电感耦合等离子体原子发射光谱法(ICP-AES)测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K,Na,Ca,Mg,Zn,Fe,Cu,Mn,Se,Pb,Cd和Cr 12种元素。结果表明:方法简便、快速、准确;山药富含对人体有益的K,Ca,Fe,Mg,Zn,Mn,Se等矿物质元素,其肉质中重金属元素Pb,Cd,Cr含量均未超过国家食品卫生标准。     

微波消解/ICP—AES法测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K、Na、Ca、Mg、Zn、Fe、Cu、Mn、Se、Pb、Cd和Cr等12种元素。结果表明：方法简便、快速、准确度高;四种山药均富含对人体有益的K、Ca、Fe、Mg、Zn、Mn、Se等矿物质元素,其肉质中Pb、Cd、Cr含量均未超过国家食品卫生标准。     

微波消解ICP-MS测定海洋沉积物中微量元素

采用微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定海洋沉积物中的Cr、Co、Ni、Cu、Zn、Cd、Pb7种微量元素。对微波消解酸体系和微波程序进行了优化,结果表明:由4 mL HNO3与2 mL HF组成的混合酸对沉积物消解效果好;阶段升温,最高温度200℃,消解30 min有着最佳的消解效果。采用本实验方法对7种不同类型的海洋沉积物标准物质进行了测定,测定结果与标准值一致。各元素的检出限在0.009~0.17 ng/g之间。该方法快速简便、准确度高,可用于海洋沉积物样品中多元素同时测定。     

半密闭酸溶-电感耦合等离子体质谱（ICP-MS)）法测定化探样品中的铬镍铜锌镉铅6种重金属

采用半密闭酸溶消解法处理样品，选择离线校正的方式校正了Sn对Cd的同量异位素的干扰，增加积分时间和读数次数提高了Cd的准确度和精密度，建立了电感耦合等离子体质谱仪（ICP-MS）测定化探样品中Cr、Ni、Cu、Zn、Cd、Pb六种重金属元素的方法。对前处理方法和仪器的参数条件进行了优化，结果表明，半密闭体系可达到回流的目的，样品分解完全且无污染现象，在最优的实验条件下，标准曲线的相关系数均不小于0.9997，检出限为0.019~1.65 μg/g ，测定下限为0.057~4.95 μg/g 。按照实验方法对岩石、水系沉积物和土壤国家标准物质中Cr、Ni、Cu、Zn、Cd、Pb平行测定12次，各元素的测定结果与认定值基本一致，相对偏差均不大于3.55%，相对误差均不大于 10.34% 。采用实验方法对土壤样品进行分析，测定结果与四酸溶解-ICP-OES测定Cr、Ni、Cu、Zn、Pb，火焰-石墨炉原子吸收法测定Cd的结果基本吻合。     

原子吸收光谱法测定莲子和莲子心中7种金属元素含量

利用火焰原子吸收光谱法测定6种不同产地的湘莲莲子和莲子心中7种金属元素含量. 莲子和莲子心样品经粉碎干燥后, 用硝酸-高氯酸混合液进行消解处理,采用火焰原子吸收光谱法测定样品中Cr、Cu、Zn、Fe、Mn、Pb、Cd的含量. 莲子和莲子心中富含微量元素Fe、Mn、Zn、Cu、Cr,有害金属元素Pb和Cd未检出. 各元素的加标回收率为98.58%~101.53%,RSD在0.78%~1.89%之间. 方法快速、简便、灵敏,结果准确可靠,为莲子和莲子心中金属元素含量测定提供了一种可靠的方法.     

