钛及钛合金气体标准试样的制备及定值

研究了钛及钛合金的气体标准试样制备工艺和数据处理方案，对标准试样长期考察的结果。证明了它的准确性，稳定性是令人满意的。适用于氢氧分析仪器的校准和分析的验证。     

Spectrophotometric Determination of Trace Amounts of Titanium in Geochemical and Metallurgical Samples

Abstract

The reaction between cyclohexan-1,2-dione bissalicyloylhydrazone and titanium(IV) has been studied spectrophotometrically. An orange complex (λ = 470 nm, ? = 1.49 × 10⁴ 1.mol^?1.cm^?1) is quickly formed at pH 1–2.5 in a 3+2 V/V ethanol/water medium. Interferences (more than 65 species) have been investigated. In presence of some masking agents most of metal ions do not interfere. The orange complex has been satisfactorily used for the determination of titanium in amphibolites, granites, suspended matter, Portland cement, bauxite, cast iron and duraluminium alloy. The results are compared with those obtained using AAS and ICP methods.     

微波消解样品-石墨炉原子吸收光谱法测定高温镍基合金中的痕量银

采用微波消解样品-石墨炉原子吸收光谱法测定镍基高温合金中的痕量银。采用硝酸-氢氟酸-水(5+1+5)溶液对样品进行微波消解,以硝酸钯-硝酸镁的混合溶液为基体改进剂,石墨炉灰化温度为1 000℃,原子化温度为1 850℃,采用塞曼校正技术扣除背景。方法的检出限(3s/k)为2.3pg,加标回收率在98.3%~104%之间。方法应用于镍基高温合金中痕量银的测定,ICPMS的测定结果与之相吻合。     

Spectrophotometric Determination of Iron and Cobalt in Super Alloys

The quantitative analysis of iron and cobalt in super alloys has been studied. 1,-10-Phenanthroline and nitroso-R salt provide the chromophores for iron(II) and cobalt(II), respectively. The possibility of applying these photometric methods to a relatively complex substance, such as a super alloy, has been evaluated on the bases of precision and accuracy. The absorbance characteristics of metal complexes and the possible interference from foreign ions have also been carefully investigated. The presence of a high concentration of Ni results in a reducation of the amount of 1,10-phenanthroline available for the formation of ferroin complexes while Mo does not have this effect. The analytical methods have been applied to the super alloys, Inconel 718, Hastelloy X, and Inconel X-750. The modified 1,10-phenanthroline photometric method and the standard nitroso-R salt photometric method give high accuracy and good precision. This illustrates the analytical applicability of these reagents to super alloys.     

氢化物发生-原子荧光法测定高温合金中痕量铋的测量不确定度评定

介绍氢化物发生–原子荧光光谱法(HG–AFS)测定高温合金中痕量铋(Bi)的不确定度评定方法,建立了数学模型,分析了测量过程中不确定度的来源,并对不确定度分量进行了量化。当高温合金中铋含量为0.00016%时,扩展不确定度为0.00002%(k=2)。     

Persulfate Oxidation and Diphenylcarbazide Photometric Determination of Chromium in Super Alloys

The quantitative analysis of Cr in super alloys with the presence of a wide variety of elements, Al, B, C, Co, Cu, Hf, Fe, Mn, Mo, Ni, Nb, P, Si, S, Ti, Ta, W, Zr; and trace amounts (a few ppm) of Pb, Se, Bi, Tl and Te has been studied. Persulfate oxidation and diphenylcarbazide photometric method were studied with the purpose of developing a relatively fast and reliable measurement for Cr by wet chemical analysis. The results indicate that the latter is supperior to the former in practical view. In the photometric method, solid sample (0.1g alloys) when treated with HClO₄ and H₂SO₄ took ca. 72 hrs. for complete dissolution. When treated with HCl followed by HNO₃, 0.1 g alloys were completely dissolved within 1&1/2; hours. The best experimental conditions for diphenylcarbazide photometric determination of Cr was thus established. Photometric determination of Cr complexes was made at 540 nm.     

