviation is +/-1.1%.     

Separation of traces and minor amounts of lead from large amounts of zinc,indium, gallium and other elements on a low cross-linked anion-exchange resin

Lead is separated from gram amounts of Zn, In, Ga, Fe(III), Cu(II), Co(II), Mn(II), U(VI), Ca and Ba on a short column of AG1-X4 anion-exchange resin in the bromide form. Lead is retained from 0.2 M hydrobromic acid while the other elements are eluted completely with this reagent. Lead is then eluted with 2 M nitric acid. Separations are sharp and quantitative and, especially for gram amounts of zinc, much better than those obtained with an 8% cross-linked resin; up to 10 mg of lead can be separated from 2 g of zinc. Results are given for synthetic mixtures and lead is determined in several analytical grade chemicals.     

Cation-exchange separation and determination of silver in admixture with mercury(II)

Cation-exchange separation of silver from mercury(II), copper(II), cobalt(II), nickel and zinc, based on the differences in the stability constants of the complexes formed by these elements with EDTA at pH 4.6, is described. Silver is eluted with 16% nitric acid and is determined by Volhard's method.     

Anion-exchange separation of cadmium in organic solvent-nitric acid media

The anion-exchange separation of cadmium from zinc and aluminium in organic solvent-nitric acid mixtures was studied. The distribution coefficients of the 3 elements in various 90% organic solvcnt-10% 5 N nitric acid media were determined for Dowex I-X8 resin. A 90% ethanol-10% 5 N nitric acid medium was most satisfactory for the quantitative separation of cadmium from zinc and aluminium. The method was applied to the analysis of some copper and aluminium base alloys. Methyl glycol or acetic acid could be used instead of ethanol. Both cadmium and zinc were strongly adsorbed from a 90% propionc acid-10% 5 N nitric acid medium; separation was then effected by gradient elution.     

Determination of zinc in ammoniacal ore leaching solutions by X-ray fluorescence spectrometry using a radioactive source

A method was developed for the fast determination of zinc in leaching solutions by radioisotope energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The measured intensities were used to develop regression models for estimating the zinc concentration. The primary radiation was provided by the ²⁴⁴Cm radioisotope. Several experimental parameters including the saturation thickness and detection limit were determined. The advantages of the utilization of conditioning agents with elements of low atomic number such as nitric acid were established.     

微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定含铜污泥中多种重金属

为了填补现有方法的技术空白,本方法采用微波消解和电感耦合等离子体原子发射光谱法（ ICP-AES）相结合,实现对含铜污泥中铅、锌、铬、镉、砷、镁、铝、锑量的同时测定。首先采用盐酸-硝酸-氢氟酸微波消解进行样品的前处理,消解后加入高氯酸置于电热板进行除碳并赶酸,溶样效果理想,且有效避免了高温溶样对易挥发元素砷、锑的损失,整个过程安全、高效、无损。溶样后以电感耦合等离子体发射光谱法（ ICP-AES）进行测定。对含铜污泥的分解方法进行了合理选择,并对测定时的元素分析谱线及各测定元素间干扰情况等进行了讨论。该方法的加标回收率在95.31%~107.28%%,相对标准偏差（RSD）在0.31%~2.05%之间（n=7),结果表明,该方法准确度高,操作简单快捷,可同时测定多种元素,能满足批量的测定含铜污泥中铅、锌、镍、铁、镉、铬、砷、锑含量的测定要求。     

Determination of cobalt, copper, iron, nickel and zinc in cemented tungsten carbides with cobalt as a binder by FAAS: Matrix effect control by multivariate technique

A new approach for the determination of cobalt, copper, iron, nickel and zinc in cemented tungsten carbides with cobalt as a binder by flame atomic absorption spectrophotometry (FAAS) is reported. Real samples were dissolved in phosphoric, hydrochloric and nitric acid. PTFE bomb or alternatively small amounts of HF were used for the enhancement of the recovery of the elements investigated. Synthetic samples were used for interference studies. Multiple linear regression was applied for the control of matrix effects and it proved to be very effective in the search for interfering elements. Using simple acid based standards, all investigated elements could be determined sequentially in a complex matrix by using an appropriate method of calculation. The method described has been succesfully applied to real type commercial samples. Results were compared with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES) and X-ray fluorescence spectrometry (XRF), being in good agreement with each other and having relative standard deviations better than 5%.