Variable temperature dewar type tubular desiccator

An aqueous solution of the Solochromate Fast Grey RA. dye has proved a suitable indicator for the direct determination of thorium, ferric iron, bismuth and zinc, or the analysis of binary mixtures. thorium-iron, zinc-calcium, zinc-magnesium or zinc-thorium, with EDTA. Thorium can he determined in presence of U, Fe, Zn, Ba, Be, Mg, and comparatively large amounts of rare earths. Ferric iron and zinc can be estimated in presence of U, Mg, Ca, Ba and Be. Cations of the rare and the alkaline earths do not interfere with the determination of bismuth.     

电感耦合等离子体原子发射光谱测定混合稀土铜合金中稀土和非稀土元素

本文提出了用电感耦合等离子体原子发射光谱(ICP—AES)法直接测定混合稀土铜合金中13个非稀土和稀土元素。选用了合适的分析线对及ICP光源的工作参数。探讨了观察高度、功率、酸度、载气和基体量的变化对被测元素谱线强度的影响。不用化学分离,可一次同时测定La、Ce、pr、Nd、Sm、Sn、Zn、Fe、Al、Ni、Pb,Mg和Mn。测定范围(％):La_2O_3:0.096～6.4;CeO_2:0.24～16;Pr_6O_(11):0.0384～2.56;Nd_2O_3:0.096～6.4;Sn:0.096～3.2;Mg、Mn、Fe,Sm_2O_3:0.024～1.6;Zn:0.396～6.7;Pb:0.092～6.4;Ni:0.096～3.2;Al:0.0384～1.28。相对标准偏差±3.0～9.1％;回收率85～116％满足冶炼上的要求,得到了满意的结果。     

The accurate determination of bismuth in lead concentrates and other non-ferrous materials by AAS after separation and preconcentration of the bismuth with mercaptoacetic acid

A method for determining 0.0001% and upwards of bismuth in lead, zinc or copper concentrates, metals or alloys and other smelter residues is described. Bismuth is separated from lead, iron and gangue materials with mercaptoacetic acid after reduction of the iron with hydrazine. Large quantities of tin can be removed during the dissolution. An additional separation is made for materials high in copper and/or sulphate. The separated and concentrated bismuth is determined by atomic-absorption spectrometry using the Bi line at 223.1 nm. The proposed method also allows the simultaneous separation and determination of silver.     

Separation of tervalent rare earths and scandium from aluminium, iron(iii), titanium(iv), and other elements by cation-exchange chromatography in hydrochloric acid-ethanol

Tervalent rare earths and Sc are separated from the silicate-forming elements Al, Fe(III), Mg and Ti(IV), and also from Mn(II), U(VI), Be, Ga, In(III), Tl(III), Bi(III), Ni, Zn, Cu(II), Cd and Pb by cation-exchange chromatography. The other elements are eluted with 3.0 M HC1 containing 50% ethanol from a column of 60 ml of AG50W-X8 resin (200-400 mesh) while the rare earths are retained. Separation factors are larger than in aqueous hydrochloric acid. Th, Zr, Hf, Ba, Sr, Ca, K, and Rb are the only elements which accompany the rare earths group, but these can easily be separated by other methods which are described. Relevant distribution coefficients, elution curves and accurate results of quantitative separations of synthetic mixtures are presented.     

Analytical aspects of some organic acids

Summary A direct complexometric titration of iron(III) with EDTA using o- and p-cresotic acids indicators is given. The colour change at the end point is from blue-violet to light yellow or colourless [at low concentrations of iron(III)]. The optimum range of pH and temperature for carrying out the titrations is 1.99 to 4.2 and 35° to 55°C and 1.42 to 4.4 and 30° to 60° C, respectively. Iron(III) may easily and accurately be estimated in macro- and micro-gram quantities with the help of these metal indicators. Be, Mg, Ca, Sr, Ba, Cd, UO₂ and Mn are without any interference in the estimation. Back titration procedures for determination of zirconium and thorium with iron(III) and o- and p-cresotic acids are carried out.Part V: See Z. analyt. Chem. 173, 196 (1960).     

