X射线荧光光谱法快速测定黑铜中的铜、砷、锑、铋、铅、镍、锌和锡

建立X射线荧光光谱法快速测定黑铜中的铜,砷,锑,铋,铅,镍,锌和锡等多种元素含量的方法。采用自制的黑铜样品作为标准样品建立标准工作曲线。实验确定了样品加工时最佳的铣样速度及谱线重叠干扰的校正方法,并用理论影响系数校正基体干扰。试验结果表明,各元素的工作曲线线性关系较好,线性相关系数均大于0.996。各元素的检出限在17~47μg/g之间。测定结果的相对标准偏差为0.038%~2.73%(n=7)。两个样品的测定结果与标准分析方法的测定结果相符。该方法具有较好的准确度和精密度,分析速度快,能满足炉前快速分析的需要。     

氨水-氯化铵二次沉淀-碘量法快速测定冰铜中铜的含量

基于冰铜基体成分特点,在传统碘量法的基础上,对冰铜样品的前处理方法进行了改进,硝酸-氯酸钾溶解样品除硫,氨水-氯化铵二次沉淀分离铜,一次完成测定,省略了原子吸收光谱法补正的步骤,满足了碘量法快速测定冰铜中铜含量的要求。实验表明,相对标准偏差(RSD)在0.61%~1.9%,经国家标准物质验证及分析方法比对,结果准确可靠,精密度和准确度均能满足检测要求。方法简便,快速,大大提高了工作效率。较好地解决了冰铜中铜含量的快速测定,易于推广应用。     

X射线荧光光谱法快速测定铅铋合金中的铅、铋、金、银、铜、砷、锑、锡和碲

建立快速测定铅铋合金中铅、铋、金、银、铜、砷、锑、锡、碲含量的X射线荧光光谱法。采用自制的铅铋合金样品作为标准样品,用台式车床制样,用X射线荧光光谱法快速测定铅铋合金中各元素含量,并用α理论系数法和经验系数法相结合对基体效应进行校正。各组分校准曲线的相关系数均大于0.998,检出限为5.54～101μg/g,测定结果的相对标准偏差为0.06%～7.73%(n=9)。用该方法对3个铅铋合金样品进行分析,测定结果与参考值吻合,相对误差小于8.33%。该方法简便快捷,结果准确,能满足铅铋合金中各元素检测要求,对炉前分析具有很强的实用价值。     

标准曲线质量控制图在水质总磷检测中应用

建立测定水中总磷的标准曲线斜率、截距和质控样品质量浓度的X控制图。收集水质中总磷检测的27条标准曲线,绘制水质总磷标准曲线斜率、截距和质控样品中总磷质量浓度的X控制图,并应用于水质中总磷检测的质量控制。结果表明,钼酸铵分光法测定总磷标准曲线的斜率控制在0.008 90～0.009 84范围内,截距控制在–0.006 94～0.004 94范围内。利用该控制图上点的分布及趋势可以快速对实验过程中的标准曲线进行分析判断,验证实验过程是否处于受控状态,确保检测结果的准确性和可靠性。     

X-射线荧光光谱法测定白云石中主次量组分

采用粉末压片x-射线荧光光谱法测定白云石中氧化镁、氧化钙、二氧化硅、三氧化二铝、三氧化二铁和二氧化钛含量。采用校正曲线和基体校准一体的回归方程进行谱线重叠干扰校正和基体效应校正。将白云石样品进行磨细处理,在压片机上制成样片,直接在X-射线荧光光谱仪上按照选定的分析条件,以标准样品做工作曲线,利用工作曲线测定样品含量。通过与国家标准化学法以及熔片法对照,分析结果与标准值、熔片法结果吻合,主含量元素测定结果相对误差不超过10％,同一样品12次测定结果相对标准偏差不超过10％。该方法简便、快速、准确、重现性好。     

