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.

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.

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.

Laser Induced Breakdown Spectroscopy for Comparative Quantitative Analysis of Betel Leaves from Pakistan

Laser induced breakdown Spectroscopy(LIBS)was applied for the elemental analysis and exposure of the heavy metals in betel leaves in air.Pulsed Nd∶YAG(1064 nm)in conjunction with a suitable detector(LIBS 2000+,Ocean Optics,Inc)having the optical resolution of 0.06 nm was used to record the emission spectra from 220 to 720 nm.Elements like Al,Ba,Ca,Cr,Cu,P,Fe,K,Mg,Mn,Na,P,S,Sr,and Zn were found to present in the samples.The relative abundances of the observed elements were calculated through standard calibration curve method,integrated intensity ratio method,and weight percentage LIBS approach.LIBS findings were validated by comparing its results with the results obtained using a typical analytical technique of Inductively Coupled plasma-optical emission spectroscopy(ICP-OES).Limit of detection(LOD)of the LIBS system was also estimated for heavy metals.The experience gain through this work implies that LIBS could be highly applicable for testing the quality and purity of food products.

Compound Ceramic Coatings Grown by Micro-plasma Oxidation on Ti-6Al-4V Alloy

Compound ceramics coatings on the Ti-6Al-4V alloy were prepared by the direct current micro-plasma oxidation （MPO） in NaAlO2 solution. The composition and morphology of the coatings were studied with the X-ray diffraction （XRD） and the scanning electron microscopy （SEM）, respectively. Inductively coupled plasma atomic emission spectrometer technique was used to analyze the solution features of Ti-6Al-4V alloy in the process of preparation. The results reveal that Al2TiO5 forms in the coatings at the initial stages of MPO reaction, and its content changes rapidly with the reaction continuing： after 20 min, the ceramics coatings are composed of α-Al2O3, 7-Al2O3 and Al2TiO5, but after 40 min, its main composition is of α-Al2O3. The content of Ti in the solution will increase when the MPO time extends, and as will Al in the anode area until, after 30 min, it reaches the maximum and keeps constant from then on. Both substrata of Ti and Al in the electrolyte join the MPO reaction at the initial stage, where the formation of Al2TiO5 happens; but as the MPO reaction prolongs, more and more Al in the electrolyte will take part in the reaction, leading to the appearance of a large amount ofAl2O3.

Determination and Multidimensional Analysis of 22 Kinds of Inorganic Elements in Leontopodium franchetii Beauv. from Different Production Areas

[Objectives]To determine the content of inorganic elements in Leontopodium franchetii Beauv. from different production areas, and provide a reference for quality control, safety assessment, and clinical application of L. franchetii Beauv.. [Methods] The contents of Al, B, Ba, Ca, Cd, Cu, Fe, K, Mn, Mo, Na, Ni, P, Pb, Si, Sn, Sr, Ti, V, Zn, Hg, Cr in the sample of L. franchetii Beauv. were determined by the wet digestion and technique of inductively coupled plasma optical emission spectrometry(ICP-OES), and the principal component analysis was carried out for the determination results. [Results] A total of 20 inorganic elements were detected from the samples of L. franchetii Beauv. from different production areas, among which the contents of Ca, Al, P and Fe were higher. There were significant differences among different elements, and samples of different production areas show similar distribution patterns of main elements. Correlation analysis shows that 17 elements had an extremely significant positive correlation and 19 elements had a significant positive correlation. According to the principal component analysis, B, Ca, K, Mn, Mo, Pb, Sn, Sr, Fe, Ni, Ti, V, Zn, Al, and Cd were characteristic inorganic elements of L. franchetii Beauv. [Conclusions] This method is simple, rapid and accurate, and can be used for the analysis and determination of inorganic elements in L. franchetii Beauv., and provides a theoretical basis for better development and utilization of L. franchetii Beauv.

