Application of ICP-AES with Microwave Digestion to Detect Trace Elements in Oysters from Jiaozhou Bay,China

Using ICP-AES with microwave digestion, we determined the concentrations of 16 trace elements in oysters from six sampling points in Jiaozhou Bay.The distributions of the wholesome elements Zn, Fe and Mn, and heavy metals such as As,Cd,Hg and Pb were studied.The oysters collected are all rich in the wholesome trace elements,and the oysters from Licun River have the highest concentrations of the three wholesome trace elements.The concentrations of heavy metals in oysters from Licun River are the highest and those from Hongdao are the lowest. Compared with the domestic and foreign sea-areas,the heavy metal contents in the oysters from Jiaozhou Bay are less in amount than those from some developed countries, and more than those in Southeast China.This implies that the Jiaozhou Bay's oysters have been polluted by the environment to some extent.

Application of closed-vessel microwave digestion method for the determination of multi-elements in environmental samples by sequential ICP-AES

A closed-vessel microwave digestion method is described for the rapid dissolution of environmental samples such as foods, soils and sediments. Depending on the sample type, 0.1-0.2 g sample was decomposed with HNO3/H2O2 or HNO3 / H2O2/HF acid mixture in a PTFE digestion vessel by using microwave heating for 2-3 min at 500W of microwave power. The solution, or to which 0.5 g of boric acid was added, was diluted to 25-50 ml and directly determined by sequential ICP-AES. The accuracy of the procedure was validated by the analysis of six standard reference materials for 10 elements. Ail results were in a good agreements with the certified values.

Determination of Lead in Lime-preserved Egg by Microwave Digestion and Flame Atomic Absorption Spectroscopy

[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision departments. [Methods] The lead content in lime-preserved eggs was measured by the microwave digestion and flame atomic absorption spectroscopy. [Results] The method had a correlation coefficient of r2=0.998 in the injection concentration range of 0-4 mg/L. The detection limit of the method was 0.008 2 mg/kg. In the range of 0.2 to 1.0 mg/kg addition concentration, the recovery rate of the method was 92.5%-108.0%, and the relative standard deviation(RSD) was <5%. [Conclusions] This method is accurate and reliable, simple and efficient, and is suitable for the detection of lead in lime-preserved eggs.

Determination of Arsenic and Mercury in Soil by Microwave Digestion and Hidride GenerationAtomic Fluorescence Spectrometry

[Objective] The aim was to develop a rapid, simple method for determina- tion of arsenic and mercury in soil samples by atomic fluorescence spectrometry. [Method] The method for determination of As and Hg in soil by combined atomic fluorescence spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-80.0μg/L of As and 0-8.0 μg/L of Hg, and the detection limits of As and Hg was 0.036 μg/L and 0.015 μg/L, respectively. The precision for elevenfold determination of As at 40.0 ug/L level and Hg at 4.0μg/L level were 1.1% and 2.2%（RSD）, respectively. Recoveries of 103.0%-106.6% for As and 90.0%-95.0% for Hg were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of As and Hg in soil samples.

Determination of Chromium and Zinc in Soil by Microwave Digestion and Flame Atomic Absorption Spectrometry

[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by combined flame atomic absorption spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-0.8 mg/L for Cr and 0-0.8 mg/L for Zn, the detection limits of Cr and Zn was 0.0025 mg/L and 0.002 3 mg/L, respectively. Recoveries of 102.4%-103.2% for Cr and 97.7%-98.3% for Zn were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of Cr and Zn in soil samples.

Determination of Mg Content in Crayfishby Microwave Digestion-Flame Atomic Absorption Spectrometry

[Objective] This study was conducted to investigate the Mg level in cray- fish. [Method] Microwave digestion was applied to treat crayfish sample, Mg content in which was then determined by flame atomic absorption spectrometry, and recov- ery test and the determination of standards were also performed. [Result] This method was used for the detection of Mg in crayfish, obtaining satisfactory effect. The sample recoveries were in the range of 90.0%-110%, and the detection limit was 0.8 mg/kg. [Conclusion] The method is rapid, simple, accurate and reliable, worth extending.

