氢化物连续发生电感耦合等离子体原子发射光谱法测定高纯铟中砷锑锡

采用氢化物连续发生与电感耦合等离子体原子发射光谱联用技术对高纯铟中砷、锑和锡的测定进行了研究。考察了酸介质及其浓度、硼氢化钠浓度及还原剂等对信号强度的影响,砷、锑和锡的检出限分别为0．13,0．017和0．12μg·g-1,回收率分别为108％,93．1％和91．1％。     

示波极谱法快速测定金属锑中微量锡

提出了一个快速测定金属锑中微量锡的新方法;在硫酸-草酸-次甲基蓝极谱吸附波体手中,利用锑自然水解沉淀与锡相分离;以及反向极谱残锑不干扰锡测定的原理,直接测定了金属锑中0．000x-0．0x%范围内的锡,效果良好。     

示波极谱法测定电解锰用阳极板中锡

样品经硝酸分解，有硫酸钡共沉淀分离铅后，锡在硫酸氯化钠底液中，在峰电位－0．52V处产生良好的还原波，能直接测定电解锰电解锰用阳极板中锡。回收率为98．0％－101．6％，相对标准偏差0．91％－2．98％，方法简便，快速，准确、优于容量法，已应用于工业分析。     

流动注射—氢化物发生双道原子荧光仪同时测定水样中砷和锑

提出一种流动注射－氢化物发生双道原子荧光同时测定水样中痕量砷和锑的新方法,砷和锑的标准曲线范围为0－40ug.L^-1相对标准偏差小于5％,回收率为90－107％,检出限为0．025ug.L^-1。     

氢化物－气相色谱的元素光度检测器

研究开发的一种新型的元素光度检测器主要用于锗、砷、锡和锑的氢化物气相色谱检测，具有高灵敏，高选择性。它是在普通火焰光度检测器的基础上加装了特制的滤光片改制而成的。对锗、砷、锡和锑的检测限分别为３．０×１０￣（－１１）ｇ、７．０×１０￣（－１１）ｇ、７．０×１０￣（－１０）ｇ和１．１×１０￣（－８）ｇ，相对标准偏差分别为１．８％、２．４％、２．６％和３．０％。     

ICP-MS法测定铅栅板中微量及杂质成分

用电感耦合等离子体质谱法（ICP-MS）法直接测定铅栅板中钙、锡、铝、锑、银、铋、铁、锌、镍、镉、铜、砷等12种元素含量。样品用硝酸（1＋2）溶解后，用硫酸作沉淀剂，95％～98%的铅以生成PbSO4的形式沉淀，降低了测量过程中的铅离子强度，得到了较低的检出限。加入适量的盐酸，有效地防止了锡、锑等元素的水解。选择适当的同位素，克服了测定过程中的质谱干扰，以元素^45Sc、^115In、^204Tl作内标，采用内标法有效地补偿了因基体效应、接口效应及仪器波动的影响。方法的加标回收率为93．2%～105．0%，相对标准偏差为2．0％～7．0％。     

氢化物—原子吸收光谱法测定六味地黄丸中砷和锑

本文建立了氢化物原子吸收光谱法测定六味地黄丸中砷和锑的方法。方法的相对标准偏差砷为１．３％，锑为１．６％，回收率在９０％－１１０％之间，检出限分别为砷０．０６ｎｇ／ｍＬ，锑０．１ｎｇ／ｍＬ，本方法可用于中成药中砷和锑的测定。     

碱性氢化物发生—火焰原子吸收光谱法测定锡

对Ｓｎ－ＮａＯＨ－ＫＢＨ４体系进行了系统研究，采用三乙醇胺－ＥＤＴＡ联合干扰抑制剂，可消除一定量铁及合金元素的干扰，对于锡含量小于０．０１％的试样，用苯萃取锡后所有元素不干扰测定。测定液中锡量为０－４μｇ／１０ｍｌ，呈线性关系，灵敏度为０．００４ｍｇ／Ｌ／１％，检出限为０．００８ｍｇ／Ｌ，测定钢中大于０．００１％锡，结果满意。     

氢化物－气相色谱的元素光度检测器

 研究开发的一种新型的元素光度检测器主要用于锗、砷、锡和锑的氢化物气相色谱检测，具有高灵敏，高选择性。它是在普通火焰光度检测器的基础上加装了特制的滤光片改制而成的。对锗、砷、锡和锑的检测限分别为３．０×１０￣（－１１）ｇ、７．０×１０￣（－１１）ｇ、７．０×１０￣（－１０）ｇ和１．１×１０￣（－８）ｇ，相对标准偏差分别为１．８％、２．４％、２．６％和３．０％。     