钛铁试剂光度法测定硅铁中钛

随着科学技术及外贸事业的迅猛发展 ,出口硅铁的质量要求越来越高 ,硅铁及稀土硅铁中需检测钛 ,现有的标准中没有硅铁中钛的检测方法 ,不能适应新时期外贸商检工作的需要。本法选择在 pH 2～ 4的盐酸介质中 ,钛与钛铁试剂络合进行显色反应。由试验结果可知 ,钛含量的线性范围为 0～10 0 μg·ml- 1,相关系数为 0 .9992 ,其最大吸收波长为 390nm ,摩尔吸光系数为 2 .2 2× 10 4 L·mol- 1·cm- 1,回收率在 98%～ 10 1%之间 ,能够满足硅铁中钛的测定。1　试验部分1.1　主要仪器与试剂72 1型分光光度计 (上海分析仪器厂 )苯二甲酸氢钾溶液 :5 …     

钒钛物料中钒钛化学物相分析现状及最新进展

主要概述了钒钛炉渣原料中价态钒(V2+,V3+,V4+,V5+),低价钛(Ti 2+,Ti 3+),金属钒(MV),氮化钒(VN),碳化钒(VC),碳化钛(TiC),氮化钛(TiN)及钢铁材料里固溶钒(Vsol),氮化钒(VN),碳化钒(VC),固溶钛(Tisol),碳化钛(TiC),氮化钛(TiN)等的化学物相分析的现状流程及最新进展,为从事钒钛化学物相分析方法研究者提供了参考依据。     

邻硝基苯基荧光酮流动注射分光光度法测定微量钛

本文研究了以邻硝基苯基荧光酮－溴化十六烷基三甲基铵为试剂的流动注射分光光度测定钛的新方法。该方法分析频率达到１００次／ｈ，线性范围为０～１．０μｇ／ｇ方法重性好，用于合金钢及纯铝中钛的测定，结果满意。     

3,4-Dihydroxybenzoic Acid As A Reagent for the Spectrophotometric Determination of Titanium

Abstract

The reaction between titanium(IV) and 3,4-dihydroxybenzoic acid in aqueous media results in an intensely colored complex which is stable for at least 8h. It allows the spectrophotometric determination of titanium in silicate rocks. The proposed method, in pH 4.0–6.0, shows a molar absorptivity of 1.43.10⁴ L.mole^?1.cm^?1 at 380 nm. Beer's Law is obeyed up to 3.0 μg/mL of titanium(IV). The interference of iron(III) can be eliminated by reduction to iron(II) with hydroxylamine hydrochloride. The method was applied to the determination of titanium in various standard rocks and the results indicated that the accuracy and precision are satisfatory.     

催化褪色光度法测定痕量钛的研究

本发现钛（Ⅳ）在稀硫酸介质中催化孔誉绿与碘化钾、碘酸钾之间的褪色反应，建立了褪色反应速率方程式和测定痕量钛（Ⅳ）的新方法。方法检测限为３．４ ×１０＾－１０ｇＴｉ（Ⅳ）／ｍＬ，测定范围为０～１．０μｇ／２５ｍＬＴｉ（Ⅳ）。用于测定人发中的微量元素钛的含量，获得了满意结果。     

钛铁试剂分光光度法直接测定轻稀土中的铈

利用铈的变价以及Ｃｅ（Ⅳ）－Ｔｉｒｏｎ配合物在不同酸度条件颜色的特殊性，建立了无需预先分离而直接测定混合稀土中铈含量的分光光度法，在ＰＨ为９．０条件下，借助空气的氧化，Ｃｅ（Ⅲ）和Ｃｅ（Ⅳ）都与Ｔｉｒｏｎ形成Ｃｅ（Ⅳ）－Ｔｉｒｏｎ配合物。该配合物在ＰＨ为５．０时呈亮黄色，在４３５ｎｍ处有最大吸收。     

稀土-二安替匹啉甲烷-I~--CHCl_3选择性萃取铁镍合金中稀土元素及其测定

本文提出用CHCl_3选择性萃取稀土-二安替匹啉甲烷-I~三元络合物的方法,从铁、镍合金中分离微量稀土元素,借偶氮胂Ⅲ光度测定。本文较为详细地研究了稀土三元络合物的定量萃取条件及Cu(Ⅱ).W(Ⅵ)对萃取的影响等。在确定的最佳分离及测定条件下,大多数金属离子不干扰测定。方法的测定下限为0.001%RE,相对标准偏差小于8.0%。     