Determination of silver, bismuth, cadmium, copper, iron, nickel and zinc in lead- and tin-base solders and white-metal bearing alloys by atomic-absorption spectrophotometry

A simple atomic-absorption spectrophotometry method is described for the determination of silver, bismuth, cadmium, copper, iron, nickel and zinc in lead- and tin-base solders and white-metal bearing alloys, with use of a single sample solution. The sample is dissolved in a mixture of hydrobromic acid and bromine, then fumed with sulphuric acid. The lead sulphate is dissolved in concentrated hydrochloric acid. The method is particularly suitable for the determination of silver and bismuth, which are co-precipitated with lead sulphate. The other elements can also be determined after removal of the lead sulphate by filtration.     

Determination of trace elements in wines and classification according to their provenance

Provenance and authenticity of wines can be recognized on the basis of typical mineral and trace element patterns by means of chemometric methods. Therefore analytical methods were developed for the determination of As, Be, Co, Cs, Ga, Li, Nb, Ni, Rb, Te, Ti, W, Y, and Zr as well as Mo, Cd, Sb, Tl, U, and the rare earth elements in wines by inductively coupled plasma mass spectrometry (ICP-MS). For low risk of contamination or loss of analyte as well as depletion of sample amount and an easy sample pretreatment, direct measurement of diluted wines was studied. The accuracy of the analytical results was proven by recovery experiments by method comparison with standard addition methods and measurement of digested wines. In addition to applying statistical methods for characterizing the precision of the methods, the uncertainty of the measurements was estimated.Results for the elements mentioned above and additional 16 elements (Al, B, Ba, Ca, Cr, Cu, Fe, Mn, Mg, P, Pb, Si, Sn, Sr, V, and Zn) were evaluated by data analytical methods. Due to a specific choice of the analytes for multivariate statistical investigation a prediction rate by cross validation of 88.6% could be achieved.     

Extraction chromatographic separation of iron from complex liquid samples and the determination of <Superscript>55</Superscript>Fe

Summary Iron separation is described from liquid samples with a high concentration of ions that enables simple determination of ⁵⁵Fe. One of the described methods consists of iron precipitation from a large volume seawater by sodium hydroxide and/or ammonium carbonate and separation from other elements (Ca, Sr, Cu, Mg, etc.) on a TRU column with 4M HCl or 8M HNO₃. In the other procedure iron is separated directly from a mixture of seawater samples and HCl on a TRU column. In both methods, the iron recovery is almost 100%. After separation, ⁵⁵Fe is determined by counting with a liquid scintillation counter. The binding of Fe and Zn on TEVA, U/TEVA and TRU resins from seawater solutions of HCl and HNO₃depends on the type of the resin, concentration of acid and other ions. Iron and zinc can be separated from seawater on a U/TEVA column with 2M HCl.     

Improved separation of iron from copper and other elements by anion-exchange chromatography on a 4% cross-linked resin with high concentrations of hydrochloric acid

Iron(III) can be separated from copper(II) and many other elements by eluting these from a column of AG1-X4 anion-exchange resin with 8M hydrochloric acid, while iron(III) is retained and can be eluted with 0.1M hydrochloric acid. The separation is much better than the customary one with 3.5M hydrochloric acid. Columns containing only 8.8 ml (3 g) of resin can separate traces or up to more than 1 mmole of iron(III) from more than 1 g of copper. Mn(II), Ni, Al, Mg and Ca are quantitatively eluted together with copper(II). Lead, the alkali metals, Be, Sr, Ba, Ra, Sc, Y and the lanthanides, Ti(IV), Zr, Hf, Th and Cr(III) have not been investigated in detail but should be separated according to their known distribution coefficients. Separations are sharp and quantitative, less than 1 mug of copper remaining in the iron fraction when more than 1 g was present originally. Relevant elution curves and results of the quantitative analysis of synthetic mixtures are presented.     