定南县废弃稀土矿区优势植物中5种重金属元素含量的测定

目的通过对赣南定南县某废弃稀土矿区生长的植物样品中5种重金属元素Cu、Mn、Cd、Pb和Cr的含量进行测定。方法采用火焰原子吸收分光光度法测定样品中Cu、Mn、Cd含量,采用石墨炉原子吸收分光光度法测定了样品中Pb和Cr的含量。结果在植物样品中,Mn含量最高的是芒萁(1 081.305 mg/kg);含Cd最高的是山鸡椒(0.716 mg/kg),Pb、Cu、Cr的含量未超过植物正常值。结论山鸡椒和芒萁可分别作为废弃稀土矿区Mn和Cd元素理想的植物修复备选植物。     

电感耦合等离子体原子发射光谱法测定新疆洋葱籽中常量/微量元素

采用微波消解法处理样品,以电感耦合等离子体原子发射光谱法(ICP-AES)测定新疆洋葱籽样品中Co、Cr、Ca、K、Mg、P、Fe、Mn、Na、Ni、Sn、Zn、Cd、As、Se、Cu、Mo和V 18种常量/微量元素。结果显示,新疆洋葱籽中含有丰富的K、Mg、P、Ca和Na等常量元素,此外微量元素Fe、Mn、Zn、Cr、Ni、Cu的含量也较丰富。新疆洋葱籽中含有很多对人体有益的常量及微量元素,有较高的药用价值。     

快速消解-电感耦合等离子体发射光谱测定林地土壤中9种金属元素

建立了测定林地土壤中9种金属元素(Ba、Cu、Co、Cr、Mn、Ni、Pb、V、Zn)的快速消解-电感耦合等离子体发射光谱法。采用聚丙烯管作为消解容器,优化了酸使用量和消解时间,在0.1 g称样量的情况下,加入4 mL王水和0.3 mL HF,消解温度为125℃,消解时间为90 min,赶酸时间为20 min,消解液采用电感耦合等离子体发射光谱仪测定。采用优化后方法对8种不同类型标准土壤样品进行测试,其测定值与与标准值一致。同时采用该方法与环保部标准前处理方法进行实际林地土壤样品的比较验证发现:两种方法无显著性差异(P0.05)。相比于现行标准方法,此消解方法用酸量少,操作简单,设备投入小,实验效率高,适合批量土壤样品中的金属元素分析。     

微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定畜禽粪便中7种重金属元素

粪便样品干燥、研磨后,称取0.25 g样品,加入8 mL硝酸,采用微波消解方法进行前处理.采用KED模式消除质谱干扰,采用内标校正消除非质谱干扰(Ge作为Cu、Zn、Cr的内标,Bi作为Hg和Pb的内标,Rh作为As和Cd的内标),建立了可同时测定畜禽粪便中Cu、Zn、Cr、As、Cd、Pb、Hg 7种重金属元素的微波...     

微波消解/ICP-AES法测定污水处理厂污泥中的重金属

采用微波消解/电感耦合等离子发射光谱法(ICP-AES)测定了城市污水处理厂污泥中Cd、Cr、Cu、Mn、Mo、Ni、Pb、Zn等8种重金属元素,并优化了ICP仪器工作参数及微波消解条件.方法的检出限为0.001～0.01mg/L.相对标准偏差为2.0%～9.2%(n=7),回收率为85.3%～105.0%.     

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.     

Direct determination of toxic trace metals in honey and sugars using inductively coupled plasma atomic emission spectrometry

A rapid method for the determination of Pb, Cd, Cu, Cr, Co, Ni, Mn and Zn in honey and sugars without prior digestion or ashing of the sample was developed, using inductively coupled plasma atomic emission spectrometry (ICP-AES). The critical instrumental parameters such as sample flow rate and radio frequency incident power were thoroughly optimized. The effect of matrix type and its concentration was also examined for glucose/fructose, sucrose and honey matrices. The sensitivity was investigated using calibration curves obtained in presence of the above matrices. The obtained recoveries for Cd, Cu, Cr, Co, Ni and Mn at the μg l⁻¹ level were satisfactory and practically independent of the matrix used for the calibration standards. The recoveries of Pb and Zn were less sufficient. Various commercial samples of honey, sugar, glucose and fructose were analyzed with respect to their toxic metal content. The method can be applied for routine analysis, quality and environmental pollution control purposes at the μg l⁻¹ level of concentration, after suitable dilution of the samples.     

