Determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn in red wine samples by inductively coupled plasma optical emission spectroscopy: Evaluation of preliminary sample treatments

A comparative study of sample treatment for removing the organic matter (mainly alcohol) to analyse red wine samples for metal content (Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn) from ICP-OES has been carried out. Thus, three procedures have been assayed before metal analysis: Dry ashing (DA), wet ashing (WA) and the removal of alcohol by evaporation (AR). The obtained results showed that the three methods lead to unbiased recoveries close to 100%. However, the uncertainty of AR method was about twice of the remainder ones. From practical considerations, the DA procedure was considered more suitable for determining metal elements in wine samples by ICP-OES.     

Comparison of partial digestion procedures for determination of Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, and Zn in milk by inductively coupled plasma-optical emission spectrometry

A fast procedure was developed for determination of Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, and Zn in milk samples. This procedure consisted of a partial digestion with hydrochloric acid on a hot plate. The results obtained were compared with 3 other digestion procedures (dry ashing and 2 microwave digestions). All the procedures showed similar precision levels, with coefficients of variation <10% for most analyzed elements. Accuracy was evaluated by using certified reference materials, and the values obtained were within the confidence intervals for these products. The results obtained were not considered statistically different. The partial digestion on a hot plate with HCl can be very practical for laboratories with relatively large numbers of sample analyses.     

Determination of thirteen common elements in food samples by inductively coupled plasma atomic emission spectrometry: comparison of five digestion methods

Five sample digestion procedures were evaluated for the determination of Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn in food samples by inductively coupled plasma atomic emission spectrometry. The 5 procedures include dry ashing at 500 degrees C, wet digestion with HNO3-HClO4, microwave digestion with HNO3, microwave digestion with HNO3-H2O2, and microwave digestion with HNO3-H2O2-HF. For microwave digestion with HNO3-H2O2-HF, silicon (IV) oxide was used to eliminate the excess HF, making it possible to determine total Al, B, and other common elements accurately and simultaneously. Seven National Institute of Standards and Technology standard reference materials (SRMs) were analyzed to compare the recovery of 13 elements with above digestion procedures. The results demonstrated that the microwave digestion procedure with HNO3-H2O2-HF yielded the best recoveries for all 13 elements in the selected SRMs. The determined concentrations of most elements were close for all 3 microwave digestion procedures with the exception of Al in oyster tissue, bovine liver, and spinach. Notably, the wet digestion with HNO3-HClO4 is the simplest and the most effective procedure for the selected elements except Al and B. Although there are several concerns with the dry ashing procedure, it might be a preferable procedure for those analyses where only nonvolatile elements are to be determined and the concentrations of the elements are low.     

Elements analysis of infant milk formula by ICP-OES: a comparison of pretreatment methods

Sample pretreatments are critical steps for achieving true and precise results in element analysis for infant milk formula. In this study, we made a comparative study of four pretreatment methods: dry ashing (DA), wet ashing (WA), microwave ashing (MA) and slurry dispersion analysis. Nine elements (Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn) were determined by inductively coupled plasma optical emission spectrometry. Infant formula (GBW08509) with certified values was used for assessment of trueness and precision. The data showed that all relative standard deviations (RSD) of the observed values were <15 %. In contrast to other pretreatment, results for MA had the lowest RSD (≤5 %) for all the elements. For Cu and Mn, there was no significant difference between measurement results and certified values in four pretreatments. But, after DA and WA the results for Ca, K, Na, P and Zn differed significantly from the certified values.     

The determination of eight elements in human liver tissue by flame atomic absorption spectrometry in sulphuric acid solution

A flame atomic-absorption spectrometric method is detailed for the determination of Ca, Mg, Zn, Fe, Cu, Mn, Rb and Cd in human liver tissue. Metal losses for three alternative sample destruction procedures are discussed; in the recommended procedure, low-temperature ashing in an oxygen plasma is followed by dissolution in sulphuric acid and aspiration into an air—acetylene flame. The necessity of close matching of the K, Na, phosphate and sulphuric acid contents for samples and standards is demonstrated for several elements. The accuracy of the method was established by using NBS SRM Bovine Liver and carefully prepared synthetic standards. The relative standard deviation is typically 5%, although variations in the blood content between portions of liver tissue lead to poorer precision for iron.     