Chelate von β-dicarbonylverbindungen und ihren derivaten : Teil L. Die extraktionsphotometrische bestimmung von zink und wismut mit thiodibenzoylmethan

Thiodibenzoylmethane is suitable for the extraction-photometric determination of traces of zinc and bismuth. The method is satisfactory in glycine-buffered solutions at pH 12.6 Interfering metal ions are masked by diethanolamine-dithiocarbamate in the determination of zinc and by cyanide in the case of bismuth; many foreign ions can be tolerated in more than 100-fold amounts     

Simultaneous determination of major,minor and trace elements in biocarbonates by inductively coupled plasma mass spectrometry

A method was developed for simultaneous determination of major (Ca), minor (Mg and Sr) and trace (Ba and U) elements in biocarbonates by inductively coupled plasma mass spectrometry (ICP-MS). The method precision (RSD%) is 0.73% for Ca, 0.77% for Mg, 0.59% for Sr, 2.02% for Ba, 1.13% for U, 0.67% for Mg/Ca, 0.27% for Sr/Ca, 2.06% for Ba/Ca and 1.23% for U/Ca. The ratio precision suggests that ICP-MS is satisfactory for obtaining multi-ratio data from biocarbonates. This technique was applied to 67 continuous coral samples.     

Spectrophotometric determination of the rare earths yttrium and cerium by bromopyrogallol red

A method is described for the spectrophotometric determination of microgram quantities of rare carths, yttrium and cerous cerium ions, using the colour of the complexes formed with bromopyrogallol red. The procedure has been applied to pure solutions containing 10–50 μg of the element.     

Spectrophotometric determination of rare earth elements and thorium with arsenazo

The simultaneous spectrophotometric determination of rare earth elements (lanthanum and gadolinium) and thorium with arsenuzo is described. In 0.05 N nitric acid, thorium alone forms a colored complex with the reagent; at PH 7.2 both thorium and the rare carths form colored complexes. Satisfactory results were obtained with weight ratios of Th/rare earths ranging from 0.2 to 10.     

Über die verteilung von metall-8-oxychinolin-verbindungen zwischen wasser und organischen lösungsmitteln : Mitt. photometrische bestimmung des magnesiums nach extraktion seines oxinates mit chloroform bei gegenwart von aminen

Under normal conditions, magnesium oxinate does not dissolve in non-polar organic solvents. In the presence of 2% butyl amine, however, magnesium can be extracted quantitatively in the pH range 10.5–13.6 by a 0.1% oxine-chloroform solution (concentration range 0.05–10γ Mg/ml), and can be determined photometrically by measurement of the extinction at 380 mμ. This reaction has been elaborated to a specific method of determination for small quantities of magnesium in the presence of the most important other elements. Furthermore, determination of magnesium can be combined quite simply with a photometric determination of slight iron content, also as the oxinate. The practical application of the method is demonstrated by determination of magnesium and iron in several calcium minerals, aluminium alloys and a zinc alloy.     

微波消解-电感耦合等离子体质谱法测定血液中30种微量元素

建立了微波消解-电感耦合等离子体质谱法定量测定血液中微量元素的方法.采用微波消解进行样品前处理,在硝酸-双氧水混合体系中消解后稀释,电感耦合等离子体质谱法(ICP-MS)测定全血中铜(Cu)、铅(Pb)、锌(Zn)、银(Ag)、钡(Ba)、锡(Sn)、镍(Ni)、钴(Co)、钒(V)、锑(Sb)、铊(Tl)、汞(Hg)、锰(Mn)、钼(Mo)、硒(Se)、铬(Cr)、镉(Cd)、钍(Th)、钛(Ti)、铝(Al)、砷(As)、铁(Fe)、钙(Ca)、镓(Ga)、锶(Sr)、锂(Li)、镁(Mg)、铍(Be)、钠(Na)和钾(K)元素的含量.对样品前处理过程和仪器工作参数进行了优化,通过内标校正法降低基体效应.结果表明,上述元素相关系数R²均大于0.999 8,检测精密度为0.142%～12.856%.方法简单、准确、快速,可精确测定全血中多种微量元素的含量,为全血中元素含量的测定提供了高效可靠的分析手段.     

