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.

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.

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.

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.

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.

Enhancement of thermophilic anaerobic digestion of thickened waste activated sludge by combined microwave and alkaline pretreatment

Pretreatment of thickened waste activated sludge （TWAS） by combined microwave and alkaline pretreatment （MAP） was studied to improve thermophilic anaerobic digestion efficiency. Uniform design was applied to determine the combination of target temperature （110-210°C）, microwave holding time （1-51 min）, and NaOH dose （0-2.5 g NaOH/g suspended solids （SS）） in terms of their effect on volatile suspended solids （VSS） solubilization. Maximum solubilization ratio （85.1%） of VSS was observed at 210°C with 0.2 g-NaOH/g-SS and 35 min holding time. The effects of 12 different pretreatment methods were investigated in 28 thermophilic batch reactors by monitoring cumulative methane production （CMP）. Improvements in methane production in the TWAS were directly related to the microwave and alkaline pretreatment of the sludge. The highest CMP was a 27% improvement over the control. In spite of the increase in soluble chemical oxygen demand concentration and the decrease in dewaterability of digested sludge, a semi-continuous thermophilic reactor fed with pretreated TWAS without neutralization （at 170~C with 1 min holding time and 0.05 g NaOH/g SS） was stable and functioned well, with volatile solid （VS） and total chemical oxygen demand （TCOD） reductions of 28% and 18%, respectively, which were higher than those of the control system. Additionally, methane yields （L@STP/g-CODaded, at standard temperature and pressure （STP） conditions of 0°C and 101.325 kPa） and （L@STP/g VSadad） increased by 17% and 13%, respectively, comoared to the control reactor.

Experimental continuous sludge microwave system to enhance dehydration ability and hydrogen production from anaerobic digestion of sludge

Dehydrating large amounts of sludge produced by sewage treatment plants is difficult.Microwave pretreatment can effectively and significantly improve the dewaterability and hydrogen production of sludge subjected to anaerobic digestion. The aim of this study was to investigate the effects of different microwave conditions on hydrogen production from anaerobic digestion and dewaterability of sludge. Based on an analysis of the electric field distribution, a spiral reactor was designed and a continuous microwave system was built to conduct intermittent and continuous experiments under different conditions. Settling Volume, Capillary Suction Time, particle size, and moisture content of the sludge were measured. The results show that sludge pretreatment in continuous experiments has equally remarkable dehydration performance as in intermittent experiments; the minimum moisture content was 77.29% in the intermittent experiment under a microwave power of 300 W and an exposure time of 60 sec, and that in the continuous experiment was 77.56% under a microwave power of 400 W and an exposure time of 60 sec.The peak measured by Differential Scanning Calorimeter appeared earliest under a microwave power of 600 W and an exposure time of 180 sec. The heat flux at the peak was 4.343 W/g, which is relatively small. This indicates that microwave pretreatment induced desirable effects. The maximum yield of hydrogen production was 7.967% under the conditions of microwave power of 500 W, exposure time of 120 sec, and water bath at 55℃. This research provides a theoretical and experimental basis for the development of a continuous microwave sludge-conditioning system.

Microwave assisted digestion followed by ICP-MS for determination of trace metals in atmospheric and lake ecosystem

The study of trace metals in the atmosphere and lake water is important due to their critical effects on humans, aquatic animals and the geochemical balance of ecosystems. The objective of this study was to investigate the concentration of trace metals in atmospheric and lake water samples during the rainy season （before and after precipitation） between November and December 2015. Typical methods of sample preparation for trace metal determination such as cloud point extraction, solid phase extraction and dispersive liquid- liquid micro-extraction are time-consuming and difficult to perform; therefore, there is a crucial need for development of more effective sample preparation procedure. A convection microwave assisted digestion procedure for extraction of trace metals was developed for use prior to inductively couple plasma-mass spectrometric determination. The result showed that metals like zinc （133.50-419.30 μg/m3） and aluminum （53.58-378.93 μg/m3） had higher concentrations in atmospheric samples as compared to lake samples before precipitation. On the other hand, the concentrations of zinc, aluminum, chromium and arsenic were significantly higher in lake samples after precipitation and lower in atmospheric samples. The relationship between physicochemical parameters （pH and turbidity） and heavy metal concentrations was investigated as well. Furthermore, enrichment factor analysis indicated that anthropogenic sources such as soil dust, biomass burning and fuel combustion influenced the metal concentrations in the atmosphere.

Biogas recovery from microwave heated sludge by anaerobic digestion

Biogas generated from sewage sludge,livestock waste,and food waste by anaerobic digestion is a valuable renewable energy resource.However,conventional anaerobic digestion is not an efficient process.A long hydraulic retention time and low biogas recovery rate hinder the applications of those resources.An effective pretreatment method to destroy sludge microbial cells has been one of the major concerns regarding improvement of the biogas production.This article focuses on the effects of microwave heating on sludge anaerobic digestion.Volatile suspended solid(VSS) and chemical organic demand solubilization of heated sludge were investigated.Microwave heating was found to be a rapid and efficient process for releasing organic substrates from sludge.The increase of organic dissolution ratio was not obvious when holding time was over 5 min with microwave heating.The effect of the VSS solubilization was primarily dependent on heating temperature.The highest value of VSS dissolving ratio,36.4%,was obtained at 170°C for 30 min.The COD dissolving ratio was about 25% at 170°C.Total organic carbon of treated sludge liquor was 1.98 and 2.73 g/L at 150°C and 170°C for 5 min,respectively.A biochemical methane potential(BMP) test of excess sludge and a mixture of primary and excess sludge demonstrated an increase in biogas production.The total biogas from microwave treated mixture sludge increased by 12.9% to 20.2% over control after 30 days of digestion.Biogas production was 11.1% to 25.9% higher for excess sludge than for untreated sludge.The VS removal ratios of mixture sludge and excess sludge were 12% and 11% higher,respectively,compared to the untreated sludge.

An Experimental Method for Effectively Digesting Geological Samples

The material composition of geological samples is very complicated. Generally, the method for accurately determining trace elements in geological samples needs to digest the solid samples into liquid state, which is convenient for inductively coupled plasma mass spectrometry. The previous digestion method takes a long time and the operation process is complicated. The Ultra CLAVE microwave digestion instrument was used to digest the geological samples. The types and dosages of the acid used for digestion and the optimal conditions for instrumental testing were published. The results show that this method has short processing time, small data error, safer operation and good digestion effect. This method is suitable for geological sample analysis.

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。