红外吸收光谱法测定钒铝合金中的碳和硫

通过工作曲线法、增量法、回收率实验、重复性实验等研究,验证了红外吸收光谱法测定钒铝合金中碳、硫结果的准确度,从而确立了无标准样品情况下测定钒铝合金中碳、硫的红外吸收光谱分析方法。通过测定标准样品并与实际值对照得知方法准确度高,误差小,实用性强。     

铅试金富集-电感耦合等离子体原子发射光谱(ICP-AES)法测定冰铜中的金、银、钯

冰铜的成分比较复杂,若酸溶后直接利用电感耦合等离子体原子发射光谱法测定贵金属的含量,杂质元素含量过高,干扰较为严重,导致结果偏差较大。为了准确地测定冰铜样品中的金、银、钯的含量,本试验首先用铅试金法在高温熔融状态下去除冰铜样品中的大部分杂质元素将贵金属富集到铅扣中,将铅扣灰吹除铅后得贵金属合粒,利用二次试金补正试验结果,用醋酸洗涤两次试金得到合粒后称量质量,合粒经硝酸溶解将金与其他元素分离,称量金粒质量,分金液中加入适量的盐酸溶液继续加热处理,然后采用电感耦合等离子体原子发射光谱仪在选定的最佳仪器工作条件下测定分金液中的金、铅、铋、铜、钯的浓度,通过给定的公式计算得出冰铜样品中金、银、钯的含量。试验讨论了氧化铅用量、灰吹温度以及基体干扰对测定结果的影响,当氧化铅加入量为200g,灰吹温度为890℃时,试验效果最好,干扰试验表明,样品中银的含量高低均不会对Au、Pb、Bi、Cu和Pd的测定产生影响。试验结果表明,银加标回收率在97.7 %～100.4 %之间,金的加标回收率在98.6 %～102.2 %之间,钯的加标回收率在98.0%～101.6%之间。该方法操作简单,在测定冰铜样品中金、银、钯的含量均有很好的准确度和精密度,RSD值均在1.067 % ~ 3.290 %之间,可以满足实际检测的需求。     

极谱法测定人发中痕量铜的研究

研究了痕量铜与CNS-及TriTonX 30 5非离子表面活性剂形成多元配合物 ,用示波极谱分析法测定痕量铜的新方法 .新方法铜的析出限为 1× 10 -10 g/mL ,工作曲线线性响应浓度范围为 5× 10 -9～ 5× 10 -7g/mL ,回收率为 98%～ 10 3% .直接用于人发、血清等样品中痕量铜的测定 ,其结果与原子吸收分光光度法测定结果对照相吻合     

电感耦合等离子体原子发射光谱法同时测定土壤中的铜、锌、镍、铬

建立电感耦合等离子体原子发射光谱法同时测定土壤中铜、锌、镍、铬的含量。在土壤样品中分步加入盐酸、硝酸、氢氟酸,电热板加热消解,将土壤标准物质GSS–17,GSS–22,GSS–8,GSS–27与样品按相同的方法处理绘制工作曲线。铜、锌、镍、铬的分析波长分别为327.39,206.20,231.60,267.72 nm。在一定的质量浓度范围内工作曲线表现出良好的线性关系,相关系数均大于0.999,4种元素的方法检出限分别为0.4,0.5,0.3,0.6 mg/kg。采用土壤标准物质GSS–26,GSS–20,GSS–16对方法准确度进行验证,测定值与标准值基本一致,样品加标回收率为82.3%～107.0%,测定结果的相对标准偏差为1.58%～4.68%(n=8)。该方法检出限、准确度和精密度均满足检测要求,可用于快速准确检测批量土壤样品中的重金属含量。     

固体标准物质绘制工作曲线在ICP—MS法测定土壤中重金属的应用

采用ICP-MS测定土壤中重金属含量,土壤样品因成分复杂而存在一定的基体干扰,选择与土壤样品基体成分相近的固体标准物质绘制工作曲线,并与传统的用标准溶液绘制工作曲线法进行比较,结果表明用固体标准物质绘制工作曲线与用标准溶液绘制工作曲线一样,线性关系好,符合样品测定的要求;应用于ICP-MS测定7种土壤或沉积物样品中Cu,Pb,Zn,Cd,Cr,Ni含量的结果说明,采用固体标准物质绘制工作曲线法,除cr外均存在较小的系统误差,但误差均在允许范围内,其中79％的分析数据的误差优于标准溶液绘制工作曲线法。     

