Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.

Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix byinductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line ofyttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium.In mis work, a method based on wavelet transform was proposed for the spectral interferencecorrection. Haar wavelet was selected as the mother wavelet. The discrete detail after the thirddecomposition, D3, was chosen for quantitative analysis based on the consideration of bothseparation degree and peak height. The linear correlation coefficient between the height of the leftpositive peak in D3 and the concentration of Y was calculated to be 0.9926. Six synthetic sampleswere analyzed, and the recovery for yttrium varied from 96.3 percent to 110.0 percent. The amountsof yttrium in three ytterbium metal samples were determined by the proposed approach with an averagerelative standard deviation (RSD) of 2.5 percent, and the detection limit for yttrium was 0.016percent. This novel correction technique is fast and convenient, since neither complicated modelassumption nor time-consuming iteration is required. Furthermore, it is not affected by thewavelength drift inherent in monochromators that will severely reduce the accuracy of resultsobtained by some chemometric methods.

CORRECTION OF WING INTERFERENCE WITH KALMAN FILTERING IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.

A Perspective of Laser Sampling for Inductively Coupled Plasma-Atomic Emission Spectro metry for Rock and Mineral Analysis

The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.

Determination on Heavy Metals Content of Achyranthes bidentata Blume. through Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

[Objective] The inductively coupled plasma mass spectrometry(ICP-MS)was constructed to determine the contents of lead,cadmium,mercury and arsenic in Archyranthes bidentata Blume.[Method]Under the optimum operation condition of ICP-MS,the samples were digested by microwave.The element 114In was taken as an internal standard element to compensate body effect and ICP-MS method was used to determine the contents of lead,cadmium,mercury and arsenic.[Result]For the determined elements,the correlation coefficient(r)of standard curve was over 0.9995 and recovery rate was from 96.7% to 106.4% while RSD was less than 11.2%.The result of determination showed that the heavy metal content in Archyranthes bidentata Blume.beyond standard was serious.[Conclusion]The constructed ICP-MS method with simple operation,rapid response,accuracy and high sensitivity in this experiment could be used for quality control of Chinese medicinal materials by detecting heavy metal contents in different Chinese medicinal materials from original places.

The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

Diagnostics of Argon Inductively Coupled Plasma and Dielectric Barrier Discharge Plasma by Optical Emission Spectroscopy

An experimental setup was built up to carry out radio frequency (RF) inductively coupled plasma (ICP) and dielectric barrier discharge (DBD), and to depict the optical emission spectra (OES) of the discharges. OES from argon ICP and DBD plasmas in visible and near ultraviolet region were measured. For argon ICP, the higher RF power input (higher than 500 W for our machine), the higher degree of argon plasma ionization. But that doesn't mean a higher mean electron energy. With the increase in the power input, the mean electron energy increases slightly, whereas the density of electron increases apparently On the contrary, argon DBD discharge behaves in the manner of a pulsed DC discharge on optical emission spectroscopy and V-I characteristics. DBD current is composed of a series of pulses equally spaced in temporal domain. The Kinetics of DBD emission strength is mainly governed by the frequency of the current pulse.

Speciation of Volatile Selenium Species in Plants Using Gas Chromatography/Inductively Coupled Plasma Mass Spectrometry

Gas chromatography/inductively coupled plasma mass spectrometry (GC/ICP-MS) coupled with solid phase micro-extraction can provide a simple, extremely selective and sensitive technique for the analysis of volatile sulfur and selenium compounds in the headspace of growing plants. In this work, the technique was used to evaluate the volatilization of selenium in wild-type and genetically-modified Brassica juncea seedlings. By converting toxic inorganic selenium in the soil to less toxic, volatile organic selenium, B. juncea might be useful in bioremediation of selenium contaminated soil.