Determination of trace elements by inductively coupled plasma mass spectrometry of biomass and fuel oil reference materials using milligram sample sizes

Most of the analytical techniques used to quantify elements associated with solid samples suffer from high detection limits and cannot be used for trace elements in biomass samples, particularly when only 20 mg are available for analysis. Inductively coupled plasma mass spectrometry (ICP-MS) can achieve detection limits of parts-per-trillion with liquid sample introduction by solution nebulisation. This technique was therefore tested with two standard biomass reference materials: oriental tobacco leaves and cabbage leaves. Two preparations successfully used on coal standards were used to digest the solid samples: a total digestion method (wet ashing digestion) and a partial leaching (microwave extraction). The concentrations of up to seventeen elements (As, Ba, Be, Cd, Co, Cr, Cu, Ga, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn) were measured after the two preparations. The accuracy and sensitivity of the measurements improved when the dilution factor decreased from 5000 to 1000 and to 500. Since the proportion of mineral matter in biomass samples is small (5%), the microwave digestion extracted elements that are generally not completely extracted from coal samples (e.g. Sb). However, some trace element concentrations were below the limit of quantification after microwave extraction, even with a reduced dilution factor (As, Se and Mo) and could not be quantified. A fuel oil was also digested. The trace element concentrations were very low (between 28 and 0.1 microgram g(-1)) but acceptable results were obtained by applying a dilution factor of 100. Only six elements in the fuel oil (As, Ba, Co, Ni, Se and V) had certified or indicated values. Factors affecting the accuracy and sensitivity of the analyses are discussed. The reproducibility of analysis of the tobacco leaf standard was checked over a period of nine months by both digestion methods. The wet ashing method gave acceptable reproducibility for Ba, Cd, Co, Cu, Ga, Mn, Mo, Ni, Pb, V and Zn but poor precision for Cr, Se and Sn and showed evidence of residual chloride interference for As. The microwave extraction gave good reproducibility for As, Ba, Cd, Co, Cr, Cu, Mo, Ni and Zn but poor precision for Se and low recoveries for Ga, Mn, Sn and V. In spite of the small quantities of material analysed, it proved possible to determine the trace elements at levels down to 0.1 microgram g(-1) in the reference materials.     

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.     

Determination of calcium, potassium, manganese, iron, copper and zinc levels in representative samples of two onion cultivars using total reflection X-ray fluorescence and ultrasound extraction procedure

The chemical characterization of onion cultivar samples is an important tool for the enhancement of their productivity due to the fact that chemical composition is closed related to the quality of the products. A new sample preparation procedure for elemental characterization is proposed, involving the acid extraction of the analytes from crude samples by means of an ultrasonic bath, avoiding the required digestion of samples in vegetable tissue analysis. The technique of total reflection X-ray fluorescence (TXRF) was successfully applied for the simultaneous determination of the elements Ca, K, Mn, Fe, Cu and Zn. The procedure was compared with the wet ashing and dry ashing procedures for all the elements using multivariate analysis and the Scheffé test. The technique of flame atomic absorption spectrometry (FAAS) was employed for comparison purposes and accuracy evaluation of the proposed analysis method. A good agreement between the two techniques was found when using the dry ashing and ultrasound leaching procedures. The levels of each element found for representative samples of two onion cultivars (Yellow Granex PRR 502 and 438 Granex) were also compared by the same method. Levels of K, Mn and Zn were significantly higher in the 438 Granex cultivar, while levels of Ca, Fe and Cu were significantly higher in the Yellow Granex PRR 502 cultivar.     

