紫外分光光度法测定12种药材中的微量硒

采用紫外分光光度法，以邻苯二胺为显色剂测定了12种药材中微量硒的含量。本法回收率为98．95％，变异系数1．34％．     

紫外分光光度法分析陈皮中微量元素硒

采用紫外分光光度法,在检测波长为335 nm,以邻苯二胺做显色剂,分析了中药陈皮中微量元素硒。结果表明,广东、陕西城固、四川陈皮中硒元素平均含量分别为5.3754,2.9008;2.7570μg/g。     

分光光度法测定浙贝母中不同价态的硒含量

基于３，３＇－二氨基联苯二胺对Ｓｅ＾４＋的选择性测定，同时选择用２ｍｏｌ／Ｌ盐酸将Ｓｅ＾６＋定量还原为Ｓｅ＾４＋，测定了浙贝母中不同价态的硒含量。本法测Ｓｅ＾４＋回收率大于９３％，测Ｓｅ＾６＋回收率大于９５％，变异系数均小于５％，检出限为０．０２ｍｇ／Ｌ。     

巯基棉富集分离分光光度法测定尿硒含量

为探索用巯基棉富集分离分光光度法测定尿硒含量的最佳实验条件,在表面活性剂吐温-80溶液存在下,改变酸度、温度、显色剂用量测定了尿样硒含量。结果表明,该法准确度、精密度高,用于尿硒、血硒含量测定,均能收到满意效果。     

紫外分光光度法测定富马酸二甲酯的含量

本文研究了用紫外分光光度法测定富马酸二甲酯含量的方法 ,探讨了测定过程中有关条件的变化对测定的影响 ,获得了测定的适宜条件 :波长 2 1 0± 2nm ;温度 1 9～ 2 5℃ ;无水乙醇为溶剂 ;测定体系的pH为7.2 5～ 8.2 5。DMF的含量与溶液的吸光度的关系为P =0 .0 933A +0 .0 4 1 6,经与色 -质谱分析结果对比表明本法具有较高的准确性     

大米中硒含量的测定

为使人们更好地控制和调节硒的摄入量,用紫外分光光度法测定了大米中的硒含量。样品通过混酸消化,将有机硒转化成无机硒,酸性条件下,Se(Ⅳ)与邻苯二胺反应,产物在335nm有最大吸收峰。测定结果表明,天津小站米、东北米、丝苗米、泰国香米、富硒米的有机硒含量分别为:0.041、0.046、0.035、0.034、2.021μg/g,有机硒含量占总硒含量的比例分别是89.13%、82.14%、87.50%、80.95%、98.92%。富硒米硒含量及有机硒的比例明显高于其它种类的米。     

花旗参中硒含量的光度法测定

在Ｔｒｉｔｏｎ－Ｘ－１００存在下，Ｓｅ（Ⅳ）与硫氰酸钾、罗丹明Ｂ在酸性介质中生成三元配合物，最大吸收波长 ６０５ｎｍ ，摩尔吸光系数 ３．２ ×１０，Ｓｅ（Ⅳ）含量在 ０～３．２μｇ／２５ ｍＬ范围内符合比耳定律。方法灵敏，选择性好，用于花旗参样品中微量硒的直接测定，取得满意结果。     

紫外分光光度法测定中草药中铁的含量

对白芍、党参、白术、茵陈、天冬、枸杞子、当归、菟丝子、金银花、桔梗中微量元素铁的含量进行了测定,为进一步研究其药理作用提供基础。中草药消化后配制成溶液,用邻二氮菲作显色剂,使用UV-1200型紫外分光光度计在510 nm处测定各样品的吸光度(A),求出样品中微量元素铁的含量。结果显示,当归和金银花中铁的含量较丰富,分别为(135.367 8±0.111 1)μg/g和(125.936 4±0.159 9)μg/g;桔梗含铁量最少,为(3.510 9±0.159 9)μg/g,10种中草药中铁含量有显著性差异(P<0.05)。结果为使用中草药治疗系统疾病提供了可靠数据,10种中草药在用量范围内Fe含量适合人体每天正常摄入量。     

紫外分光光度法测定丙酮酸

基于丙酮酸在紫外吸收光谱290～340nm区有较强的吸收,建立了分光光度法测定丙酮酸(盐)的方法。在pH11．0的水溶液中,位于320nm处,丙酮酸有吸收,而其他有机酸和杂质无吸收或吸收不明显。在320nm处,丙酮酸在0．2～2．8g／L范围内符合比耳定律,其R2为0．9997,平均回收率99．8％,RSD0．46％。该法适合于发酵液和分离提取过程中丙酮酸及其盐类的测定。     

紫外分光光度法测定富马酸含量的新方法

研究了紫外分光光度法测定富马酸含量的新方法.在乙醇溶液中,富马酸最大吸收在210.5 nm处,表观摩尔吸光系数为ε210.5=1.05× 104L·mol-1·cm-1.方法的检出限为0.1μg/mL,此法具有灵敏度高、操作简便、快速等优点.     