Uncertainty Evaluation of Simultaneous Determination of Lead, Cadmium and Arsenic in Cosmetics by Inductively Coupled Plasma Mass Spectrometry

This study aimed to evaluate the uncertainty of simultaneous determination of lead(Pb),cadmium(Cd)and arsenic(As)in cosmetics by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)with ^72Ge,^115In and ^209Bi as internal standards.According to the method of Safety and Technical Standards for Cosmetics(2015),a mathematical model was established to evaluate the sources and components of uncertainty for the determination of lead,cadmium and arsenic in cosmetics.The results showed that the uncertainties in the determination of lead,cadmium,and arsenic elements in cosmetics were(10.1±0.6)mg/kg,k=2,(4.84±0.28)mg/kg,k=2,(2.04±0.18)mg/kg,k=2,respectively.The main factors that affect the uncertainty of determination results were standard substance,calibration curve,recovery and measurement repeatability.

<i>In Situ</i>Analysis of Copper Alloys by Femtosecond Laser Ablation Inductively Coupled Plasma Mass Spectrometry: Constrains on Matrix Effects

Direct analysis of copper-base alloys using laser ablation techniques is an increasingly common procedure in cultural heritage studies. However, main discussions remain focused on the possibility of using non-matrix matched external reference materials. To evaluate the occurrence of matrix effects during in situ microanalysis of copper-base materials, using near infrared femtosecond laser ablation techniques (NIR fs-LA-ICP-MS), two bronzes, i.e., (Sn-Zn)-ternary and (Sn)-binary copper-matrix reference materials, as well as a reference synthetic glass (NIST-SRM-610) have been analyzed. The results have been compared to data obtained on a sulfide-matrix reference material. Similar values in relative sensitivity averages of 63Cu, 118Sn and 66Zn, as well as in 118Sn/63Cu and 66Zn/63Cu ratios were obtained, for all analyzed matrix types, i.e., copper-base-, silicate-, and sulfide-reference materials. Consequently, it is possible to determinate major and minor element concentrations in copper alloys, i.e., Cu, Sn and Zn, using silicate and sulfide reference materials as external calibrators, without any matrix effect and over a wide range of concentrations (from wt.% to ppm). Equally, Cu, Sn and Zn concentrations can be precisely determined in sulfides using homogeneous alloys (reference) materials as an external calibrator. Thus, it is possible to determine Cu, Sn and Zn in copper-base materials and their ore minerals, mostly sulfides, in a single analytical session, without requiring specific external calibrators for each matrix type. In contrast, immiscible elements in copper matrix, such as Pb and Fe show notable differences in their relative sensitivity values and ratios for different matrix-materials analyzed, implying that matrix-matched external calibrations remain to be applied for their trace quantification.

基于破乳诱导萃取和ICP-MS/MS分析渣油中的微量金属元素

基于破乳诱导萃取提出利用电感耦合等离子体串联质谱(ICP-MS/MS)测定渣油中多种金属元素的新策略。渣油样品经二甲苯稀释降低黏度后采用质量分数6%的Triton X-114乳化,超声水浴破乳25 min,利用体积分数40%的盐酸萃取渣油中金属元素至水相,采用ICP-MS/MS测定其中10种金属元素Na、Mg、Al、Ca、V、Cr、Fe、Ni、Cu、Zn的含量。详细评估了破乳诱导萃取条件对渣油中金属元素萃取效率的影响,在串联质谱(MS/MS)模式下,利用氦碰撞气或不同反应气消除了金属元素的质谱干扰,采用标准参考物质NIST SRM 1634c(燃油中的微量元素)验证了方法的准确性,以微波消解技术处理渣油样品并采用扇形磁场电感耦合等离子体质谱(SF-ICP-MS)进行对比分析验证了方法的可靠性。结果显示,金属元素在各自的含量范围内呈现良好的线性关系(线性相关系数≥0.9997),检出限(LOD)为2.05~31.4 ng/L,NIST SRM 1634c的测定结果与标准参考物质提供的认证值及文献报道的参考值基本一致,置信度水平达到95%,ICP-MS/MS方法与SF-ICP-MS的对比分析结果无显著性差异。所建立的ICP-MS/MS方法操作简单,分析速率快,准确可靠性好,已用于渣油中多种金属元素的质量评价。