Determination of mineral and trace element concentrations in pine needles by ICP-OES: evaluation of different sample pre-treatment methods

In the present study, the determination of mineral and trace elements (Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn) from pine needles using three sample pre-treatment methods followed by inductively coupled plasma optical emission spectrometry, was examined. Sample pre-treatment methods tested were microwave digestion, ultrasound-assisted digestion and dry ashing. The new ultrasound-assisted digestion method was optimised by the analysis of the standard reference material (SRM) 1575a (pine needles) sample. The speed of dry ashing method was significantly increased by ultrasound dissolution after ashing. All the ICP-OES measurements were performed in robust plasma conditions which were tested by measuring the Mg II 280.270 nm/Mg I 285.213 nm line intensity ratios. The microwave digestion resulted generally in slightly higher element concentrations than ultrasound-assisted digestion. B, Cu and Na resulted in such low concentrations that they could not be accurately determined by using the microwave digestion method. The t-tests found no significant differences between the certified and the determined element concentrations of the SRM 1575a using the dry ashing method followed with ultrasound dissolution.     

Multielemental Analysis of Camellia Oil by Microwave Dry Ashing and Inductively Coupled Plasma Mass Spectrometry

A simple and practical method is reported for the determination of Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, and Pb in camellia oil by inductively coupled plasma-mass spectrometry (ICP-MS). Camellia oil was treated using microwave dry ashing at 380 degree Celsius for carbonization and 550 degree Celsius for ashing in a 110 minute procedure. The operational conditions of the dynamic reaction cell with ammonia as the reaction gas were optimized to minimize interferences. The recoveries and the relative standard deviations of optimized method were between 85.6 and 98.4 percent and 1.1 and 5.5 percent, respectively. The detection limits for Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, and Pb were 31, 48, 0.6, 4, 22, 0.4, 0.6, 0.9, 3, and 1 micrograms per kilogram, respectively. The developed method has significant potential for the determination of metals in edible oils.     

Microwave muffle furnace assisted decomposition of vegetable samples for flame atomic spectrometric determination of Ca, Mg, K, Fe, Mn and Zn

Summary Calcium, magnesium, potassium, iron, manganese and zinc can be accurately determined in vegetable samples by flame atomic absorption and flame emission spectrophotometry after a previous dry ashing of the sample in a microwave muffle furnace. This treatment is carried out in 45 min using a new accessory developed by us to obtain high temperatures on a domestic microwave oven. Sample ashes, obtained in the muffle, are diluted with nitric acid and the obtained slurry is introduced directly into an air-C₂H₂ flame for the analysis of Fe, Mn, and Zn, or injected into a double-channel FIA manifold to determine Ca, Mg and K. The obtained results agree with those certified and also with those obtained by a previous dry ashing in a conventional muffle furnace and they are more precise for all the determined elements.Presented at the XXVII CSI in Bergen (Norway), June 1991     

不同产地杜仲叶中金属元素的含量及其变化趋势分析

采用火焰原子吸收光谱法测定了陕西杨凌、陕西安康和河南灵宝产杜仲叶中Fe、Cu、Mg、Ca、Mn、Zn 6种金属元素的含量,并对其含量的变化趋势进行了分析比较.结果表明,杜仲叶中含有丰富的人体必需金属元素,且不同产地来源的样品中金属元素的含量有明显差异,其中尤以Fe、Zn、Mn和Mg含量差异最大,Cu和Ca的差异不明显....     