超级微波消解-ICP-AES法测定铑粉中16种杂质元素

在高温高压条件下用盐酸-双氧水消解铑粉样品,采用电感耦合等离子体发射光谱仪(ICP-AES)测定其中16种杂质元素[1]。进行了光谱干扰研究、谱线选择、加标回收、精密度以及基体匹配比对试验。该方法简便、快速、准确,其测定范围为0.0005%~0.10%,RSD在1.88%~12.15%之间,加标回收率在92.0%~114.6%之间,不同方法结果对照数据吻合良好。该方法可满足铑粉中16种杂质元素的测定要求。

超级微波消解-ICP-AES法测定铑炭催化剂中铑含量

建立一种采用超级微波消解,ICP光谱法测定5%Rh/C催化剂中Rh含量的方法。通过单因素实验和正交优化,对称样量、酸体系、消解温度、消解时间等因素进行考察,确定最佳消解方法:约0.10 g试样在密闭消解罐中,以9 mL硝酸和1 mL过氧化氢为酸体系,240℃消解温度下保持40 min,经赶酸定容后,采用ICP-AES法测定溶液中的贵金属含量。该方法简便、快捷,消解试样完全且结果稳定,相对标准偏差小于1.0%。

微波消解-ICP-AES技术测定土壤中微重金属元素探究

本实验通过酸液辅助微波消解样品,联合电感耦合等离子-原子发射(ICP-AES)技术,分析测定了土壤样品中重金属元素Cr、Zn、Mn、Cu的含量。结果表明,土壤中Cr、Mn、Cu、Zn含量分别为62.47 mg·kg^(-1)、284.50 mg·kg^(-1)、47.07 mg·kg^(-1)、98.98 mg·kg^(-1),未超过农用地土壤污染风险管控值。实验表明,该方法用于分析测定复杂样品中的金属元素含量,具有操作简单、分析迅速、灵敏度高、准确度好、检测限低等优点,具有广泛的应用价值。

Microwave digestion method in environmental analysis

This paper introduced the history,equipment and mechanism of the microwave digestion method. This paper studied the optimization parameter of digestion conditions, such as acid and acid combination, digestion time and applied microwave power,particle size,and other factors.The analytical performance in environmental research and the modification of the microwave digestion method were also discussed.

Microwave Assisted Acid Digestion of Biomorphic Ceramic Obtained from Cedar Wood Infiltrated with ZrO2

This work proposes the use of experimental design for optimization of microwave-assisted digestion of bio- morphic ZrO2-ceramic. Cedar wood is used as template and it was infiltrated with ZrO2 via sol-gel process. XPS, SEM and XRD have been used to verify the effectiveness of the synthesis. The effects of different combination of acids in the digestion of this sample have been optimized taking as response the concentra- tion of several metallic ions measured by ICP-MS.

Determination of Palladium II in 5% Pd/BaSO₄by ICP-MS with Microwave Digestion, and UV-VIS Spectrophotometer

Determination palladiums have been reported 5% (w/w) Pd/BaSO4 known as Rosenmund Catalyst. The determination of palladium II known as Rosenmund Catalyst is always an expensive procedure usually involving procedures such as flame atomic absorption spectrophotometry, emission spectrometry, and many spectrophotometric methods. In this study, palladium II in 5% Pd/BaSO4, was synthesized and employed to develop an extractive UV-Visible Spectrophotometric, and an inductively coupled plasma mass spectrometry ICP/MS methods for the determination of palladium II. Specification for Pd is 4.85% to 5.10%;the result was 4.97% for the UV-Visible spectrophotometer and 4.90% for the ICP/MS. Both results meet the requirements.

Theoretical Research on the Import and Export of Iron Ore and Harmful Element Detection Method based on Microwave Digestion Inductively Coupled Plasma Mass Spectrometry Approach

In this paper, we conduct research on the import and export of iron ore and harmful element detection method based on microwave digestion inductively coupled plasma mass spectrometry approach. Our country gradually increased demand for iron ore, iron ore trade, in order to ensure that the quality of the iron ore and taste which must be tested for total iron content. At the same time it also increased the demand for iron ore, although China＇ s iron ore production has been greatly improved. Our proposed approach optimizes the traditional detection method which will be meaningful.