陈爱敏,魏海英*

室温下,硒(IV)与邻苯二胺配位生成黄色配合物,用环己烷萃取后,在最大吸收波长330nm处测定其吸光度。实验结果表明：硒含量在4～20 μg/mL内线性关系良好,线性方程Y=0.1999C-0.0011(R=0.9995)。最优化条件下测定硒盐中硒的含量取得满意结果。该法操作简单,设备和药品价格低廉,准确度高,稳定性好,适宜于基层实验室对食品中微量元素硒的检验。     

Kinetic studies on the reduction of a nickel (III) oxime-imine complex by sulphur(IV) and selenium(IV)

The kinetics of the reduction of [Ni^III(L¹)]²⁺ (where HL¹ = 15-amino-3-methyl-4,7,10,13-tetraazapentadec-3-en-2-one oxime) by sulphur(IV) and selenium (IV) over the regions pH 2.50–8.02 and 2.01–4.00 respectively have been investigated at 30°C. Attempts were made to evaluate the reactivity of all the reacting species, of sulphur(IV) and selenium(IV) by considering suitable pH ranges. The oxidation of SC₂·H₂O and HSO ₃ ⁻ is proposed to proceed through the formation of a hydrogen-bonded adduct. The reaction with SO ₃ ²⁻ seems to follow a direct outer-sphere route which is well supported by Marcus crossrelation calculation. The oxidation of HSeO _l3 ⁻ is ≈ 10³ times slower than that of H₂SeO₃. The kinetic data indicate that the oxidation of sulphur(IV) by [Ni^IIIL¹)]²⁺ is much more favourable as compared to the corresponding oxidation of selenium(IV).     

Oxidative Rearrangement via Oxycerication with Ce(IV) Salt

α-Arylpropanoic acids are pharmaceutically interesting compounds, some of them exhibit anti-flammatory and analgestic activities1. Even the enormous progress made in the synthesis of α-arylpropanoic acids by 1,2-aryl rearrangement of arylpropanone using thalium (III) nitrate1,2, silver (I) compounds,3,4 lead (IV) acetate5,6 and iodinate7 during the last decades. The route is, however, unsuitable for the preparation of pharmaceutical products (Naproxen, Ibuprofen and so on) because of the …     

The Spectrophotometry Determination of Mn(III) in the Presence of Mn(IV)

Abstract

The spectra of complex of Mn(III) and Mn(IV) with pyrophosphoric acid are investigated. The molar absorption coefficient of the complex of Mn(III) with pyrophosphoric acid is 80.6/Mcm at 510nm which is close to that of Mn(IV), 110/Mcm, however, the molar absorption coefficient of the complex of Mn(HI) with pyrophosphoric acid is only 4.98/Mcm at 398nm which is much less than that of Mn(IV), 390/Mcm. Based on this absorbance difference between Mn(III) and Mn(IV) at wavelength 398nm and 510nm, a procedure of determination of Mn(III) in the presence of Mn(IV) has been developed.     

Determination of Selenium (IV) in Biological Sample by Cathodic Stripping Voltammetry

Abstract

The determination of selenium (IV) in biological sample using cathodic stripping voltammetry is reported. It was found possible to determine selenium directly in biological samples containing such metals as zinc (II), lead (II), iron (III), arsenic (III) and magnesium (II). The results for selenium in bovine liver are reported.     