Application and Development Trends of Spectral Analysis in Draft of Non-Ferrous Metal Standards in China

Spectral analysis was a method of identifying substances, determining their chemical composition and calculating their content based on their spectral characteristics. This paper mainly discussed the application of various spectroscopic techniques, mainly including atomic absorption spectrometry (AAS) inductively coupled plasma emission spectrometry (ICP-AES) X-ray fluorescence spectroscopy (XRF) atomic fluorescence spectroscopy (AFS) direct reading spectroscopy (OES) glow discharge emission spectroscopy (GD-OSE) laser-induced breakdown spectroscopy (LIBS), in the formulation of non-ferrous metal standards in China. The AAS method was the most widely used single-element microanalysis method among the non-ferrous metal standards. The ICP-AES method was good at significant advantages in the simultaneous detection of multiple elements. The XRF method was increasingly used in the determination of primary and secondary trace elements due to its simple sample preparation and high efficiency. The AFS was mostly detected by single-element trace analysis. OES GD-OES and LIBS were playing an increasingly important role in the new demand area for non-ferrous metals. This paper discussed matrix elimination, sample digestion, sample preparation, instrument categories and other aspects of some standards, and summarized the advantages of spectral analysis and traditional chemical analysis methods. The new methods of future spectroscopic technology had been illustrated in the process of developing non-ferrous metal standards.

Determination and Multidimensional Analysis of 29 Inorganic Elements in Cardamine tangutorum O.E.Schulz of Different Origins

[Objectives]This study aimed to determine the contents of inorganic elements in Cardamine tangutorum O.E.Schulz samples from different origins to provide a scientific reference for the quality control,safety evaluation and clinical medicinal use of C.tangutorum O.E.Schulz.[Methods]The contents of Al,As,B,Ba,Ca,Cd,Co,Cr,Cu,Fe,Hg,K,Mg,Mn,Mo,Na,Ni,P,Pb,Pd,Rb,Se,Si,Sn,Sr,Ti,Tl,V and Zn in the C.tangutorum O.E.Schulz samples were determined simultaneously by wet digestion and inductively coupled plasma optical emission spectroscopy(ICP-OES),and the determination results were analyzed by principal component analysis.[Results]A total of 28 inorganic elements were detected in the samples of C.tangutorum O.E.Schulz from different origins.The contents of heavy metals did not exceed the limits.Among the elements,the determined values of Hg in all samples were below the detection limit,so it was not detected.The contents of Ca,Al,P and Fe were relatively high,and they were essential nutrients in the human body.There were significant differences among different elements.Samples from different origins show similar patterns in the distribution of main elements.Correlation analysis shows that 15 pairs of inorganic elements out of 24 elements had extremely significant positive correlations,and 26 pairs of elements had significant positive correlations.The principal component analysis determined Al,As,Ba,Ca,Cd,Fe,Mn,Ni,P,Pb,Pd,Se,V and Zn were the characteristic inorganic elements in the samples of C.tangutorum O.E.Schulz.[Conclusions]The contents of toxic heavy metals in C.tangutorum O.E.Schulz samples from different origins met the edible requirements.The method was simple,rapid and accurate,and could be used to analyze and determine the inorganic elements in the samples of C.tangutorum O.E.Schulz,providing a theoretical basis for the better development and utilization of C.tangutorum O.E.Schulz.

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。

电感耦合等离子体发射光谱法测定土壤中有效磷的不确定度评价

为准确测定土壤中有效磷的含量,采用电感耦合等离子体光谱仪进行测定,并对测定过程中相关因素引起的不确定度进行评定。整个实验过程中不确定度来源主要包括以下5个方面:(1)样品称量时引入的不确定度u(m);(2)加入浸提液时浸提液体积V引入的不确定度u(V);(3)标准溶液配置时引入的不确定度u(C_(s));(4)标准曲线拟合引入的不确定度u(C0);(5)样品测量重复性引入的不确定度u(R)。结果表明,样品测量重复性、标准溶液配置、标准曲线拟合在整个实验中引入的不确定度影响较大。因此,在实际样品测定过程中,一定要注意对结果有影响的不确定度因素,加强质量控制,使结果准确可靠。

电感耦合等离子体发射光谱法测定石灰岩中游离二氧化硅

建立电感耦合等离子体发射光谱(ICP-AES)法和粉末压片制样-X射线荧光光谱(XRF)法联合测定石灰岩中游离二氧化硅含量。准确称取经105℃烘干2 h的石灰岩样品0.1000 g,置于30 mL聚四氟乙烯坩埚中,加入8m L浓磷酸,置于300℃电热板上沸腾20 min,冷却后定容在100 mL容量瓶中,静置12 h。采用ICP-AES测定溶解在溶液中的二氧化硅含量,采用XRF测定石灰岩中二氧化硅总含量,用总的二氧化硅含量减去溶液中二氧化硅的含量就得出了游离二氧化硅的含量。经4种标准物质验证,游离二氧化硅含量分析结果与标准值满足规范中相对误差允许限的要求。该方法操作步骤更为简便,分析速度快,低含量游离二氧化硅结果准确度高,适用于批量石灰岩样品中游离二氧化硅含量分析。