Separation and preconcentration of the rare-earth elements and yttrium from geological materials by ion-exchange and sequential acid elution

The abundance of rare-earth elements (REE) and yttrium in geological materials is generally low, and most samples contain elements that interfere in the determination of the REE and Y, so a separation and/or preconcentration step is often necessary. This is often achieved by ion-exchange chromatography with either nitric or hydrochloric acid. It is advantageous, however, to use both acids sequentially. The final solution thus obtained contains only the REE and Y, with minor amounts of Al, Ba, Ca, Sc, Sr and Ti. Elements that potentially interfere, such as Be, Co, Cr, Fe, Mn, Th, U, V and Zr, are virtually eliminated. Inductively-coupled argon plasma atomic-emission spectroscopy can then be used for a final precise and accurate measurement. The method can also be used with other instrumental methods of analysis.     

A systematicstudy of insoluble substances. II

The antimonates of Be, Mg, Zn, Cd. Cr, Mn, Co, Ni, Cu, Ca, Sr, Ba, Al. 'I'h. Zr and U when heated to 900° were found to become sufficiently resistant to the standard acid treatment to be considered insoluble. The corresponding stannates do not become insoluble on being subjected to this treatment. The corresponding arsenates with the exception of those of Zi, Ti, Cr and Sn also do not become insoluble on being heated.     

Quantitative separation of lanthanides and scandium from barium,strontium and other elements by cation-exchange chromatography in nitric acid

The lanthanides plus yttrium and scandium are separated from Ba, Sr, Ca, Mg, Pb(II), Bi(III), Zn, Mn(II) and U(VI) by eluting these elements with 2.0 M nitric acid from a column of AG50W-X8 cation exchange resin (200-400 mesh). The lanthanides are retained and can then be eluted with 4 M nitric or hydrochloric acid. Separations are quantitative and applicable to microgram and millimolar amounts of the lanthanides and the other elements. Elements such as Cu(II), Co(II), Ni(II), Cd. Hg(II), T1(I). Ag, Be, Ti(IV) and the alkali metals should accompany barium quantitatively according to their known distribution coefficients. Relevant elution curves and results of analysis of synthetic mixtures are presented.     

电感耦合等离子体发射光谱法测定稀土发火合金中铁、镁、铜和锌

采用盐酸辅以加热的方式处理稀土发火合金样品,以电感耦合等离子体原子发射光谱法测定稀土发火合金中铁、镁、铜和锌含量。采用矩阵模拟实验优化分析谱线,利用多点定标校正曲线法计算测量结果。在最佳实验条件下,稀土发火合金中的基体元素对待测元素的测定结果无明显影响,各元素在检测范围内线性关系良好,相关系数均为0.999 9,方法检出限为0.001~0.010μg/m L。测定结果的相对标准偏差为1.10%~1.75%(n=11),样品加标回收率在96.00%~104.05%之间。该方法简便、快速且具有较高的灵敏度,适用于稀土发火合金中铁、镁、铜、锌等非稀土元素的测定。     

Carbon—carbon bond formation with bismuth salt. A chemoselective Grignard-type addition of allyl unit to aldehydes

In the presence of bismuth(III) chloride—metallic zinc or bismuth(III) chloride—metallic iron, allylic halides were found to react with aldehydes under mild conditions to give the corresponding homoallylic alcohols in high yields with high chemoselectivity.