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.

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.

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.

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.

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.

Study on the Generation of Ultra-Wideband (UWB) High Power Microwave

The experimental study of ultra-wideband (UWB) technology, its generation and on-line measurement are presented. An experimental repetitive UWB system is designed, manufactured, and tested. High-pressure spark gap switch and its components, as well as oil spark gap switch are studied experimentally on the system. Experimental results indicate that the system operates at a 200 pps repetitive rate with a stable performance. 100 MW peak power UWB pulses are obtained on the system. Fast-time response capacitive divider is designed and fabricated, allowing for an accurate measurement of the high power UWB signal. The main issues related to the design of the switch and the UWB signal online measurement are discussed.

Microwave Synthesis of Au Nanoparticles with the System of AuCl_4-CH_3CH_2OH

The Au nanoparticles has been prepared by microwave high-pressure procedure with alcohol as the reducing agent. The color of colloidal Au nanoparticles is blue-violet. The maximum absorption spectrum of colloidal Au is at 580 nm, and the resonance scattering peak is at 580 nm. Using this method, the colloidal Au of long-time stability can be prepared Simply and quickly.

The Effects of Microwave Pretreatment of Dairy Manure on Methane Production

This study was undertaken to evaluate the efficiency of a liquid-solids separation process and microwave pretreatment, as well as anaerobic biodegradability of microwave pretreated dairy manure. Liquid-solids separation of raw dairy manure resulted in solid and liquid fractions having different properties, with the solid fractions richer in total and volatile solids content and liquid fractions richer in nutrients and metal ions. Substantial amounts of soluble chemical oxygen demand and nutrients were released into the solution after the microwave treatment. The microwave pretreated dairy manure was also subjected to anaerobic digestion. The kinetic parameters of methane production potential, maximum methane production rate and lag time were determined using the modified Gompertz equation. Anaerobic digestion of liquid manure, without microwave treatment, outperformed the sets with microwave treatment. The microwave-treated liquid dairy manure, without acid addition had better results in terms of methane potential and methane production, than with acid addition. Thermophilic digestion exhibited a higher maximum methane production rate than that of mesophilic digestion, but lower methane yields. The microwave pretreatment of dairy manure resulted in high soluble chemical oxygen demand;however, methane yield was not increased.

微波消解-电感耦合等离子体质谱法同时测定有机肥料中9种有毒有害元素的含量

提出了微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定有机肥料中As、Cd、Co、Cr、Ni、Pb、Sb、Tl、V等9种有毒有害元素含量的方法。取0.10 g有机肥料样品于聚四氟乙烯微波消解罐中,以2.5 mL盐酸、7.5 mL硝酸和2.0 mL氢氟酸为混合酸进行微波消解。消解结束后,于140℃赶酸,然后加入1.0 mL 50%(体积分数)硝酸溶液,再用水定容至50 mL,摇匀,过滤,取滤液待测,在线加入混合内标溶液。结果表明:9种元素标准曲线的线性范围均为2~100μg·L^(-1),方法检出限(3s)为0.59~66.75μg·kg^(-1);按照标准加入法对典型有机肥料样品进行回收试验,9种元素测定值的相对标准偏差(n=7)为2.0%~3.5%,回收率为81.5%~112%。

微波消解-电感耦合等离子体质谱法测定有机肥中镉、砷、汞、铅、铬含量

采用电感耦合等离子体质谱法(ICP-MS)测定,比较湿法消解30 min,湿法消解至近干和微波消解等不同前处理方法对有机肥料中镉、砷、汞、铅、铬元素的提取效果,建立了一种基于ICP-MS测定有机肥料多种重金属元素含量的方法。结果表明:湿法消解至近干和微波消解法对有机肥多元素成分分析标准物质(RMH-F001)中5项重金属含量的测试结果均满足标准要求,方法定量值、标准值偏差分别低于6.3%、5.7%;硝酸/过氧化氢体系-微波消解处理下,样品结果稳定性最佳,相对标准偏差为0.8%~6.8%,相对偏差为1.1%~9.0%,相对相差为2.2%~18.0%,加标回收率为99.4%~102.9%。硝酸/过氧化氢体系-微波消解-ICP-MS法可作为有机肥中5项重金属统一化测定的常规方法。