萃取/反萃取-电感耦合等离子体发射光谱(ICP-OES)法测定肥料样品中铅、镉、汞、铊、锑、砷

为保障农产品的质量与安全,肥料中的有毒有害物质,尤其是重金属含量被严格限制。为提高肥料中有毒有害物质检测的效率,利用铅、镉、汞、铊、锑、砷在盐酸介质中形成稳定的碘络合物的特性,采用甲基异丁基酮(MIBK)萃取、硝酸溶液反萃取的方法实现肥料样品中基质与待测元素的分离,通过电感耦合等离子体发射光谱法测定肥料样品中的6种重金属元素。通过考察萃取条件及残余基体对分析结果的影响,结果证实,在6 mol/L的盐酸萃取体系中加入5 mL碘化铵(30%)溶液,采用10 mL的MIBK萃取2~3次即可使样品中的铅、镉、汞、铊、锑、砷等被完全萃取,通过萃取/反萃取的方法实现了样品的分离富集,方法的检出限(3σ)为铅0.042 mg/kg、镉0.005 mg/kg、汞0.059 mg/kg、铊0.026 mg/kg、锑0.024 mg/kg、砷0.052 mg/kg,加标回收率在90.1%~108%,可以满足不同肥料样品的质量控制要求。按照实验方法测定6种不同肥料样品中的重金属含量,并采用标准方法进行方法比对,结果表明两种方法的测定结果基本一致。

Elemental Content in Brown Rice by Inductively Coupled Plasma Atomic Emission Spectroscopy Reveals the Evolution of Asian Cultivated Rice

The phylogenetic relationship for classification traits and eight mineral elements in brown rice （Oryza sativa L.） from Yunnan Province in China was carried out using microwave assisted digestion followed by inductively coupled plasma atomic emission spectroscopy, and the analytical procedures were carefully controlled and validated. In general, the results show that the mean levels of K, Ca, Mg, Fe and Cu in brown rice for 789 accessions of rice landraces was distinctly lower than that of improved cultivars. They further demonstrate that Ca plays an important role in the differentiation of subspecies indica-japonica, especially to enhance adaptation of cold stress, and that five mineral elements in brown rice enhance the eurytopicity from landrace to improved cultivar. Hierarchical cluster analysis, using average linkage from SPSS software based on eight mineral elements in brown rice, showed that Yunnan rice could be grouped into rice landrace and improved cultivar, with the rice landrace being further clustered into five subgroups, and that, interestingly, purple rice does not cluster with either of the groups. Our present data confirm that indica is the closest relative of late rice and white rice, and that they constitute rice landraces together, whereas japonica is the closest relatives of non-nuda, early-mid and glutinous rice. It is further shown that japonica, non-nuda, early-mid, glutinous, white and red rice might be more primitive than indica, nuda, late, non-glutinous and purple rice, respectively.

ICP-MS/MS测定轻质油中痕量氯含量

基于H_(2)反应模式下的质量转移反应消除干扰,建立电感耦合等离子体串联质谱(ICP-MS/MS)测定轻质油中痕量Cl的分析方法。轻质油经简单稀释后直接采用ICP-MS/MS进行测定,在MS/MS模式下使用H_(2)作为反应气,利用在碰撞/反应池(CRC)中Cl^(+)与H_(2)发生二次H原子转移反应形成的子离子(H_(2)Cl^(+))进行测定,消除所有质谱干扰,获得Cl的灵敏度和检出限(LOD)明显优于O_(2)反应模式,LOD低至7.56μg/kg。通过与扇型磁场ICP-MS(SF-ICP-MS)对比分析标准参考物质NIST SRM 1634c,评价方法的准确可靠性。结果表明,标准参考物质的分析结果与认证值基本一致,相对标准偏差(RSD)为3.1%~4.7%,2种方法的对比分析结果在95%的置信度水平无显著性差异。所建立分析方法的灵敏度、准确度和和精密度高,MS/MS模式和H_(2)质量转移法的结合可无干扰测定轻质油中的Cl,适用于轻质油中痕量Cl的质量控制与评估。