Synthesis and characterization of uranium (IV) phosphate-hydrogenphosphate hydrate and cerium (IV) phosphate-hydrogenphosphate hydrate

A new uranium (IV) phosphate of proposed formula U₂(PO₄)₂HPO₄·H₂O, i.e. uranium phosphate-hydrogenphosphate hydrate (UPHPH), was synthesized in autoclave and/or in polytetrafluoroethylene closed containers at 150 °C by three ways: from uranium (IV) hydrochloric solution and phosphoric acid, from uranium dioxide and phosphoric acid and by transformation of the uranium hydrogenphosphate hydrate U(HPO₄)₂·nH₂O. The new product appears similar to the previously published thorium phosphate-hydrogenphosphate hydrate Th₂(PO₄)₂HPO₄·H₂O (TPHPH). From preliminary studies, it was found that UPHPH crystallizes in monoclinic system (, , , β=91.67(3)° and ). Heated under inert atmosphere, this compound is decomposed above 400 °C into uranium phosphate-triphosphate U₂(PO₄)P₃O₁₀, uranium diphosphate α-UP₂O₇ and diuranium oxide phosphate U₂O(PO₄)₂.Crystallized cerium (IV) phosphate-hydrogenphosphate hydrate Ce₂(PO₄)₂HPO₄·H₂O (CePHPH) was also synthesized from (NH₄)₂Ce(NO₃)₆ and phosphoric acid solutions by the same method (monoclinic system: , , , β=91.98(1)° and ). When heating above 600 °C, cerium (IV) is reduced into Ce (III) and forms a mixture of CePO₄ (monazite structure) and CeP₃O₉.     

催化动力学光度法测定富硒茶叶中痕量硒

本文研究了Se催化过氧化氢氧化甲基橙反应体系测定痕量Se的方法。硒浓度在0～65．7μg／L范围内与褪色反应率lg(A0／A)呈线性关系。方法检出限为0．76μg／L。用于茶叶中硒的测定，结果较满意。     

Gravimetric Determination of Mercury(II) and Vanadium(IV) with Benzoylacetanilide

Abstract

Gravimetric methods for the determinations of mercury(II) and vanadium(IV) with benzoylacetanilide have been described. These metals have been separated from commonly associated ions and a procedure for the determination of vanadium content of steel has been developed. By these methods, 14 to 50 mg. of mercury and 5 to 20 mg. of vanadium have been estimated with relative standard deviations of 0.18% and 0.10%, respectively.     

催化动力学光度法测定海产品中痕量硒

在硝酸介质中,硒（Ⅳ）能催化溴酸钾氧化亚甲蓝使之褪色。研究了这一催化反应的动力学条件,建立了一种动力学光度法测定痕量Ｓｅ（Ⅳ）的新方法。其灵敏度为３．８×１０＾－７ｇ／Ｌ Ｓｅ（Ⅳ）,Ｓｅ（Ⅳ）的含量在０￣８μｇ／Ｌ范围内与褪色反应速率１ｇ（Ａ０／Ａ）成正比。通过萃取纯化,使方法具有良好的选择性和准确度。用于多种海产品中痕量硒的测定,结果满意．     

Darstellung und spektroskopische Charakterisierung von bindungsisomeren Halogenoselenocyanato-Osmaten(IV) und -Rhenaten(IV)

Preparation and Spectroscopic Characterization of Bond Isomeric Halogenoselenocyanato-Osmates(IV) and -Rhenates(IV) By oxidative ligand exchange of appropriate chloro-iodo complexes of Os^IV or Re^IV with (SeCN)₂ in CH₂Cl₂ or by heterogeneous reaction with Pb(SeCN)₂ or AgSeCN in CH₂Cl₂ the new complexes cis-[OsCl₄(NCSe)(SeCN)]^2?, tr.-[OsCl₄Br(NCSe)]^2?, tr.-[OsCl₄Br(SeCN)]^2?, [ReCl₅(NCSe)]^2?, [ReCl₅(SeCN)]^2?, tr.-[ReCl₄I(NCSe)]^2?, tr.?[ReCl₄(NCSe)(SeCN)]^2? and tr.?[ReCl₄(NCSe)₂]^2? are formed and isolated as pure compounds by ion exchange chromatography on DEAE-cellulose. The bond isomers are significantly distinguished by the frequencies of innerligand vibrations: n?_CN(Se) > n?_CN(N); n?_CSe(N) > n?_CSe(Se); δ_NCSe > δ_SeCN. The electronic spectra (10 K) of the solid salts reveal a bathochromic shift for the charge transfer bands of the Se isomers as compared with the corresponding N isomers. The intra-configurational transitions are observed for the Os^IV complexes at 600 to 2400 and for the Re^IV complexes at 500 to 1600 nm. The ⁷⁷Se nmr signals of the Os^IV bond isomers are registrated for Se binding in the region 970 to 1040 ppm, for N coordination downfield at 1540 to 1640 ppm.