低锑砷合金中微量元素的测定

研究了火焰原子吸收光谱法测定低锑砷合金中微量元素含量的最佳测量条件,包括燃助比,燃烧器高度,灯电流,光谱通带以及基体元素对测定的影响,实验表明,在选定实验条件下,Cu,Ag元素欲望在0－4mg/L,Sb元素含量在0－80mg/L范围内均符合比尔定律,相关系数（r)为0．9979－0．9987,方法简便,快速,选择性好,该法用于低锑砷合金中微量元素Cu,Ag,Sb的测定,结果令人满意,方法的回收率为91－97％。相对标准偏差为1．1％－2．4％。     

分光光度法同时测定无机多组分体系的研究 Ⅵ 锑、锡和锗的同时测定

本文提出一个快速同时分光光度测定锑、锡和锗的方法。锑、锡和锗经磷酸三丁酯萃取后,用苯基萤光酮显色,各配合物重叠光谱的相互干扰用CPA-矩阵法处理,方法简捷,灵敏度及准确度均较好,用于合成样品及河流沉积物中锑、锡和锗的测定,获得满意的结果。     

Determination of Antimony in Brass by On-line Hydride Generation Atomic Fluorescence Spectrometry Alkaline Solution

The hydride generation(HG) technique combined with atomic spectrometry as a detection system has become one of the most powerful analytical tools for the determination of elements, such as As, Sb, Bi, Se, Te,Ge, Sn and Pb. Normally, the hydride is generated by the reaction between an acidic sample solution with tetrahydroborate. However, when some inorganic ions such as the transition metal ions are present in the reaction matrix, interference arise. Some approaches for minimizing the interference have been suggested, including the addition of various reagents such as thiourea and iron(III) solution. Interfering metals can also be removed by precipitation. The procedure involved filtration before the solution was acidified. In order to reduce the steps of the process, hydride generation from alkaline solution was described for the determination of selenium in copper and nickel materials.     

电感耦合等离子体原子发射光谱法(ICP-AES)测定N18锆合金中Nb,Sn,Fe,Cr元素含量

建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定N18锆合金中Nb,Sn,Fe和Cr含量的分析方法。对溶样方法、基体影响、谱线选择等进行了讨论,结果表明,锆基体对测定结果有一定的影响,在实验中采用基体匹配法消除基体干扰,并对实验条件进行了优化。在优化的实验条件下,该方法用于样品中Nb、Sn、Fe、Cr的测定,测定结果与化学法测定结果基本一致,加标回收率为96.7%~101.0%,相对标准偏差(RSD,n=11)均小于3%。     

Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry

A quartz multiatomizer with its inlet arm modified to serve as a trap (trap-and-atomizer device) was employed to trap tin hydride and subsequently to volatilize collected analyte species with atomic absorption spectrometric detection. Generation, atomization and preconcentration conditions were optimized and analytical figures of merit of both on-line atomization as well as preconcentration modes were quantified. Preconcentration efficiency of 95 ± 5% was found. The detection limits reached were 0.029 and 0.14 ng mL⁻¹ Sn, respectively, for 120 s preconcentration period and on-line atomization mode without any preconcentration. The interference extent of other hydride forming elements (As, Se, Sb and Bi) on tin determination was found negligible in both modes of operation. The applicability of the developed preconcentration method was verified by Sn determination in a certified reference material as well as by analysis of real samples.     

Application of a wall-stabilized argon plasma arc for the determination of some volatile hydride-forming elements

Volatile hydrides of As, Se, Sb and Sn, produced by a continuous manifold hydride generator, have been swept with argon and injected into the plasma of home-made direct current wall-stabilized argon plasma arc via one of its stabilizing segments. The arc burns in argon with an arc current of 20 A and a cathode-anode voltage of 40 V. Measurements were carried out using a 1 m focal length computer-controlled monochromator (Jobin Yvon 1000R) equipped with a holographic grating having 2400 grooves mm^− 1. Optimal values of the experimental variables that give the highest value of intensity ratio of line-to-background were determined. These are: plasma gas flow rate 1.0 l min^− 1, carrier gas flow rate 0.35 l min^− 1 for As and Sb and 0.6 l min^− 1 for Se and Sn, concentration of nitric acid used for acidification of the sample 2 M for As and Sb, 0.5 M for Se and 0.1 M for Sn and sodium borohydride concentration: 1.5% for As and Se and 2% for Sb and Sn. Chemical interference of some transition elements that affect the hydride generation process and a trial to mask their interference effect were investigated. Calibration curves were linear and limits of detection calculated on the base of 3σ of the background were found to be as low as 3.9, 6.8, 9.8 and 13.2 ng ml^− 1 for As, Se, Sb and Sn, respectively. Finally, the analytical applicability of the arc device was tested by the determination of As in four lake sediment samples, LKSD 1, LKSD 2, LKSD 3 and LKSD 4, of the Centre for Mineral and Energy Technology, Ottawa, Ontario, Canada, which have been analyzed for As using atomic absorption spectrometry (AAS). The results were in good agreement with those obtained by AAS.     