铬污染场地的地下水中钾钠钙镁测定方法的比对

采用电感耦合等离子体发射光谱法(ICP-OES)和原子吸收光谱法(AAS),分别测定了水质标准质控样和铬污染场地的地下水中钾、钠、钙、镁的含量,对检出限、精密度、准确度等指标进行了比对。结果表明,2种方法的测定结果无显著差异,均能满足实验室的质控要求。相比AAS法,ICP-OES法无需进行样品稀释和换灯,操作更简单,并可同时测定多种元素。

伟晶岩型锂矿石中锂的化学物相分析方法研究

伟晶岩型锂矿石中产出的锂云母和锂辉石是重要的提锂原料,化学物相分析能够为这类锂矿石的地质勘探、矿床评价和高效选冶等提供重要的技术支撑。由于各类含锂矿物在化学性质上非常相似,目前尚未见与锂矿石化学物相分析相关的报道。本文建立了一种针对伟晶岩型锂矿中锂进行化学物相分析的方法。将锂物相分为铁锂云母中锂、锂云母中锂和锂辉石中锂三相。采用稀盐酸选择性浸出铁锂云母中锂,浓硫酸选择性浸出锂云母中锂,最后残渣用氢氟酸挥发除硅,王水溶解测定锂辉石中锂,并探索确立了各相态的最佳浸出条件。通过对川西某锂矿中锂物相进行6次分析,得到各相态锂的相对标准偏差(RSD)为1.27%~3.79%,均小于5%,各相态锂的加和与总锂结果的相对偏差为1.22%,小于5%,说明该方法适用于伟晶岩型锂矿石中锂的化学物相分析。

线叶金雀花茶中矿物质元素含量测定及饮用安全性分析

分析线叶金雀花茶的饮用安全性,为其加工和质量控制提供参考。采用电感耦合等离子体发射光谱法(inductively coupled plasma-atomic emission spectroscopy,ICP-AES)测定线叶金雀花茶中的钾、钙、钠、镁、磷、铁、锌、锰、铜、砷、铅、镉12种矿物质元素含量,并研究基于冲泡时间和冲泡次数对矿物质元素溶出率的影响,探讨其饮用安全性。结果表明:中国、南非2种不同产地的样品中矿物质元素含量排序均为钾>钠>钙>镁>磷>铁>锰>锌>铜,波兰样品中矿物质元素的含量排序为钠>钾>钙>镁>磷>铁>锰>锌>铜,砷、铅、镉在三种样品中均未检出,三种样品中铁元素含量差异显著(P<0.05),除铁元素外,南非和波兰的线叶金雀花茶中矿物质元素的含量无显著差异(P>0.05)。通过对矿物质元素的溶出特性进行探讨,线叶金雀花茶可在90℃、冲泡5 min条件下,冲泡2次;在此条件下,人体通过饮用线叶金雀花茶摄入过量钙、磷、铁、锌、铜、锰、砷、铅、镉元素的风险较低。鉴于矿物质元素摄入量的可获得性和可承受性,线叶金雀花茶能补充少量的矿物质元素,是一种良好的饮品原料。

微波消解-电感耦合等离子体原子发射光谱法测定硼铁中硅铝磷的含量

采用盐酸、硝酸和氢氟酸经微波消解样品,使用电感耦合等离子体原子发射光谱法(ICP-AES)对硼铁中硅、铝、磷的含量进行测定。方法确认了最佳微波消解条件,选择Si 288.158 nm、Al 394.401 nm、P 213.618 nm为分析谱线。干扰试验结果表明,在选定的分析谱线下样品中共存元素对待测元素的干扰可忽略。试验方法应用于硼铁实际样品中硅、铝、磷含量的测定,精密度试验测定结果的相对标准偏差(n=11)为1.77%~2.76%,加标回收率为96%~103%。按照该方法测定硼铁标准样品中硅、铝、磷的含量,测定值与认定值相吻合。