Trace element analysis in CRM of plant origin by inductively coupled plasma mass spectrometry

Three CRMs of plant origin (SRM 1515 Apple Leaves, SRM 1570a Trace Elements in Spinach Leaves, and SRM 1575 Pine Needles) were used for analytical quality assurance of Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Mo, Cd, and Pb determination by ICP-MS. The samples were decomposed using microwave assisted pressurized digestion by HNO₃ and HNO₃ + H₂O₂ mixture and temperature programmed dry ashing. Concentrations of elements in samples were evaluated by external calibration. All samples, blanks, and standards were spiked to 100 μg/L concentration of In and Bi as internal standards. During the measurement, signals of ⁵²Cr, ⁵³Cr, ⁵⁴Fe, ⁵⁵Mn, ⁵⁹Co, ⁶⁰Ni, ⁶²Ni, ⁶³Cu, ⁶⁵Cu, ⁶⁶Zn, ⁹⁵Mo, ¹¹¹Cd, ¹¹²Cd, ¹¹⁵In, ²⁰⁶Pb, ²⁰⁷Pb, ²⁰⁸Pb and ²⁰⁹Bi were monitored. Results of Pb, Cd, Cu, Zn, Mo and Co determination were in good agreement with certified values. In order to obtain accurate results for As at low levels, it was necessary to mathematically correct the analytical signal. This correction effectively eliminates the influence of interfering ArCl⁺ ions. For Cr analysis it is advisable to use as powerful oxidizing conditions during sample decomposition as possible.     

糙米、胚芽米、精白米中多种矿质元素和B族维生素含量的比较研究

对产自黑龙江省绥化市的同一批粳稻分别进行加工制得糙米、胚芽米和精白米,经过干灰化法或微波消解处理后,采用电感耦合等离子体发射光谱法（ICP—OES）、原子吸收光谱法（AAS）和原子荧光光谱法（AFS）测定了其中Al、As、B、Ba、Ca、Cd、Co、cr、Cu、Fe、Hg、K、Mg、Mn、Mo、Na、Ni、P、Pb、Rb、S、Se和zn共23种矿质元素的含量,,并采用高效液相色谱法（HPLC）和荧光分光光度法测定了其中维生素B．,烟酸,烟酰胺,维生素B。和维生素B：的含量。另外,还研究了经水淘洗后这3种类型大米中矿质元素和B族维生素含量的损失情况。结果表明,矿质元素和B族维生素含量呈现糙米,胚芽米,精白米由高到低的基本特征,淘洗可使各种矿质元素和B族维生素产生不同程度的损失,其中精白米中维生素B．经水淘洗后已损失殆尽。3种类型大米中cd、Cu、Mo、Ni、S、Se、Zn等元素含量差异相对较小,并且淘洗对Mo、S元素含量几乎没有影响,而cd、cu元素含量经水淘洗后反而略有增加。     

全反式维甲酸治疗动脉粥样硬化兔肝脏微量元素含量的变化

目的探讨实验性动脉粥样硬化兔肝脏组织中zn、Fe、Cu、Mn和cr、Pb、cd含量的变化。方法用高脂饮食复制兔动脉粥样硬化模型,然后给予全反式维甲酸建立治疗组模型,获取肝脏,用硝酸、过氧化氢混合液微波消解样品,采用原子吸收光谱法测定肝脏组织中zn、Fe、Cu、Mn和Cr、Pb、cd的含量。结果高脂组肝脏组织zn、Fe、Cu、Mn和cr、Pb、cd含量分别为86．09、277．1、11．07、5．366mg／kg和115．2、286．0、210．5μg／／kg,治疗组肝脏组织zn、Fe、Cu、Mn和cr、Pb、cd含量分别为135．3、347．7、10．72、7．218mg／kg和137．3、209．4、250．2μg／kg。结论经过维甲酸治疗后,zn、Fe、Mn、Cr含量明显提高,基本达到正常组水平。