野生中草药木贼中微量元素的测定

目的测定中草药木贼中微量元素的含量。方法用湿法消化及于法灰化两种方法处理样品并进行了比较,用火焰原子吸收法测定了中草药木贼中7种微量元素的含量。结果测定结果湿法的RSD在0．5％～3．0％,干法的RSD在0．5％-7．5％之间。结论湿法处理金属离子损失小,测量精密度更好。木贼中微量元素的含量由高到低顺序为：Mg,Fe,Mn,Zn,Cu,Ph,Ni。     

Improvement of X-ray fluorescence sensitivity by dry ashing method for elemental analysis of bee honey

Elements, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb, and Sr in bee honey samples were determined using an improved dry ashing (DA) method for XRF with Mo-secondary target (Mo-XRF). The sensitivity of the DA method was significantly improved in comparison to the wet ashing (WA) and the direct (D) methods. The limits of detection (LODs) obtained by DA (3.4–0.007 µg/g) method were better by an order of magnitude than those obtained by WA (34.0–0.120 µg/g) and D (61.2–0.270 µg/g) methods. Further improvements in the sensitivity of the DA-XRF were achieved by using a Cu-secondary target for the excitation of the elements of K, Ca, Ti, Cr, and Mn. In this instance, the LODs were in the range of 0.220–0.024 µg/g. The results of DA-XRF analysis revealed a very good accuracy with errors less than 7.1% and a precision with a relative standard deviation (RSD) better than ± 8.8%.The improved DA-XRF analysis was applied for the determination of the above mentioned elements in several Syrian bee honey samples. The results were comparable to those obtained by the atomic spectrometry method with correlation coefficients better than 0.9927.     

火焰原子吸收光谱法对中药拳参中六种无机元素含量的测定

采用浓硝酸微波消解法处理样品,利用火焰原子吸收光谱法对中药拳参中常量元素Ca、Mg及微量元素Fe、Cu、、Mn、Zn的含量进行了测定。结果表明,中药拳参中含有丰富的人体必需常量和微量元素,Ca、Mg、Fe、Cu、Zn、Mn的质量分数分别为10 662.860、1 961.242、144.557、9.778、10.166、2.314μg.g-1,各元素加样回收率在96.0%~102.0%之间。该法操作简单、结果准确,是中药拳参中无机元素检测的理想方法。     

Development and validation of routine analysis methods for the determination of essential, nonessential, and toxic minor and trace elements in cereal and cereal flour samples by inductively coupled plasma-atomic emission spectrometry

Various digestion procedures were carefully investigated and accurately evaluated with respect to their effect on the analysis of cereals and cereal flours. Multielement methods were selected and well developed for the determination of essential (Cr, Cu, Fe, Mg, Mn, and Zn), nonessential (Ag, Al, Ba, Bi, In, and Ga), and toxic (Cd and Pb) minor and trace elements by inductively coupled plasma-atomic emission spectrometry. Only Ag could be determined, either with aqueous standard or standard addition calibration methods, while the standard addition methods were more accurate for the determination of other elements. The recoveries were mostly within the range of 84.1-113% for the expected values of all analytes with respect to certified reference material NIST SRM 1586a (rice flour). The results proved that, for cereals and cereal flours, the use of H2O2 for wet digestion and HNO3 for dry ashing were not necessary. Linear regression analysis and Student's paired t-test were applied to evaluate the significant differences between different procedures and type of samples.     

九死还魂草中微量元素的分析

为测定九死还魂草中6种微量元素的含量,并给该检测提供科学方法,采用浓硝酸微波消解法处理样品,利用火焰原子吸收光谱法对九死还魂草中Ca、Mg、Fe、Cu、Mn、Zn 6种元素的含量进行了测定.结果表明,九死还魂草中含有丰富的微量元素,Ca、Mg、Fe、Cu、Zn、Mn的含量分别为3 012.421、1 911.325、1...     

Cadmium and other metals in Swedish wheat and rye flours: longitudinal study, 1983-1997.