电感耦合等离子体原子发射光谱法测定锆合金中5种元素的含量

提出了电感耦合等离子体原子发射光谱法测定锆合金中锡、铌、铁、铬、镍含量的方法。取样品0.1 g,加入5 mL水、5 mL硝酸和0.5 mL氢氟酸,于100℃加热5 min,用水定容至25 mL。设置仪器射频功率为1300 W,雾化气流量为0.80 L·min^(-1),进样量为2.0 mL·min^(-1),测定5种元素在Sn 242.949 nm、Nb 309.418 nm、Fe 259.941 nm、Ni 221.648 nm、Cr 267.716 nm等分析谱线处的响应强度,基质匹配法定量。结果表明:锡、铌的质量浓度在150μg·mL^(-1)以内,铁、铬、镍的质量浓度在15μg·mL^(-1)以内分别与对应的响应强度呈线性关系;锡检出限(3s)为16μg·g^(-1),其他元素检出限(3s)均低于3.0μg·g^(-1);各元素方法重复性的相对标准偏差(n=10)均小于2.0%,加标回收率为99.0%~109%;采用锆合金标准物质SRM360b进行验证,测定值均在认定值的不确定度范围内。

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。

偏硼酸锂熔融-酒石酸络合-超声提取-电感耦合等离子体原子发射光谱法测定岩矿型锆矿石中10种元素的含量

为实现岩矿型锆矿石样品中锆、铪、钾、钙、钠、镁、铝、铁、钛、锰等10种元素含量的准确测定,优化了熔融、提取等试验条件,提出了题示方法。取干燥后的样品0.1 g于铂坩埚中,加入0.5 g偏硼酸锂,搅匀后盖上坩埚盖,于1 000℃熔融30 min。冷却后将铂坩埚置于装有25 mL含20 g·L^(-1)酒石酸的20%(体积分数)盐酸溶液中,超声振荡至熔块完全溶解,用水定容至100 mL,用电感耦合等离子体原子发射光谱仪测定。结果显示:上述10种元素的质量浓度分别在一定范围内与对应的谱线强度呈线性关系,检出限(3s)为1.90~40.8μg·g-1;方法用于由锆含量较低的基性岩岩石标准物质和锆精矿标准物质复配成的以锆石、斜锆石为主的岩矿型锆矿石样品的分析,测定值的相对误差为-1.9%~4.0%,测定值的相对标准偏差(n=12)为0.46%~4.5%,准确度和精密度试验结果的绝对值均优于DZ/T 0130.3-2006规定的控制指标,且方法可拓展应用于砂矿型锆矿石的准确测定。

电感耦合等离子体原子发射光谱法测定WC-Co硬质合金中铪元素含量

铪在硬质合金生产中,常作为添加剂以提高硬质合金的力学性能,故而硬质合金中铪含量的准确测定具有重要的意义。现存化学容量法测定硬质合金中铪,存在危险性较大、操作复杂、分析效率低等缺点。本文从样品前处理、分析线的选择、基质效应的探究等方面对硬质合金中铪的测定方法进行了探究,建立了电感耦合等离子体原子发射光谱法测定WC-Co硬质合金中铪含量,该方法具有安全、高效、操作简单、低成本等优点。在选定的条件下,选择体积比1∶1的硫酸、硫酸铵混合液结合柠檬酸和双氧水作为前处理溶剂,选择铪谱线264.141 nm作为分析谱线,利用基质匹配法配制标准溶液,方法校正曲线线性大于0.9999,线性范围为0.0~2.0μg/mL,检出限为0.0084μg/g,加标回收率为99.17%~103.63%,相对标准偏差RSD<0.758%。本方法为WC-Co硬质合金中铪含量的检测提供了可行性方法。

锗元素测定方法综述

锗在国防工业、航空航天和通信等领域中具有战略性意义,锗含量的测定对于保证材料质量和满足国际标准至关重要。对锗含量测定方法的多种技术进行了综述,包括分光光度法、原子荧光光谱法、原子吸收光谱法、电感耦合等离子体原子发射光谱法、电感耦合等离子体质谱法以及滴定法等。在每种检测方法的介绍中,详细探讨了方法的原理、前处理步骤以及应用范围,并分别总结了各方法的优势和不足。最后,强调了锗含量测定方法的意义,特别是在满足出口监管和促进科学研究方面的作用。同时对锗元素的测定方法进行了展望,为未来的发展提供了参考方向。