怀菊花中微量铁的测定

为探讨邻二氮菲分光光度法测定怀菊花中微量元素铁含量的可行性,怀菊花的药理功效、食用营养价值与微量元素含量可能存在的关系,根据铁离子与特定显色剂显色产生可见吸收,采用混合酸y（HNO3）：V（HClO4）=4＋1对怀菊花样品湿法消化处理,在pH2～9的溶液中试剂与铁生成稳定的橙色络合物,并用分光光度法测定了怀菊花中微量元素铁含量。结果表明,所选的怀菊花中铁含量303．9～337．9μg／g,加标回收率为90．2％～100．6％。分光光度法操作简便、干扰离子少,测量快速、结果准确度和灵敏度高,易推广和 普及使用。     

铁(Ⅲ)-邻苯三酚红-十六烷基三甲基溴化铵双波长分光光度法测定铁

<正>铁是人体必需的微量元素之一,对人体的代谢和生长发育具有重要的作用。因此准确分析铁含量具有重要意义。目前测定微量铁的方法有火焰原子吸收光谱法[1-2]、荧光法[3-4]和光度法[5-6]等。光度法因具有简便、灵敏、快速、仪器设备价兼等优点被广泛应用。双波长分光光度法测定铁已有报道[7],本工作采用铁(Ⅲ)-邻苯三酚红-十六烷基三甲基溴化铵(CTMAB)体系双波长分光光度法测定铁。1试验部分     

利用FAAS法测定利水渗湿类中草药中锌、铁、铜、锰含量

采用火焰原子吸收分光光度法（FAAS）测定了6种利水渗湿类中草药（茯苓、泽泻、苡仁、茵陈、猪苓、革解）中锌、铁、铜、锰4种微量元素的含量．采用浓的HNO3＋HClO4（4＋1,V/V）混合酸消解样品,对测定结果进行了准确度和精密度评价,其加标回收率在92．3％-109．0％之间,相对标准偏差（RSD）不大于2．31％．测定结果表明：6种中草药中都含有丰富的微量元素,其中Cu含量相对偏低．     

治疗脑血管疾病中成药中钙铁铬铅含量的测定

采用原子吸收分光光度法测定了十种治疗脑血管疾病的中成药中钙铁铬铅的含量。结果表明,该类中成药中微量元素铁的含量较高,微量元素铅含量较低,该结果为探讨钙铁铬铁元素与治疗脑血管疾病的中成药药效关系提供了有用的数据。     

不同方法提取菟丝子微量元素Fe，Mn和Mg的比较研究

为比较不同提取方法对菟丝子中微量元素含量的影响,采用酸式提取法、碱式提取法、沸水提取法及超声提取法对中药菟丝子中的微量元素进行提取,用原子吸收分光光度法测定了提取液中微量元素铁、锰和镁的含量并进行了比较。结果表明,4种提取方法对微量元素的溶出率由高到低顺序为：铁-酸提,超提,碱提,沸提;锰-酸提,超提,沸提,碱提。镁酸提,沸提,超提,碱提。     

电感耦合等离子体原子发射光谱法(ICP-OES)测定地下水中多种元素

应用电感耦合等离子体原子发射光谱法(ICP-OES)测定地下水中钾、钠、钙、镁、铁、锰元素的含量,使用分光光度法测定氟的含量,测定的相对标准偏差为0.7%~2.8%,加标回收率为92.1%~105.2%。结果表明,大部分地区地下水中钠和氟化物的含量均偏高,常量与微量元素的组成含量差别不大。     

海兴地区地下水中多元素含量的测定

应用电感耦和等离子体发射光谱(ICP-OES)法测定地下水中钾、钠、钙、镁、铁、锰的含量,使用分光光度法测定氟的含量,测定的相对标准偏差为0.7%-2.8%,回收率为92.1%-105.2%。结果表明,大部分地区地下水中钠和氟化物的含量均偏高,常量与微量元素的组成含量差别不大。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定地下水中多种元素

应用电感耦合等离子体原子发射光谱法(ICP-AES)测定地下水中钾、钠、钙、镁、铁、锰元素的含量,使用分光光度法测定氟的含量,测定的相对标准偏差为0.7%~2.8%,加标回收率为92.1%~105.2%。结果表明,大部分地区地下水中钠和氟化物的含量均偏高,常量与微量元素的组成含量差别不大。     

