Simultaneous spectrofluorimetric determination of iron and manganese by a differential kinetic catalytic method

A kinetic method is presented for the simultaneous determination of iron(III) and manganese(II) based on the different reaction rates resulting from the catalytic effect of both metal ions on the oxidation of 2-hydroxybenzaldehyde thiosemicarbazone by hydrogen peroxide in an ammoniacal medium. The reaction is monitored spectrofluorimetrically at 440 nm and with excitation at 365 nm. Two sets of reaction conditions are established to maximize the effect of manganese compared to iron, and vice versa, and the data are evaluated from simultaneous equations. Mixtures of these metal ions at ng ml^?1 levels for iron/manganese ratios from 8:1 to 1:2 can be determined with an accuracy and precition of about 3% and 1%, respectively. The methods has been applied successfully to the determination of both metals in aluminium and copper alloys, beer, cheeses and soils.     

Heavy metal content of a medicinal moss tea for hypertension

The content of various heavy metals (arsenic, cadmium, chromium, copper, iron, lead, mercury, nickel, manganese and zinc) in the moss species Rhodobryum ontariense (Kindb.) Kindb. and its tea are presented in this study. Pursuant to the use of this tea in traditional Chinese medicine for hypertension, the aim of this study was to examine its safety in regard to the metals. All heavy metals were determined by adequate EPA methods. The concentrations of all metals for daily intake in its tea were below the safety levels for human consumption. These results indicate the importance of manganese in R. ontariense tea traditionally used for hypertension and other heart disorders.     

洛阳牡丹花中营养元素和有害元素含量分析

为了提供洛阳牡丹花能否作为蔬菜食用的科学依据,采用原子吸收法测定了洛阳红、胡红、凤丹3个品种的牡丹花中钙、铁、锰、锌、铜、铅、镉元素含量。结果表明,洛阳红、胡红、凤丹花中含有丰富的营养元素钙、锰、铁;金属元素铜、锌含量在国家食品卫生限量标准内,有害元素铅、镉含量超出了国家限量标准。从微量元素含量的角度来评价,食用洛阳红、胡红、凤丹牡丹花,存在对人体健康产生危害的风险。测定结果的RSD为0.07%～16.1%,精密度高,可靠。     

Differentiation of Spanish brandies according to their metal content

Eleven metals, namely, aluminium, calcium, cadmium, copper, iron, lead, magnesium, manganese, potassium, sodium and zinc were determined in twenty samples of Sherry brandies and twelve samples of Penedés brandies by applying atomic spectrometry techniques. Flame atomic absorption spectrometry was used for quantitating calcium, copper, iron, magnesium, manganese and zinc; atomic emission spectrometry to determine potassium and sodium; and graphite furnace atomic absorption spectrometry to analyse aluminium, cadmium and lead. A chemometric approach was followed to study the discrimination between brandies from Sherry or Penedés according to the metal profile.     

The application of 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane to the extraction of metal ions

The use of 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane (Tet) in chloroform solutions provides quantitative extraction of lead(II), cadmium(II), copper(II) and zinc(II) at different pH values from solutions containing perchlorate and cyclohexanecarboxylic acid. Nickel(II) and cobalt(II) ions are not extracted quantitatively. Single extractions of mixtures of copper with transition metals gave the best separations for the copper/nickel system. Separations of copper from cobalt, lead, manganese and iron were less satisfactory.     

The application of cathodic sputtering to the production of atomic vapours in atomic fluorescence spectroscopy

Cathodic sputtering is used as a source of atomic vapour for the chemical analysis of metals and alloys by atomic fluorescence spectroscopy. The sputtered vapour is produced in a Pyrex glow-discharge chamber which is suitable for the rapid interchange of flat, metallic samples. The discharge operates with a water-cooled cathode specimen and a flow-through gas control system. Linear calibration curves are obtained for the determination of nickel, chromium, copper, manganese and silicon in some iron-base alloy standards. For nickel, chromium and copper, detection limits are of the order of 20 ppm in the iron, and for manganese and silicon about 70 and 400 ppm respectively. The reproducibility of the fluorescence measurements is about ±1%. The system can be readily adapted to provide simultaneous multi-element analysis.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定电镀废弃物中的七种元素

采用HCl-HNO3-HF-HClO4体系溶解试料,电感耦合等离子体原子发射光谱法测定电镀废弃物中的钙、铝、镉、钴、铁、锰、镁七种元素含量。通过加标回收实验,这几种元素的加标回收率为96.1%~102%,相对标准偏差均小于3%(n=7),此方法操作速度快、检测效率高,是一种理想的分析方法。     

An assessment of the levels of phthalate esters and metals in the Muledane open dump,Thohoyandou, Limpopo Province,South Africa

Background  

This work reports the determination of the levels of phthalate esters (dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), diethyl hexyl phthalate (DEHP)) and metals (lead, cadmium, manganese, zinc, iron, calcium) in composite soil samples. The soil samples were collected randomly within the Muledane open dump, Thohoyandou, Limpopo province, South Africa. Control samples were collected about 200 m away from the open dump. The phthalate esters were separated and determined by capillary gas chromatography with a flame ionization detector, whilst the metals were determined by atomic absorption spectrophotometry.     