A comparative analysis of gold-rich plant material using various analytical methods

During 2003 a field demonstration of gold phytoextraction technology was conducted in Brazil. As there is no commercially available biogeochemical standard reference material with an elevated concentration of gold, the trial biomass was analysed for its gold content using five analytical methods, at five laboratories, to confirm the concentration of gold in the harvested plant material. Nitric and hydrochloric acid digest followed by ICP-OES solution analysis of a doré bead prepared through fire assay of vegetative material was considered the benchmark analytical method to which the other results were compared. The gold concentrations reported by the five laboratories varied widely. Flame atomic absorption analysis of a solution prepared through the digest of plant ash by aqua regia proved the most accurate analytical method relative to fire assay. Gold concentrations reported by a New Zealand commercial laboratory using ICP-MS and a standard ‘biological materials digest’ procedure were affected by the digest method employed. X-ray fluorescence results may have been affected by synthetic standards that were prepared specifically for this investigation. Alternatively, matrix effects may not have been fully corrected for using XRF. Analysis of metal-rich biomass is becoming more common due to the popularity of studies that use plants to absorb heavy metals. The results of our comparative investigation emphasise that due care and consideration must be given to the selection of the analytical method chosen to analyse such plant material. Our results also highlight the need for standard reference materials that are suitably enriched in metals, such that these may be of use to phytoextraction studies.     

Dynamic calibration and automated instrumental analysis

The role of the analytical machine and the computer command in automated instrumental analysis are discussed and the eminent role of true and adapted reference material is stressed. The application of charts in process control (SPC) neglects the analytical potential which is contained in trends. As an improvement on-line calibration is suggested employing a set of high quality reference samples in a moving manner with subsequent regressions after each new analysis of one of the members of the set. The number of members of the set and the sequence of their analysis determine the corrective force of the system and weighted regression provides for large concentration ranges. The performance of the correction system was tested by simulation and results of application to OES and XRF in practice over long periods of time are communicated. The analysis of steel and oxide matter in form of iron ore sinter and blast-furnace slag resulted at any time in negligible bias between nominal and observed values of the set of reference samples. Residual standard deviations near or equal to the repeatabilities of the methods were observed.     

Analysis of hydrogen concentration in low-alloy steel

The hydrogen concentration for the reference material low-alloy steel was estimated using prompt gamma neutron activation analysis. The hydrogen concentration had a range of 0.91–1.14 mg/kg as measured by the prompt gamma activation method but the reference value was about 1.0 mg/kg as measured by the ICP/AES method. The relative error appeared to be 14% and the differences showed as the background by blank. The standard reference material (NIST SRM) was used for the analytical control.     

Laser Ablation Inductively Coupled Plasma Mass Spectrometry for Determination of Trace Elements in Geological Glasses

 Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used as a powerful multielement analytical method for trace analysis of geological glasses which are useful as reference materials for geochemical in-situ microanalytical work. The quantification of the analytical results was carried out using the BCR-2G and NIST 612 glass standard reference material (SRM). The experimentally determined relative sensitivity coefficients (RSC) for both SRMs vary between 0.2 and 3 for most of the elements, with increasing mass an increasing of relative sensitivity coefficients was observed. The relative standard deviation (RSD) for determination of trace element concentration of most elements (N=3) are between 2 and 10%. The determination of trace elements in various geological glasses by LA-ICP-MS yielded a good agreement with the reference values and those results of other trace analytical methods. Received October 15, 1999. Revision April 14, 2000.     