微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定含铜污泥中多种重金属

为了实现对含铜污泥中成分的准确测定,采用盐酸-硝酸-氢氟酸微波消解进行样品的前处理,消解后加入高氯酸置于电热板进行除碳并赶酸,采用微波消解和电感耦合等离子体原子发射光谱(ICP-AES)法相结合对含铜污泥中铅、锌、铬、镉、砷、镁、铝、锑进行同时测定。溶样效果理想,且有效避免了高温溶样对易挥发元素砷、锑的损失,整个过程安全、高效、无损。对含铜污泥的分解方法进行了合理选择,并对测定时的元素分析谱线及各测定元素间干扰情况等进行了讨论。方法的加标回收率在95.3%~107%,相对标准偏差(RSD)在0.31%~2.1%(n=7)。结果表明,方法准确度高,操作简单快捷,可同时测定多种元素,能满足批量测定含铜污泥中铅、锌、镍、铁、镉、铬、砷、锑含量的要求。

微波消解-ICP-AES法测定中药材乳香中的微量元素

用电感耦合等离子体发射光谱法(ICP-AES)测定中药材乳香中的微量元素。首先用微波溶样技术,以浓HNO_(3)作为消解剂对乳香样品进行预处理,然后测定了Al、As、Ba、Cd、K、Li、Mn、Ni、Pb、Se、Sr、Tl、Zn等13种微量元素的含量。元素加标回收率实验数据为94.0%~107.5%,分析数据可靠性高。该方法可用于树脂类中药材中微量元素的快速检测。

超级微波消解—ICP-AES法测定铱粉中16种杂质元素

本方法充分发挥超级微波仪消解过程简单、产率高、消耗成本低及酸用量少、引入的污染少、安全、环保的优点,将超级微波技术与ICP-AES相结合,建立了ICP-AES法测定铱粉中16种杂质元素的分析方法[1],选用盐酸和双氧水于聚四氟消解管(TFM管)溶解铱粉,避免了氯酸钾和石英管带来的盐类污染和硅污染,方法简便、快捷,填补了铱粉中硅元素分析的空白,能满足铱粉产品测定要求。

基于微波消解/ICP-AES法同时测定山药中无机营养元素

本研究建立了山药和山药皮中多种无机营养元素含量的电感耦合等离子体发射光谱(ICP-AES)分析方法,测定了山药和山药皮中Na、Mg、P、K、Ca、Mn、Fe、Cu、Zn、Se等无机营养元素的含量。结果表明,该方法简便,快速高效,准确性好,灵敏度高,能满足实际样品的分析需求。

微波消解-ICP-AES测定土壤中Pb、Cr、Ni、Cu、Zn等十个元素

提出一种微波消解-ICP-AES同时测定土壤中多种元素含量的方法。通过与传统四酸消解法比较,该方法具有周期短、试剂用量少等优点。试验结果表明:微波消解-ICP-AES测定土壤中多种元素加标回收率介于97%~102%之间,检出限较低、准确度与精密度均优于传统四酸消解法。ICP-AES测定具有线性范围宽,抗基体干扰能力强,多元素同步分析等优点。综合判断,微波消解-ICP-AES测定可以作为土壤中多元素含量分析的较好方法。

基于微波消解/ICP-AES法同时测定山药中无机营养元素

本研究采用ICP-AES法,测定了山药和山药皮中Na、Mg、P、K、Ca、Mn、Fe、Cu、Zn、Se等无机营养元素的含量。结果表明,此方法简便快速高效,准确性好,灵敏度高,各元素的回收率介于96.2%~104.5%之间,相对标准偏差低于4.25%,能够满足实际样品的分析需求。

微波消解-ICP-AES法测定化妆品中无机元素的研究Ⅰ.固体类化妆品中As,Pb,Cd,Sr,Cr,Bi和Se等的分析方法研究

本文用国产微波消解系统，研究了安全地，有效地消化固体类化妆品最佳酸体系，以及消解罐内压力，微波功率和消化时间等参数并研究了固体类化妆品中一些无机元素的分析方法，即溶样后用ＩＣＰ－ＡＥＳ法测定砷，铅，镉，铬，锶，铋，硒元素的含量。用该法测定化妆品国家一级标样相对误差０．７４％。