常压密闭微波消解-电感耦合等离子体质谱法测定磷矿石中的稀土元素

磷矿石中的稀土元素测定方法主要使用电感耦合等离子体质谱法(ICP-MS),样品处理方式主要采用敞口混合酸溶和碱熔。传统的酸溶和碱熔处理矿石样品时间较长,试剂加入量大,操作过程较为繁琐,且易造成环境污染。微波消解直接向样品释放能量,工作效率高,且易挥发元素被保留在消化溶液中,防止挥发造成结果偏差及环境污染。本文采用微波消解对磷矿石进行处理,并在二次消解过程中加入饱和硼酸络合溶矿过程中产生的不溶物氟化钙,在线加入铑和铼双内标的方式,建立了ICP-MS测定磷矿石中15种稀土元素的方法。结果表明:二次消解过程中加入饱和硼酸能有效地络合沉淀,彻底溶解样品,经上机测定后15种稀土元素的相对标准偏差(RSD)在0.68%~4.52%之间,回收率在93.1%~106.6%之间,方法检出限为0.003~0.029μg/g。选取两个磷矿石样品,用本方法与混合酸(盐酸-硝酸-氢氟酸-硫酸)酸溶方法进行对比试验,相对标准偏差在-5.82%~5.99%之间,表明本方法测定稀土元素是有效可行的。对于样品的前处理方法,酸溶、碱熔和微波消解都有各自的特点,微波密封消解能避免一些能形成易挥发组分的损失并且外源性污染少。本方法拓展了测定磷矿石中稀土元素的样品前处理方法,操作性强,是对现行方法的有益补充。

原子吸收光谱法测定苦瓜中微量金属元素的含量

用微波消解法对苦瓜进行预处理,采用火焰原子吸收光谱法测定了苦瓜中钙、镁、铁、锌四种微量金属元素的含量。在最佳条件下测得苦瓜中各金属元素的含量分别为Ca:3843.50μg/g,Mg:2545.492μg/g,Fe:93.3415μg/g,Zn:77.685μg/g;RSD为0.19%~0.85%;检出限为0.0020μg·mL^(-1)~0.0703μg·mL^(-1);相关系数为0.9927~0.9997;加标回收率为94.60%~102.92%,此方法简单、快捷、经济、有效。

黑果枸杞中矿物元素溶出特性研究

黑果枸杞,茄科枸杞属,富含多种矿物质元素,这对人体生长发育有重要的生物学作用。黑果枸杞作为一种药食同源的物质,为了解其营养价值、指导健康食用及进一步功能开发,有必要分析矿物质溶出特性,并进行相关性分析。黑果枸杞样品制备以硝酸和过氧化氢为消解酸,微波消解仪制备消解液,以不同温度纯水浸提制备浸泡液,试验建立了电感耦合等离子体光谱法测定消解液和浸泡液中K、Na、Ca、Mg、Zn、Fe、Mn、Cu、Li、Sr十种矿物元素含量的实验方法,并进行了矿物元素溶出特性研究及相关性分析。在优化的光谱分析条件下,十种元素线性关系好(r>0.9995)、检出限低(<0.01 mg·L^(-1))、准确度高、精密度好。加标回收率在97.2%~101.8%之间,相对标准偏差小于1.99%。实验发现,黑果枸杞中矿物元素含量丰富,含量最高的是K,其次是Na、Ca、Mg,然后是Fe、Li和Sr,含量较低的是Mn、Zn、Cu。黑果枸杞中K/Na值大于8,属于典型的高钾低钠食品。Ca、Mg、Fe、Zn、Li、Sr、Mn、Cu也是人体中多种酶、激素和维生素中不可缺少的活性因子,是一种理想的食品。黑果枸杞浸泡液中,除Li与Ca、Zn、Fe之间,Mg与Zn之间关系不明显外,其余元素间呈显著正相关或极显著正相关。表明,各矿物质元素中不存在明显的拮抗作用。矿物质元素的溶出率与浸泡时间及提取温度有关。实验采用沸水和40℃纯水浸泡黑果枸杞样品,选取浸提时间5、10和20 min三个时间点研究提取温度及时间对溶出率的影响。十种元素中K、Na、Zn溶出率最高,可能是因为三种元素多以离子形式存在,容易提取。Ca、Mg、Sr、Mn、Cu含量差异大,溶出率相近,可能是价态相近,提取效率相近。Li溶出率受提取温度影响很大,沸水浸泡溶出率是40℃温水的的1.5~2倍,Fe在微量元素中含量最高,溶出率却最低,主要是由于Fe与蛋白质结合,不易萃取。试验数据可为健康食用黑果枸杞及进一步开发利用提供理论参考。

电感耦合等离子体质谱法测定平阴玫瑰中13种稀土元素

目的建立微波消解电感耦合等离子体质谱法(ICP-MS)测定玫瑰及其制品中13种稀土元素含量的分析方法。方法样品经微波消解后,以铑(^(103)Rh)、铟(^(115)In)、铼(^(185)Re)为内标元素通过在线方式加入,用ICP-MS进行定量测定。以两种国家认证的标准物质进行方法准确度验证。结果各稀土元素质量浓度在0.1~20µg/L范围内线性关系良好(r≥0.9996),检出限在0.072~0.258μg/kg之间,平均回收率在87%~116%之间,相对标准偏差(RSD)为0.8%~4.3%。对实际样品检测发现,玫瑰及其制品中13种稀土元素均有检出,其中铈(^(140)Ce)平均含量最高,镥(^(175)Lu)平均含量最低。结论该检测方法快速、准确、操作简便、灵敏度和回收率高,能够满足玫瑰及玫瑰制品中稀土元素的测定要求。