紫外-可见光分光光度法测定去铁胺的含量EI北大核心CSCD

建立了紫外-可见光分光光度法测定去铁胺含量的方法。去铁胺在HAc-NAc缓冲溶液中,与Fe(II)发生显色反应,采用紫外-可见光分光光度法测定其含量。结果表明,去铁胺在0.0897~0.8074 mg/m L范围内,呈现良好的线性关系,回归方程为Y=9.5714X-0.0069(R2=0.9988)。在供试液中分别添加去铁胺对照品0.1,0.2,0.3 mg/m L 3个水平添加下,平均回收率99.5%,相对标准偏差(RSD)为2.0%。方法可用于甲磺酸去铁胺制剂中去铁胺的质量控制。     

蒙药配方中常用药材的微量元素分析

本研究利用原子吸收分光光度法测定了蒙药配方中14种常用药材的铜、铁、锌、硒四种必需微量元素的含量。     

Trace analysis of high-purity iron by total reflection X-ray fluorescence spectrometry

Summary A combined procedure enabling simultaneous multielement analysis of trace impurities in high-purity iron is presented. After removal of the iron matrix by solvent extraction with methyl isobutyl ketone, the trace elements Ti, V, Cr, Mn, Ni, Cu, Pb and Bi are determined by means of total reflection X-ray fluorescence analysis. Detection limits are found in the range of 100 ng/g. The reliability of the method is verified by the analysis of commercial high-purity iron and by the comparison of analytical data obtained by ICP-AES.     

Solvent extraction with ammonium pyrrolidinedithiocarbamate and 2,6-dimethyl-4-heptanone for the determination of trace metals in effluents and natural waters

A method is described for the determination of ten trace metals (V, Cr, Fe, Co, Ni, Cu, Zn, Mo, Cd, Pb) in aqueous samples by simultaneous solvent extraction followed by flame atomic absorption spectrometry. 2,6-DimethyI-4-heptanone is preferred to 4-methyl-2-pentanone as the solvent, and ammonium pyrrolidinedithiocarbamate to sodium diethyl-dithiocarbamate as the extractant except when relatively large amounts of iron are present. Calibration graphs are linear, usually over the range 0–50 μg l^-1. The effects of interfering substances, in particular iron, are shown, and the need for calibration by standard additions is demonstrated. The general need for preoxidation of samples is discussed.     

Notiz zur Bestimmung von Spurenelementen in organischen Eisensalzen

Zusammenfassung Es wird ein Verfahren zur Bestimmung von Spurenelementen in organischen Eisensalzen mitgeteilt. Nach Oxydation der organischen Anteile mit Salpetersäure und Vanadium(V) als Oxydationskatalysator wird das Eisen mit Hydrazin reduziert. Cu, Pb, Ni und Zn werden kathodenstrahlpolarographisch, Mn wird photometrisch bestimmt. Die Nachweisgrenzen der Verfahren liegen bei 10^–4%.

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Summary A method is described for determining trace elements in organic iron salts. After oxidation of the organic content by wet decomposition using nitric acid and vanadium(V) as a catalyst, iron is reduced with hydrazine. Cu, Pb, Ni, and Zn are determined by cathode-ray polarography, Mn by photometry. Traces are detectable down to 10^–4%.

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Herrn Prof. Dr. C. Mahr zum 65. Geburtstag gewidmet.     

Determination of trace amounts of vanadium with a new reagent [1-(3-methoxysalicylidene-amino)-8-hydroxy-3,6-naphthalene disulfonic acid, disodium salt] by fluorescence quenching method

A fluorescence quenching method is described for the determination of trace amounts of vanadium(V) based on the formation of a complex in acidic medium with a new reagent [1(3-methoxysalicylideneamino)-8-hydroxy-3,6-naphthalene disulfonic acid, disodium salt]. The fluorescence emission is measured at 415 nm (wavelength of excitation 360 nm), and the experimental variables and interferences in this determination have been studied. The detection limit is 12.5 ng/ml and linear range is between 50 and 600 ng/ml. The method has been applied to determine trace vanadium(V) in steel and cast iron.     

Separation and determination of trace amounts of aluminium(III), vanadium(V), iron(III), copper(II) and nickel(II) with CALKS and PAR by RP-HPLC.

An RP-HPLC method for the separation and determination of aluminium(III), vanadium(V), iron(III), copper(II) and nickel(II) with CALKS (Chromazol KS) and PAR ([4-(2-pyridylazo)resorcinol]) chelating on a YWG-ODS column was developed. A mixture of methanol-tetrahydrofuran(THF)-water (60:5:35 v/v) containing 0.2 mol/L LiCl, 5 x 10(-5) mol/L CALKS, 5 x 10(-5) mol/L PAR and acetate buffer solution (pH 4.9) was selected as mobile phase. The method has high sensitivity, with the detection limits being 6 ng/mL for aluminium(III), 3.5 ng/mL for vanadium(V), 10.4 ng/mL for iron(III), 6.3 ng/mL for copper(II) and 8.7 ng/mL for nickel(II). It also has good selectivity, so that most foreign metal ions do not interfere under the optimum conditions. The method can be applied to the simultaneous determination of trace amounts of aluminium, vanadium, iron, copper and nickel in rice and flour samples.     

