微波消解与ICP-AES联用测定糖果以及蜜饯中滑石粉的含量

采用微波消解对样品快速消解,采用氢氟酸、硝酸与双氧水处理样品,使滑石粉中的镁转化成Mg2+。同时用ICP-AES(电感耦合等离子发射光谱法)测定样品中的滑石粉含量,Mg含量在0.5~5 mg/L范围内与光谱强度线性相关,线性相关系数为0.999 7。测定结果的相对标准偏差为4.87%~6.38%(n=6),回收率为93.3%~103.1%。     

微波消解ICP-AES法测定钼矿石中多种元素

建立了电感耦合等离子体发射光谱法同时测定钼矿石中钼、铜、铅、钨、钛、硫6中元素含量的分析方法。采用微波消解溶解样品,在选定的仪器工作条件下直接测定。通过试验确定了各元素的分析谱线,对试液的酸度进行了探讨。6种元素的检出限为0.042~0.612μg/ml,加标回收率为97.01%~101.59%,测定结果的相对标准偏差0.89%~3.56%(n=6).该方法灵敏度高,适用于钼矿石中多种元素的同时测定。     

ICP-AES法测定锂离子电池电解液中金属杂质元素

采用电感耦合等离子体发射光谱仪(ICP-AES)同时测定六氟磷酸锂电解液中钠、钾、钙、铁、铜、铬等多种元素,回收率在97.3%～104.1%之间,线性相关系数大于0.999,相对标准偏差在0.02%～0.66%。该方法分析速度快,灵敏度高,重现性好,适合六氟磷酸锂电解液中杂质元素的检测。     

微波消解-电感耦合等离子体发射光谱仪法同时测定藏香中7种重金属元素

对藏香多种重金属元素同时检测的方法较少研究.本文建立了微波消解-电感耦合等离子发射光谱仪(ICP-OES)法同时测定藏香中7种重金属元素(As、Cd、Cr、Cu、Hg、Ni、Pb)的方法.藏香样品在HNO3溶液中120℃加热30 min后采用程序升温在100、120、150、185℃下进行微波消解,消解后的溶液经ICP...     

微波消解-ICP-MS测定花草茶中金属元素含量

采用微波消解法对花草茶样品进行前处理,利用电感耦合等电子体质谱仪(ICP-MS)同时测定了样品中As、Cd、Cr、Pb、Sr、Mn、Cu、Zn等8种金属元素的含量。结果表明,采用微波消解-ICP-MS法的测得加标回收率为92.6~101.3%,实验结果满足检验要求,适用于花草茶中多种元素的同时快速确证检测。且该前处理方法相比干化法,检测时间更短,结果更准确。     

微波消解-电感耦合等离子体原子发射光谱法在铝合金多元素检测中的应用

本文建立了铝合金中多元素含量的微波消解-(ICP-AES)法来对铝合金中硅、锰、镁、铁、铜等9种元素含量进行检测。实验结果表明,本方法测定的各元素相对标准偏差(RSD)均小于2.0%,回收率在(96.08~102.50)%之间,方法灵敏度高,重现性好,能够满足实际样品检测要求。     

微波消解-电感耦合等离子体发射光谱法测定松茸中9种金属元素

建立松茸中钾、钠、铝、锰、锌、铜、铁、钙、镁的微波消解-电感耦合等离子体发射光谱法测定方法。样品采用3 mL硝酸和2 mL过氧化氢作为消化液,微波消解后,用电感耦合等离子体发射光谱法进行测定。结果表明:各元素线性范围为钠0～2.00μg/mL,钾0～100.00μg/mL,铝、锰、锌、铜、铁、钙、镁均为0～5.00μg/mL,平均回收率在94.14%～102.30%之间,相对标准偏差(RSD)为0.23%～3.21%范围,检出限为0.33～5.25 mg/kg,定量限为1.10～17.50 mg/kg。测得四川省6个主产区松茸中钾、钠、铝、锰、锌、铜、铁、钙、镁的含量范围分别为21～35 g/kg、42.1～117mg/kg, 183～1210mg/kg, 10.2～91.8mg/kg, 23.1～69.5mg/kg, 21.6～37.2mg/kg, 159～1174mg/kg, 51.2～349 mg/kg,441～740 mg/kg。该方法简便、快速、准确,适用于松茸中上述9种元素的同时测定。     

茶叶及茶汤中铝元素含量测定及浸出特性研究

采用微波消解-电感耦合等离子体发射光谱法测定茶叶及茶汤中铝元素含量。结果显示:相同品种茶叶间,铝含量存在差异;不同品种茶叶间,乌龙茶、红茶较绿茶、白茶,花茶铝含量高。铝含量的高低,不仅与品种、土壤环境及加工工艺有关,而且茶叶中铝含量的分布在成熟叶和老叶中居多,而嫩叶中相对含量较少;乌龙茶、红茶是用成熟叶和老叶制成,因此含量相对较高。通过冲泡时间及次数的测试发现,喝茶前洗茶很有必要,洗茶第一泡的时间10~30 min为宜。该研究对于茶叶质量控制及消费者合理购茶、科学饮茶具有参考价值。     