改良的电感耦合等离子体发射光谱(ICP-OES)法测定石灰性土壤中交换性盐基钙、镁、钠、钾

为提升石灰性土壤中交换性盐基钙、镁、钠、钾的分析效率与精确度,笔者采用电感耦合等离子体发射光谱(ICP-OES)技术测定其含量。结果表明,最优条件为用70%乙醇溶液反复淋洗样品,再用pH值为8.5的0.1 mol/L的氯化铵-70%乙醇溶液进行交换处理,蒸干后加入10mL 20%~30%的硝酸溶液进行酸化处理。经此处理,把传统的单标溶液转变为混标配置,选择谱线分别为钙317.933 nm、镁279.553 nm、钠589.592 nm、钾766.491 nm,测得国标样品的加标回收率为98.0%~100.7%,检出限分别为0.008、0.005、0.004、0.007 mg/L。对两个国标样品GBW(E)070337、GBW(E)070341进行验证,测得的相对标准偏差(RSD)为0.29%~0.98%(n=5)。对吉林土壤(样品1)测得的结果与火焰光度计+原子吸收分光光度法测得的结果无显著性差异。结果表明该方法适用于石灰性土壤交换性盐基钙、镁、钠、钾的分析。

ICP-AES法和原子荧光法检测硫熏处理对山药中重金属的影响

目的:研究硫黄熏蒸对山药中重金属含量的影响,为评估硫黄熏蒸的安全性及山药加工工艺提供科学依据。方法:选取13批不同产地的硫黄对山药进行熏蒸处理,使用微波消解法对样品进行前处理,并通过电感耦合等离子体原子发射光谱法与原子荧光光谱分析法定量分析硫黄及熏蒸前后山药中汞(Hg)、砷(As)、铜(Cu)、镉(Cd)和铅(Pb)的含量。结果:13批硫黄中Pb、As、Hg含量偏高。硫黄熏蒸后,山药中Pb含量普遍上升,且部分样品中As、Hg和Cu含量亦有增加。结论:硫黄熏蒸可能导致重金属元素从硫黄迁移到山药中,因此应制定严格的硫黄熏蒸工艺规范,确保山药的安全性和质量,减少对人体健康的潜在风险。

电感耦合等离子体原子发射光谱(ICP-AES)法测定真空精炼镁合金物料中铁、铜、镍

真空精炼是目前镁金属提纯的重要工艺,工艺原料及真空精炼提纯镁金属过程残留物中Fe、Cu、Ni含量的准确测定对工艺参数的优化及调整具有重要的指导作用。传统测定方法中以邻二氮杂菲分光光度法、新亚铜灵分光光度法、丁二酮肟分光光度法测定三种元素含量,结果准确,但操作繁琐,周期较长,难以满足工业生产中高效、快速测定的需要,且方法中所需的有机萃取剂对环境污染较大。选择电感耦合等离子体发射光谱(ICP-AES)法测定真空蒸馏精炼镁合金物料中Fe、Cu、Ni,系统探究溶解酸、溶解温度、溶解时间对物料溶解和测定的影响,选择盐酸(1+1)和过氧化氢溶解体系,200℃加热条件下反应20 min为最佳消解镁合金原料条件;选择王水溶解体系,200℃加热条件下反应25 min为真空精炼残留物最佳溶解条件。并探讨ICP-AES测定过程中各元素的检出限和测定下限以及共存元素的干扰情况,建立了ICP-AES法测定真空精炼提纯镁合金物料的方法。测定结果的相对标准偏差(RSD,n=11)为Fe 5.9%~11.5%、Cu 2.6%~11.8%、Ni 3.4%~11.5%,各元素加标回收率为Fe 96.4%~102%、Cu 101%~108%、Ni 103%~105%;按照建立的方法测定镁合金原料、真空精炼残留物中的铁、铜、镍,并与国家标准方法测定结果进行对比,结果相一致。实现了ICP-AES法快速、准确测定真空蒸馏精炼镁合金物料中铁、铜、镍含量,对及时、高效、准确评估真空精炼提纯镁工艺及产品具有重要意义。