Reversed Phase Extraction Chromatographic Separation of Manganese(II) with Tributyl Phosphate

Abstract

The extraction chromatography of manganese(II) was developed using tributyl phosphate as extractant from thiocyanate media with silica gel as the stationary phase. Manganese was extracted from 1.5 M ammonium thiocyanate, stripped with mineral acids and determined spectrophotometrically at 450 nm. It was separated from alkali metals, Mo(VI), nickel, silver and lead by selective extraction, and from iron(III), zinc, cobalt by selective stripping. The method was extended for the analysis of manganese in samples of soil and minerals.     

Development of a voltammetric method for the determination of iron(III) in Zn-Fe alloy galvanic baths

A square wave voltammetric method with a static mercury drop electrode (SMDE) was developed for the quantitative determination of iron (III) in Zn-Fe alloy galvanic baths. Real alloy bath samples were analyzed by the standard addition method and recovery tests were carried out. 0.50 mol L-1 sodium citrate (pH 6.0) or 0.20 mol L-1 oxalic acid (pH 4.0) were applied as supporting electrolytes resulting in both cases in a peak potential of about -0.20 V vs. AgIAgCl (saturated KCl). The iron (III) concentration in the alloy bath was 9.0 x 10(-4) mol L-1. A good correlation (r = 0.9999) was achieved between the iron (III) concentration and the peak current in the electrolytes studied, with linear response ranges from 1.0 x 10(-6) to 1.2 x 10(-4) mol L-1. Interference levels for some metals such as copper (II), lead (II), chromium (III) and manganese (II) that can hinder the Zn-Fe alloy deposition were evaluated; only copper (II) interferes seriously.     

Continuous-flow extraction system for elemental association study: a case of synthetic metal-doped iron hydroxide

A continuous-flow extraction system originally developed for sequential extraction was applied to study elemental association of a synthetic metal-doped amorphous iron hydroxide phase. The homogeneity and metal association of the precipitates were evaluated by gradual leaching using the system. Leachate was collected in fractions for determination of elemental concentrations. The result obtained as extractograms indicated that the doped metals were adsorbed more on the outermost surface rather than homogeneously distributed in the precipitates. The continuous-flow extraction method was also used for effective removal of surface adsorbed metals to obtain a homogeneous metal-doped synthetic iron hydroxide by a sequential extraction using acetic acid and small volume of hydroxylamine hydrochloride solution. The system not only ensures complete washing, but the extent of metal immobilization in the synthetic iron hydroxide could be determined with high accuracy from the extractograms. The initial metal/iron mole ratio (M/Fe) in solution affected the M/Fe mole ratio in homogeneous doped iron hydroxide phase. The M/Fe mole ratio of metal incorporation was approximately 0.01–0.02 and 0.03–0.06, for initial solution M/Fe mole ratio of 0.025 and 0.100, respectively.     

FT-IR and thermal studies of iron–nickel–manganese ternary levo-tartrate crystals

Several metallic tartrates deserve special attention due to their various applications. In the present investigation, mixed tartrate crystals of three different metals are reported. Using single diffusion gel growth technique, iron–nickel–manganese (Fe–Ni–Mn) ternary levo-tartrate compound crystals were grown with different concentrations. Spherulitic crystals with different coloration were obtained for various concentrations of metals. The concentrations of metals were determined by EDAX. The presence of functional groups was confirmed using Fourier transform infrared (FT-IR) spectroscopy. The powder XRD study suggested that the crystals belong to the orthorhombic system. The thermal stability of all the samples was studied from room temperature to 900 °C. It was found that the composition of the crystal affects the dehydration and decomposition behaviors. The results are discussed.     

The removal and kinetic study of Mn,Fe, Ni and Cu ions from wastewater onto activated carbon from coconut shells

Activated carbon from coconut shells (ACCS) was synthesised and used for the removal of metal ions (manganese, iron, nickel and copper) from aqueous solutions. Two different adsorption models were used for analysing the data. Adsorption capacities were determined: copper ions exhibited the greatest adsorption on activated carbon obtained from coconut shells because of their size and pH conditions. Adsorption capacity varied as a function of the pH. Adsorption isotherms from aqueous solutions of heavy metals on ACCS were determined and were found to be consistent with Langmuir’s adsorption model. Adsorbent quantity and immersion enthalpy were studied. The results were compared with other adsorbents used in a prior study.     