微波消解结合ICP-MS测定内衬纸和框架纸中7种元素

目的 基于高压密封微波消解技术,构建一种新型微波消解体系,并将其与电感耦合等离子体质谱(ICP-MS)联用,用于烟用内衬纸和框架纸中铬、镍、砷、硒、镉、汞和铅元素含量的测定.方法 在新的消解体系中,用氟化铵(NH4F)代替传统方法中的氢氟酸(HF),以降低对实验操作人员的危害,并考察不同实验条件对实验结果的影响.结果 最佳消解条件为0.2 g纸质样品在6 mL硝酸和0.5 mL NH4F体系中消解,微波消解程序为温度从室温升至185°C(20 min)保持30 min后降至55°C(20 min);7种元素的标准曲线线性良好(r2>0.9990),检出限低,加样回收率和重现性良好;在检测实际样品时,与传统方法相比,该方法的测定结果无显著性差异(P>0.05).结论 该方法快速准确、安全环保,适合于烟用内衬纸和框架纸中7种元素含量的测定.     

微波消解-电感耦合等离子体质谱法同时测定土壤样品中八种重金属元素

本文以Ge、In、Re内标校正体系,采用微波消解-电感耦合等离子体质谱（ICP—MS）对土壤样品中砷、铅、铜、锌、镉、铬、汞、镍八种重金属元素进行同时测定,通过加标回收试验,建立了土壤样品中砷、铅、铜、锌、镉、铬、汞、镍八种重金属元素ICP—MS分析方法,各元素检出限均小于1．0ng／mL,测定8种元素的相对标准偏差均小于10％,各元素的加标回收率在86．3％～101．0％。实验表明：该法操作简单、快速,灵敏度高,重现性好,而且能够对八种重金属元素进行同时测定,大大提高了检测效率。     

Optimization of an open-focused microwave oven digestion procedure for determination of metals in diesel oil by inductively coupled plasma optical emission spectrometry

This work reports the optimization of a focused microwave assisted procedure for the wet acid dissolution of diesel oil in order to allow the determination of metals in the samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The dissolution process was monitored by measuring residual carbon content (RCC), also by ICP-OES, in the final solutions obtained after application of digestion program. All experimental work was performed using a commercial sample of diesel oil containing 85.74+/-0.13% of carbon. The initial dissolution program comprised three steps: (i) carbonization with H(2)SO(4); (ii) oxidation with HNO(3) and (iii) final oxidation with H(2)O(2). During work it was verified that the first step played an important role on the dissolution process of this kind of sample. It is therefore, necessary to give a detailed optimization of such step. Employing the optimized conditions it was possible to digest 2.5 g of diesel oil with a 40 min-heating program. At these conditions, residual carbon content was always lower than 5%. Optimized methodology was applied in the determination of metals in three diesel oil samples by ICP-OES. Recovery tests were also performed by adding 10 microg of metals, as organic standards, to the samples before digestion. Recovery percentages always higher than 90% were obtained for the metals of interest (Al, Cu, Fe and Ni), except for Zn, which presented recoveries between 70 and 78%.     

氢化物发生电感耦合等离子体发射光谱法测定钢中微量砷

该文研究氢化物发生-电感耦合等离子体发射光谱法测定非合金钢(碳素钢)和低合金钢中微量砷的分析方法,考察高频功率、雾化压力、辅助气流量、泵速等仪器工作条件与消解用酸及用量、硼氢化钠浓度对光谱强度的影响,并讨论王水、铁基体、共存离子对测定结果的背景干扰与消除方法.确定的最佳工作条件为:高频功率为1350 W,雾化压力为22...     

电感耦合等离子体原子发射光谱法测定电解钴中杂质元素

金属钴试样经酸消解后,未经基体分离直接以全谱直读电感耦合等离子发射光谱仪测定其中杂质元素。确定了仪器的最佳工作条件,选择了合适的分析谱线,采用钇作为内标物质,补偿基体效应。方法测定各元素的检出限在0.0001～0.02mg.L-1范围内。方法用于样品的测定,相对标准偏差为1.5%～7.5%,回收率为94.0～104.0%,各元素的测定值与国家标准方法的测定值相符合。     

电感耦合等离子体发射光谱法测定矿石中银的研究

目前,实验室测定矿石中银的方法主要有银的光度法、火焰原子吸收光谱法、石墨炉原子吸收光谱法等等,为了更好的简化测量过程、提高工作效率,本文旨在建立更适宜的、能满足于高中低含量银的测试方法,采用电感耦合等离子体光谱法测定金属矿中银的含量.样品采用氢氟酸、硝酸、硫酸(体积比10∶5∶1)溶解,赶净氟和破坏有机物后,经(1+1...     