On the reactivity of mononuclear iron(V)oxo complexes

Ferric tetraamido macrocyclic ligand (TAML)-based catalysts [Fe{C(6)H(4)-1,2-(NCOCMe(2)NCO)(2)CR(2)}(OH(2))]PPh(4) [1; R = Me (a), Et (b)] are oxidized by m-chloroperoxybenzoic acid at -40 °C in acetonitrile containing trace water in two steps to form Fe(V)oxo complexes (2a,b). These uniquely authenticated Fe(V)(O) species comproportionate with the Fe(III) starting materials 1a,b to give μ-oxo-(Fe(IV))(2) dimers. The comproportionation of 1a-2a is faster and that of 1b-2b is slower than the oxidation by 2a,b of sulfides (p-XC(6)H(4)SMe) to sulfoxides, highlighting a remarkable steric control of the dynamics. Sulfide oxidation follows saturation kinetics in [p-XC(6)H(4)SMe] with electron-rich substrates (X = Me, H), but changes to linear kinetics with electron-poor substrates (X = Cl, CN) as the sulfide affinity for iron decreases. As the sulfide becomes less basic, the Fe(IV)/Fe(III) ratio at the end of reaction for 2b suggests a decreasing contribution of concerted oxygen-atom transfer (Fe(V) → Fe(III)) concomitant with increasing electron transfer oxidation (Fe(V) → Fe(IV)). Fe(V) is more reactive toward PhSMe than Fe(IV) by 4 orders of magnitude, a gap even larger than that known for peroxidase Compounds I and II. The findings reinforce prior work typecasting TAML activators as faithful peroxidase mimics.     

Distribution of trace and minor elements in hungarian spice paprika plants

Detailed investigations were carried out to study the distribution of trace and minor elements in different parts (fruit, seed and rib, peduncle, stem, leaf, root) of ripe Hungarian spice paprika plants. Two varieties of paprika plants were analyzed for their Cl, Co, Fe, K, Mg, Mn, Na, Rb, Sc, V and Zn content by non-destructive neutron activation analysis. The results showed that the iron contents of the samples were much higher than those of the other trace elements. For the trace elements Co, Fe, Mn, Sc, V and Zn a considerable enrichment was observed in the leaf, while the Rb and K, Na, Mg showed accumulation mainly in the peduncle. In the other parts (fruit, seed and rib, stem) of the paprika plants no significant enrichment of trace elements was found. Since some of the elements investigated may have been partially eluted during the cleaning of the roots with distilled water and, on the other hand, if the cleaning was not intensive enough, some soil particles could be retained on the samples, the data obtained for the roots should be considered with precaution.     

Determination of trace elements in iron by neutron-activation techniques

A systematic analytical procedure for the determination of some trace impurities in iron matrices was developed by employing both direct and destructive neutron-activation techniques. Irradiations in fast neutron fluxes, selective activation by epithermal neutrons and coincidence γ-spectrometry measurements were used in some cases, in order to improve the sensitivity for non-destructive analysis; for destructive methods, radiochemical separations based on ion exchange and solvent extraction were applied. Procedures are described, and some results of the determination of low concentrations of Al, Mn, Ti, V (non-destructive), P, S, Zn (destructive) and As, Co, Cr, Cu, Mo, Ni, Sc, W (both methods) in iron are reported and discussed.     

Adsorptive Preconcentration for Voltammetric Measurements of Trace Level of Iron (III) With 2- (2- Thiazolylazo)-4-Methylphenol

Abstract

This paper describes an electrochemical stripping procedure for ultratrace measurements of iron, in which preconcentration is achieved by the adsorption of a iron-[2-thiazolylazo)-4- methyl phenol] complex onto a static mercury drop electrode Cyclic voltammetry was used to characterize the interfaciai and redox behavior. For a 5 minute preconcentration time, the detection limit found was 1.8 × 10^?0mol/1. Optimum experimental conditions were found by the use of a stirred triethanolamine (pH 8.6) solution with 2-[2-thiazolylazo- 4- methyl phenol] concentration of 1.0 × 10^?5 mol/1, a preconcentration potential of ?0.46V and linear scan mode. With preconcentration for 30 sec., calibration plots for iron are linear for the 5–29 μ g/1 range. Possible interferences by masking agents and several trace ions have been investigated. The interference of copper and uranium are eliminated by addition of CyDTA and carbonate ion respectively. Simultaneous determination of iron with copper and nickel is possible. The merits of the aforementioned procedure are demonstrated in the analysis of fresh water.