Wheat flour (sifted), wheat bran, and rye flour were sampled annually in several different areas in Sweden for 15 consecutive years (1983-1997) for a total of 105, 90, and 30 samples, respectively. These samples were analyzed for their content of Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn by atomic absorption spectrophotometry with background correction after dry ashing at 450 degrees C. As part of the quality control procedures, an in-house reference material was analyzed in parallel to the samples to ensure reliability of the results. In addition, a certified reference material was analyzed to monitor accuracy of the results. The Cd level in wheat and rye flours (mean 0.029 and 0.017 mg/kg dry wt, respectively) correlated significantly with time (p < 0.05) in 2 phases, tending to increase during the first half of the period and decrease during the latter half. In wheat bran, Cd (mean 0.15 mg/kg) levels did not correlate significantly with time. In wheat flour, Cu, Mn, and Zn (means 1.7, 6.2, and 7.6 mg/kg, respectively) showed a significant linear increase (p < 0.05) in concentration over time. In rye flour, the levels of Cu, Fe, Mn, and Zn (means 3.8, 36, 30, and 28 mg/kg, respectively) all decreased significantly (p < 0.05) over time. Similarly, in wheat bran Cu (mean 14 mg/kg) increased and Pb (mean 0.027 mg/kg) decreased significantly (p < 0.05) over time, whereas Ni and Zn showed a significant curved correlation with time and peaked at about the middle of the measurement period.     

Determination of trace elements in plant materials by inductively coupled plasma optical emission spectrometry

The use of inductively coupled plasmas as spectrometric emission sources for the determination of Fe, Mn, Cu, Al, B and Zn in orchard leaves is investigated. The plasma is shown to be sufficiently sensitive for the direct determination of all of the above elements in solutions of the plant materials after a dry ashing procedure. Comparative values for the trace element concentrations by other analytical methods are given.     

高血压患者血清中八种金属元素的

通过对48名高血压患者和52名正常健康人进行血清中八种金属元素的检测,探讨了人体必需金属元素的含量变化是否与患高血压疾病有直接的关系。采用离心分离的方法处理样品,用火焰原子吸收分光光度法检测样品中钙、镁、钾、钠、锌、铜、铁和锰的水平含量。结果表明,患高血压组血清Na、Mg、Zn、Fe、Mn的水平含量均高于健康对照组,其中Na、Mn两组间比较差异显著（P＜0．05）,Zn、Fe两组间比较差异非常显著（P＜0．01）,Mg两组间比较差异无显著性（P＞0.05);患高血压组血清Na／K比值均高于健康对照组,Ca/Mg、Cu/Zn比值均低于健康对照组。检测的八种金属元素在人体内的含量多少与患高血压疾病有一定的关系。提示适当增补体内的Ca、K、Cu和Mg含量,减少Na的过多摄入,科学控制Zn、Fe、Mn的增加,注意体内Na/K、Ca/Mg和Cu/Zn比值的平衡关系,降低Na/K比,提高Cu/Zn比,补Ca的同时一定要注意适当补充Mg,保持体内各元素间的相互依赖关系,有利于高血压病的预防和治疗。     

用ICP研究鹿科动物骨质疏松症的微量元素特征

鹿科动物的骨质疏松症是近几年出现的一种疾病，它影响鹿的生长发育和繁殖，病重者死亡。我们采集梅花鹿和白唇鹿的毛，血样，用低温灰化方法和温法消解处理样品，用ＩＣＰ分析了毛，血清中微量元素的含量。病梅花鹿毛样中Ｍｇ，Ａｌ，Ｃａ，Ｔｉ，Ｆｅ，Ｃｕ，Ｚｎ的含量比正常组高，Ｔｉ，Ｃｕ，Ｚｎ的偏差率大于１５％，而Ｓｉ，Ｍｎ，Ｐ，Ｐ，Ａｇ，Ｂａ，Ｌａ，Ｃｅ，Ｐｂ比正常组低，Ｖ，Ａｇ，Ｂａ，Ｌａ，Ｃｅ，Ｐｂ存在...