Determination of Trace Elements in Super Alloy by ICP-MS

 A method is described for determination of 14 trace elements in super alloy certified reference material. Inconel 718 by ICP-MS. The interferences were investigated in detail. By using appropriate settings of the operational parameters and correcting interferences the elements without interference free isotopes were also analyzed. Non-spectral interference to the analytes was studied. No matrix separation or any other sample pretreatment but acid dissolution was made. 14 trace elements (B, Sc, Ga, Ge, In, Sn, Sb, Te, Hf, Ag, Ce, Tl, Pb and Bi) were analyzed by matrix matched standard solution calibration and using Rh as internal standard. Good agreement was achieved between the found levels and the certified values for most of the elements. The RSD (n = 4) of the determination values of Ce was lower than 20%, and RSD of the other 13 elements was lower than 10%. Received July 21, 2000. Revision May 29, 2001.     

Determination of Metals in Milling Solutions of Titanium Alloys by Differential Pulse Voltammetry

Abstract

Differential Pulse Voltammetric (DPV) methods for the determination of iron (Fe), titanium (Ti), vanadium (V) and chromium (Cr) in a synthetic milling solution of titanium alloy are presented. N-2-hydroxyethyl-ethylene diamine triacetic acid (EDTriA) or ethylene diamine tetraacetic acid (EDTA) was used to replace fluoride in complexing with all the metal ions. EDTriA was found to be a better ligand than EDTA in the determination of Fe, Ti and V. However, the reverse was true for Cr. Ti and Cr, which would interfere in the determination of V, was precipitated from the synthetic solution by adding EDTriA at very high pH. In the Cr determination, Ti and V were the major interfering species. The difficulty caused by Ti was alleviated by precipitating the Ti with EDTA at very high pH. The other difficulty, which was caused by V, was solved by using peak subtraction because of the perfect overlapping of the V and Cr peaks.     

Spectrophotometric study and analytical application of rare-earth Tiron complexes-II Determination of europium

The absorption spectra of europium-Tiron complexes in aqueous solution have been measured from 340 to 600 nm. The absorbance at 390 and 420 nm follows Beer's law up to 0.8 mg ml (pH 6.2-6.6). Other rare earths except for cerium(III) did not interfere. The interference of cerium could be removed by addition of ascorbic acid. The combining ratio of Tiron to europium has been found to be 1:1.     

The Determination of Titanium in Silicates by Atomic Absorption Spectrophotometry

Abstract

A procedure for the quantitative determination of titanium in silicates is given. Interferences usually associated with silicate parting solutions are studied in order to develop the proper conditions for the titanium sample solution.     

Extraction-Spectrophotometric or -Atomic Absorption Spectrophotometric Determination of Titanium Using Caffeic Acid and a Liquid Ion Exchanger

Abstract

A selective and sensitive method for the extraction followed by a spectrophotometric or atomic absorption spectrophotometric determination of titanium(IV) in trace amounts is described. The molar absorptivity of the caffeic acid-Aliquat 336 complex is 5.7 × 10⁴ l mol^?1 cm^?1 at 380 nm; the yellow coloured complex obeys Beer's law in the range 0.05–1.2 mg/l of titanium in the final extract. The method is applied to the preconcentration, separation and determination of titanium(IV) in steel, industrial effluents and environmental samples.     

钛及钛合金表面羟基磷灰石涂层结合强度及稳定性

钛(Ti)及其合金凭借优异的机械性能和良好的生物相容性,一直是骨和牙种植体的主要临床应用材料。由于钛及其合金自身的生物惰性,不易与周围骨组织进行快速的骨整合,因此其表面的生物活性有待进一步提高。羟基磷灰石(HA)是人体骨和牙齿的主要无机成分,具有良好的生物活性和生物相容性,受其力学性能的制约,常被作为涂层材料覆盖在钛基体表面,用以提高植入体的生物活性。但一直存在涂层与基体界面结合强度低和涂层力学稳定性差的问题,成为限制其临床广泛应用的主要因素。本文从涂层结构设计、成分设计及制备方法等方面,就国内外改善钛基底与HA涂层界面结合性能的研究现状和发展动态作一综述,为高性能钛植入体的制备和应用提供参考。