Determination of trace bismuth in human serum by cloud point extraction coupled flow injection inductively coupled plasma optical emission spectrometry

A cloud point extraction method for the preconcentration of ultra-trace bismuth in human serum prior to its determination by inductively coupled plasma optical emission spectrometry had been developed in this paper. The cloud point extraction method was based on the complex of Bi(III) with 8-hydroxyquinoline and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time were investigated in detail. An enrichment factor of 81 was obtained for the preconcentration of Bi(III) with 25 mL solution. Under the optimal conditions, the detection limit of Bi(III) is 0.12 μg L⁻¹. The relative standard deviation (n = 7) of determination was 2.3%, values of recovery of bismuth were from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination trace bismuth in human serum.     

微波辅助萃取-电感耦合等离子体质谱法检测食品中的硼砂

建立了一种应用微波辅助萃取-电感耦合等离子体质谱法检测食品中的硼砂的方法。以0.1 mol/L氨水来消除硼的记忆效应。硼含量在0～2.0μg/mL范围内线性关系良好,R=1.0000。硼砂检测限为2.0 ng/mL(σ=3),RSD小于5%,方法回收率为95.2%～103.4%。该法与GB/T21918-2008中的三种检测方法相比,具有操作简单、快速、试剂污染少的特点。可作为食品中硼砂含量的检测方法之一。     

采用电感耦合等离子体质谱测定化肥中微量Cr、Cd、As、Pb、Hg元素

采用电感耦合等离子体质谱法测定化肥中微量Cr、Cd、As、Pb、Hg元素。仪器经条件优化，以In为内标，样品的基体效应和仪器漂移能得到很好的补偿。微波消解和敞开酸溶两种样品处理方法比较可知，微波法具有更高的精密度和准确度。方法的标准加入回收率在85-120％，RSD％〈15％，误差完全符合GB18877-2002的规定，方法简便快速。     

Design, fabrication and performance evaluation of a 22-channel direct reading atomic emission spectrometer using inductively coupled plasma as a source of excitation

The indigenous design, fabrication and performance evaluation of a polychromator, using inductively coupled plasma (ICP) as a source of excitation, are described. A concave holographic grating is used as the dispersing element and a Paschen — Runge mount is chosen to focus the spectra over a wide range along the Rowland circle. Twenty-two exit slits, mounted along the circle, precisely correspond to the wavelengths used for determination of up to twenty elements present in the plasma. Radiations emerging from the exit slits are detected by photomultiplier tubes placed behind them. The photomultiplier signal is recorded by an electronic system consisting of an integrator and a PC-based data acquisition system. The performance of the spectrometer has been evaluated with an ICP excitation source. Synthetic standards in deionized water containing a mixture of twenty impurities have been analysed. Typical determination limits observed for elements range from sub-ppm to ppm levels. All the elements present as impurities can be detected simultaneously. It is also observed that each element has a different emitting region in the ICP flame for which the maximum signal to the background is obtained. The determination limits obtained corresponding to these zones are the lowest. A study of the sensitive emitting zones for several elements has been carried out and the results are demonstrated by photographs of the ICP flame. The study will help in achieving the minimum value of determination limit for an impurity element.     

ICP-AES法测定螺旋藻中的杂质元素铝

探讨用ICP-AES技术测定螺旋藻中杂质元素铝,并对共存元素光谱干扰及其消除进行研究,所建立的分析方法,快速、结果准确,有较好的精密度和准确度,适用于螺旋藻中铝的测定。     

A complete inorganic survey study to reveal and study sensitometric deviations in photographic AgX emulsions by inductively coupled plasma mass spectrometry

Abstract

Inductively coupled plasma mass spectrometry (ICP-MS) offers excellent possibilities for multi-element trace analysis of photographic silver halide emulsions. In the present study, an analytical method was developed for the simultaneous determination of essential elements, such as ruthenium, rhodium, iridium and gold, in small emulsion samples, both overall as well as on the crystal surface. Sample preparation was performed by dissolving the silver halide emulsion into a self-made acid fixer. In-house standard reference emulsion material was prepared to verify the accuracy and precision of the quantitative method. The final result is a quantitative method for the selected elements with a precision of typically 1 per cent or better with relative standard deviations of 0.1–2.0 per cent. Detection limits were in the range 0.01–0.03 μg/kg. Using the scanning mode option of the instrument, the complete mass spectrum can be generated. Overlays can be made of two mass spectra and used as ‘fingerprints’ to reveal sensitometric deviations. Hence elemental trends can be traced or anomalies pinpointed in large batches of samples.