基于MC-ICP-MS的稳定铜同位素分析在环境健康研究中的应用进展

铜(Cu)是人体内重要的微量金属元素之一,在许多生命过程中扮演着重要角色;同时,铜在人体内受到严格调控,其稳态与人体生理状态密切相关,许多疾病的发生往往伴随着铜代谢失衡的现象。通过监测铜稳态的细微变化,可以更精准地发现导致人体生理异常变化的因素,特别是环境因素对疾病发生及发展的影响。因此,稳定铜同位素分析在环境健康研究中具有广泛的应用前景。多接收器电感耦合等离子体质谱(MC-ICP-MS)是一种强大的同位素分析质谱方法,具有适用范围广、分析精度高等优点,有效促进了铜同位素分析的发展。本文综述了非传统稳定同位素分馏机理及基于MC-ICP-MS的铜同位素分析方法,总结了铜同位素分析在环境健康研究中的主要应用,并对其前景进行展望。

氧气反应模式-四极杆ICP-MS定量高温合金中痕量元素及质谱干扰消除机理研究

本研究建立了氧气反应模式-四极杆电感耦合等离子体质谱(Q-ICP-MS)法准确定量高温合金中痕量杂质元素,对不同碰撞/反应模式消除质谱干扰的效果进行研究。结果表明,氧气动态反应池(DRC-O_(2))模式下,目标元素Cd的多原子离子质谱干扰能够被有效去除;在优化气流为2 mL/min时,信噪比达到最高,检出限较标准模式(STD)降低了近3个数量级。此外,还研究了质谱干扰的消除机理,发现对于元素X(X=Rb、Nb、Mo、Cs、Ta、W或U),当X-O键能大于O-O键能时,质谱干扰组分XO转化成非干扰组分XOO为自发反应,因此,O_(2)充足时更容易生成XOO,从而消除XO干扰。在此基础上,采用高浓度基体模拟溶液(Mo、Nb、Ta、W)分别对痕量Cd、Ag、Au、Hg元素测量的方法学参数进行评估,方法检出限0.08~0.31μg/g、测量重复性相对标准偏差(RSD)2.3%~3.1%(n=6),加标回收率98%~103%,并进一步使用高温合金标准物质验证了方法的可靠性。最后,对3类典型牌号高温合金样品中的痕量杂质进行测量,证明该方法的分析速度快、检出限低、准确可靠,能够满足高温合金中主量Mo、Nb、Ta、W元素存在时被干扰杂质的测量要求。

电感耦合等离子体原子发射光谱(ICP-AES)法测定石煤钒矿石中钒、铁、钛的含量

研究一种快速准确测定石煤钒矿石中钒、铁、钛含量的方法对石煤钒矿检测行业的发展和石煤钒矿资源的开发利用、综合评价具有重要的意义。试样经过氧化钠在650℃完全熔融后保持1~3 min,取出冷却,热水浸提,盐酸酸化,定容稀释,选择V 292.402 nm、Fe 259.940 nm、Ti 334.941 nm为分析谱线,利用电感耦合等离子体原子发射光谱法(ICP-AES),建立了石煤钒矿石中同时测定钒、铁、钛含量的方法。优化了钒、铁、钛元素的分析谱线和背景校正模式,采用全程序样品空白稀释配制的校准曲线消除盐度钠基影响;研究了坩埚、熔剂种类、直接碱熔与灼烧-碱熔前处理方式、酸度效应的影响。结果表明:方法检出限为0.009%~0.019%,定量限为0.027%~0.057%;铁、钛、钒3种元素浓度在0.10~30.0μg/mL时,校准曲线线性回归方程的相关系数均大于0.9999;采用国家一级标准物质(GBW07876、GBW07877、GBW07878)进行验证,相对标准偏差(RSD,n=12)为0.49%~0.87%,且测定值与标准值吻合。方法具有快速简便、精密度好、准确度高、同时测定钒、铁、钛等优点,满足石煤钒矿石化学分析检测需求,且可为石煤钒矿化学分析标准方法的建立提供技术支撑。