Determination of Trace Elements in Super Alloy by ICP-MS

 A method is described for determination of 14 trace elements in super alloy certified reference material. Inconel 718 by ICP-MS. The interferences were investigated in detail. By using appropriate settings of the operational parameters and correcting interferences the elements without interference free isotopes were also analyzed. Non-spectral interference to the analytes was studied. No matrix separation or any other sample pretreatment but acid dissolution was made. 14 trace elements (B, Sc, Ga, Ge, In, Sn, Sb, Te, Hf, Ag, Ce, Tl, Pb and Bi) were analyzed by matrix matched standard solution calibration and using Rh as internal standard. Good agreement was achieved between the found levels and the certified values for most of the elements. The RSD (n = 4) of the determination values of Ce was lower than 20%, and RSD of the other 13 elements was lower than 10%. Received July 21, 2000. Revision May 29, 2001.     

全谱直流电弧发射光谱法同时测定钼样品中17种杂质元素

为了解决现有测定方法中样品前处理复杂、测定过程繁琐的问题,研究了直流电弧发射光谱法测定钼样品中Al、Bi、Ca、Cd、Co、Cr、Cu、Fe、Mg、Mn、Ni、Pb、Sb、Si、Sn、Ti、V等17种元素的方法。用石墨粉(98%)、碳酸钠(1%)和氟化钠(1%)作为光谱缓冲剂抑制基体元素蒸发、稳定弧焰、促进杂质元素的蒸发;采用样品装满电极后下压2 mm和滴加蔗糖乙醇水溶液(2%)的方式,防止喷溅的发生,稳定激发过程,减小基体干扰;对挥发难易程度不同的元素采用信号分段采集的方式,提高各元素信噪比。方法灵敏度高、分析速度快、操作简便,加标回收率为85%~120%,各元素分析精密度均小于15%。     

Simultaneous determination of arsenic, antimony and tin by fast-scan differential-pulse polarography and its application to alloy steels

Arsenic, antimony and tin can be determined in the presence of one another by fast-scan differential-pulse polarography (FSDPP) on a single mercury drop in 1.5M hydrochloric acid. The reduction of As(III), Sb(III) and Sn(IV) to the metals is practically reversible and the reduction peaks are sufficiently separated. The lower limits of determination are 0.05, 0.005 and 0.001 μg/ml for As, Sb and Sn respectively, the calibration graphs exhibit very good linearity and the peak heights are reproducible. For application to alloy steels employed in nuclear technology, the elements to be determined must be separated from the matrix by extraction as their covalent bromides into toluene from concentrated sulphuric acid and back-extracted into the base electrolyte (1.5M HCl + 0.012M Br⁻ + 0.03M hydrazinium sulphate). The recoveries of As, Sb and Sn are 100, 95 and 92% respectively and the relative error of determination is a few per cent.     

混凝土中重金属元素溶出量的质谱分析

利用带八极杆碰撞/反应池和屏蔽炬技术的电感耦合等离子体质谱直接测定混凝土中Cr,Mn,Ni,Cu,Zn,As,Cd,Sn,Sb,Pb等多种重金属元素的溶出量。通过向碰撞池中引入氢气和氦气消除多元素分子离子的干扰,以50μg/L的Ge,In,Tb为内标元素校正基体干扰和漂移。10种待测元素的检出限为0.001～0.033μg/L,相对标准偏差为0.85%～2.8%,样品的加标回收率在91.1%～103.9%之间。     

Sequential voltammetric determination of trace metals in meals

An analytical procedure for the sequential determination of Zn(II), Cr(VI), Cu(II), Sb(III), Sn(II), Pb(II) by square wave anodic stripping voltammetry (SWASV) and Fe(III), Mn(II), Mo(VI) by square wave voltammetry (SWV) in matrices involved in foods and food chain as wholemeal, wheat and maize meal is described.The digestion of each matrix was carried out using a concentrated HCl–HNO₃–H₂SO₄ attack mixture, employing dibasic ammonium citrate buffer solution (pH 6.9 and 8.7) as supporting electrolytes. The analytical procedure was verified by the analysis of the standard reference materials Wholemeal BCR-CRM 189, Wheat Flour NIST-SRM 1567a and Rice Flour NIST-SRM 1568a.For all the elements in the certified matrix, the precision as repeatability, expressed as relative standard deviation (s_r) was of the order of 3–5%; the accuracy, expressed as relative error (e) was generally of the order of 3–6%.In presence of reciprocal interference, the standard addition method considerably improved the resolution of the voltammetric technique.Finally, the analytical procedure was transferred and applied to commercial meals sampled on market.A critical comparison with atomic absorption spectroscopic measurements is also discussed.