象山港沉积物对重金属Fe和Mn的吸附特征

对象山港不同站点的沉积物对重金属铁、锰的吸附特征进行了研究,考察了阳离子交换量、有机质含量对铁、锰的吸附能力的影响。吸附动力学实验表明,沉积物对铜和锌的吸附量随着铁、锰的初始含量增加而增大,但分别都在40 min和30 min左右达到吸附平衡;热力学实验结果表明,不同沉积物对铁、锰的热力学吸附过程符合Freundlich等温方程,各站点沉积物对铁的吸附能力由强到弱依次是S02,S25,S17,S10,S12,D03,D08,各站点沉积物对锰的吸附能力由强到弱依次是S02,S25,S17,S12,S10,D03,D08;影响因素实验表明,有机质的含量是影响沉积物对重金属铁吸附能力的主要影响因素之一,而沉积物对锰的吸附能力与阳离子交换量存在一定的关联性,有机质的含量几乎不影响沉积物对锰的吸附能力。因此,沉积物对重金属铁、锰的吸附系数K并不与其中单个理化性质有明显的相关性,这说明沉积物对铁、锰的吸附强度受多种沉积物理化性质控制。     

Investigation of element distributions between the symplasm and apoplasm of cucumber plants by TXRF spectrometry

The lead, iron and manganese distribution between the symplasm and apoplasm of cucumber plant parts (root and leaves) was determined by total reflection X-ray fluorescence spectrometry (TXRF). Plants were grown in control or in lead-contaminated (10⁻⁵M Pb) nutrient solutions containing iron in the chemical form of Fe(III)–EDTA or Fe(III)–citrate. The total concentrations of metals in the dried plant parts were measured after their microwave-assisted digestion. For the determination of the distribution of the elements investigated between the apoplasm and symplasm, the dried root and leaf samples were infiltrated and washed with a solution containing 10 mmol/dm³ Na₂EDTA and 0.5 mmol/dm³ CaSO₄. Elements in the washing solutions and in the washed plant parts were characteristic of the apoplasm and symplasm, respectively. It was established that lead accumulated mainly in the root apoplasm. Going up towards the shoot, in the leaves, there was approximately 50–60% of lead in the symplasm. The iron — similarly to lead — was found mainly in the apoplasm in the root, while in the leaves the symplasm/apoplasm ratio was 55:45%. The distribution of manganese between the symplasm and apoplasm did not show any significant change under the different treatments. In contrast with lead and iron, there was 70% and 60% of manganese in the symplasm of the root and of the leaves, respectively.     

原子吸收光谱法测定环境水中的镉、铁、锰的研究

目的对火焰原子吸收光谱法测定环境水中的镉、铁、锰的方法进行研究。方法在选定的最佳仪器条件下,测定环境水中镉、铁、锰的含量。结果RSD分别为6．51％、1．26％、2．50％,水样中镉、铁、锰的回收率分别为90．0％、106．0％、95．0％。结论该法操作简单、测试快速、结果准确稳定。     

FAAS法连续分析测试电池锌粉中镁铁铜铅锰

提出了运用FAAS法连续分析测试电池锌粉中Mg、Fe、Cu、Pb、Mn的含量,给出了Mg、Fe、Cu、Pb、Mn最佳测定条件及线性范围,在测定中对样品中的干扰因素进行了综合考虑.方法具有很好的灵敏度和重现性,步骤简单、操作容易、干扰少.测定样品Mg、Fe、Cu、Pb、Mn含量的相对标准偏差均小于1.0%（n=10）.标准加入回收率均在97.0%-101.5%（n=6）范围内.适用于电池锌粉中Mg、Fe、Cu、Pb、Mn的含量控制分析和样品系统分析.     

花椒中五种微量元素含量的测定

采用原子吸收光谱法,测定了河南太行山区花椒及椒皮、椒籽中锰、铁、铜、锌、铅的含量。结果显示,各元素在实验范围内,线性关系良好,回收率在92%~103%之间。花椒及椒皮、椒籽中均含有微量元素,花椒中锰、铁、铜、锌、铅的含量分别为78.851、90.868、11.571、18.818、0.086μg.g-1,其中锰、铁含量丰富,有害元素铅的含量极低。椒籽中铁、铜、锌的分布量大于椒皮;椒皮中锰的分布量大于椒籽。为探讨花椒的高药用价值提供了有力的证据,椒籽中铜、锌、铁含量高于椒皮,应大力开发利用。     

The microchemical analysis of ferrous and non-ferrous alloys

Satisfactory methods are described for the determination of certain of the alloying constituents in small quantities of steels, aluminium alloys and white metals. In steels, lead is determined by using an extraction procedure with dithizone, whereas the stable colour produced by vanadium with 3 : 3' dimethylnaphthidine is used for determining this element. In aluminium alloys, absorptiometric procedures are recommended for determining copper, nickel, iron and manganese. The determination of silicon is advocated by the absorptiometric technique. For the determination of antimony, in white metals, a micro volumetric procedure with standard potassium bromate is recommended using α-naphthaflavone as indicator.     

Chemical analysis of manganese nodules: Part IV. Determination of Nickel after Anion-exchange Separation

A method is described for the a.a.s. determination of nickel in manganese nodules after its separation from interfering metals. After dissolution of the sample in a mixture of perchloric and hydrofluoric acids, manganese, iron, cobalt, copper and other elements are adsorbed on the strongly basic anion exchange resin Dowex 1 (chloride form) from 95% ethanol-5% 12 M hydrochloric acid. The nickel passes into the effluent in which it is determined by a.a.s. with an air-acetylene flame. The method was used successfully for the determination of nickel in numerous samples of nodules from the Pacific Ocean.