鼓风炉渣中氧化钙的测定方法改进

在参照DHF83-B多元素快速分析仪法测定炉渣中氧化钙的基础上,对鼓风炉渣中氧化钙的测定方法进行了改进。用盐酸（1+1）溶样,三乙醇胺掩蔽残留的铁、铝、锰等元素,以钙指示剂作指示剂,于pH值大于12时用EDTA标准溶液滴定氧化钙。EDTA滴定法分析结果的相对标准偏差RSD为2.82%,与DHF83-B多元素快速分析仪法比较,其结果基本一致。该方法具有准确度好、快速简便等优点,适合用于冶炼炉渣中氧化钙含量的测定。     

Thermal analysis and kinetics of the copper-lead matte roasting process

In this paper, the results of copper-lead matte investigations are presented. Investigated copper-lead matte is intermediate product of the lead production in TREPCA-Zvečan. In the first part of the paper characterization of starting material is presented, consisting of: chemical composition analysis (XRQ), scanning electron microscopy (SEM) and diffractometry (XRD). Thermal properties of investigated matte were determined using differential thermal analysis (DTA) at characteristic temperatures. Using results of induced analysis, mechanism of matte oxidation process was determined. In the second part of the paper kinetic parameters describing oxidative roasting of copper-lead matte are presented. For activation energy calculations, non-isothermal methods defined by Kissinger and Ozawa were used [1, 2]. Kinetic equation describing oxidation process was determined using Sharps method of reduced half time of reaction [3].     

偏振式能量色散X射线荧光光谱仪分析高炉渣

在偏振化能量色散型X射线荧光光谱仪上,使用一个HOPG次级靶,成功地对高炉渣中主要成分进行了分析。总的测量时间为120 s。此方法所得分析结果与标样中有关组分的证书值相符,也与工作标样中组分的已知值(化学法测得)一致。     

The determination of certain major and minor elements in geological samples by inductively coupled plasma atomic emission spectrometry. Some interference problems with the analysis of geological standard reference materials and nutrition supplements

Direct ICP-AES measurements of the digested geological standard reference material samples yielded the wrong information about their composition. The differences between certified and measured concentrations of the samples were due to the complicated sample matrix. The measured concentrations can be successfully corrected by using a multiple linear regression technique. The correction is based on the multiple regression line calculated from the analytical results at synthetic mixtures of matrix elements, where concentrations varied on five levels. There were no significant (P = 0.05) differences between certified and measured concentrations in standard reference materials after the correction. The same method was used in the analysis of nutrition supplements.     

ICP–AES法测定铬镍不锈钢中锰、铬、镍、硅、磷、铜、钼的含量

建立电感耦合等离子体原子发射光谱(ICP–AES)法测定铬镍不锈钢中锰、铬、镍、硅、磷、铜、钼7种元素含量的方法。试样用盐酸与硝酸混合酸溶液溶解,采用溶解国家标准样品的方法制备校准曲线溶液,确定了元素最佳分析谱线。各元素的含量在其测试范围内与原子发射强度呈良好的线性关系,线性相关系数不小于0.999,7种元素的检出限在0.000 3%~0.003 0%之间。该方法应用于铬镍不锈钢标准样品的测定,测定值与认定值相符,测定值的相对标准偏差在0.12%~1.15%之间(n=8)。应用于铬镍不锈钢样品测定时,加标回收率在90%~110%之间。该方法操作简便、迅速,可满足日常铬镍不锈钢中多元素含量的检测需要。     

微波消解-电感耦合等离子体原子发射光谱法测定钼铁合金中的钼含量

采用电感耦合等离子体原子发射光谱法（ICP-OES）测定钼铁合金试样（钼质量分数为55%～65%）中的钼含量,单点校准获得了较好的线性.样品经酸化后微波消解处理,采用钇元素作为内标以减少仪器波动的影响,在波长202.030 nm的分析谱线处测得钼元素的最佳发射强度.检测结果显示微波消解的样品溶解时间可缩短为重量法的14%,检测结果的相对标准偏差为0.17%～0.22%,采用标准样品验证结果的准确度与重量法无显著差异,可以为ICP-OES法检测高含量组分提供参考.