高效液相色谱法测定盐酸噻吩诺啡有关物质的方法研究

建立盐酸噻吩诺啡药物有关物质检查的液相色谱方法。采用ZORBAX—C18色谱柱，流动相为甲醇-乙腈-（0．002mol／L KH2PO4—0．3％三乙胺，pH3），检测波长为220nm。该方法能较好地分离药物与有关物质，样品在测定浓度范围内线性关系良好，药物纯度为99．0％以上。对药物中的未知杂质用质谱法鉴定，确认杂质来源。方法可用于盐酸噻吩诺啡药物的有关物质检测。     

ICP-AES法测定锡铅焊料中铜铁镉锌铝铋

锡铅焊料试样经盐酸、硝酸分解后，加入一定量的硫酸沉淀分离基体铅，以盐酸一氢溴酸排锡后，采用ICP—AES法同时测定铜、铁、镉、锌、铝、铋。方法没有谱线和背景干扰，检出限铜为0．000034％，铁为0．000038％，镉为0．000026％，锌为0．000071％，铝为0．00025％，铋为0．00060％，回收率在91．09／5～99．2％之间。完全满足锡铅焊料中的铜、铁、镉、锌、铝、铋测定的要求。     

N-1923在分析化学中的应用 Ⅱ.微量铌的萃取和测定

本文就高分子胺N-1923对铌的萃取特性进行了研究。证实它是铌的有效萃取剂。在0.5M硫酸介质中的萃取分配系数大于1000,并能被盐酸和酒石酸混合液所反萃,反萃液便于与比色测定相衔接。萃取是在硫酸、酒石酸介质中进行的。铁的干扰是借加入抗坏血酸使还原为低价而消除。文中提供的分析方法可用于各种试样中铌的分离和测定。测定下限为0.001％Nb_2O_5。     

蒸馏分离-分光光度法测定枸杞子中的微量锗

利用盐酸与锗元素反应生成易挥发的四氯化锗，以蒸馏方法将四氯化锗分离出来，然后在1～1．5mol／L盐酸溶液中，用显色剂苯芴酮与四氯化锗进行显色反应生成橙红色配合物，在500nm波长处进行分光光度法测定。在0～200μg／(50mL)，线性方程为A=0．1714c．相关系数r=0．9996。该方法的检出限为0．0588μg／mL，测定结果的相对标；位偏差为2．24%～2．30%(n=11)，平均回收率为95．3％～95．4％。     

衍生荧光法测定盐酸西布曲明

通过衍生反应，建立了用荧光光度法测定盐酸西布曲明的新方法。并对衍生体系、反应条件、产物稳定性等进行了研究。实验确定丙二酸和乙酸酐混合试剂与盐酸西布曲明在75℃的水浴中加热15min，所得产物发射强荧光，最大激发波长λcx=456nm，最大发射波长λem=496nm。在上述波长下，荧光强度与盐酸西布曲明的质量浓度在0．11～9．5μg／mL范围内呈良好的线性关系，检出限为13．4ng／mL，标准加入回收率在95．4％～104．2％。用于曲美胶囊中盐酸西布曲明的测定。     

方波伏安法间接测定饲料中的高含量磷

在pH=5．5的六次甲基四胺-盐酸缓冲溶液中，硝酸铅与磷酸根和氯离子反应，生成磷酸氯化铅复盐沉淀，用方波伏安法测定过量的铅离子，从而间接测定无机磷。在最佳测定条件下，当0．04mol／L硝酸铅标准溶液的用量为1．0mL时，峰电流ip与磷的质量浓度c在0．2～20μg／mL内呈良好线性关系，线性回归方程为ip=-2．39c 54．82，相关系数为0．9876，检出限为0．085μg／mL。用于饲料中磷含量的测定，测定结果的相对标准偏差为1．24％～2．44％，加标回收率为95％～99％。     

5—Br—PADAP快速光度法测定钢中铌

研究了用２－（５－溴－吡啶偶氮）－５－二乙氨苯基酚（５－Ｂｒ－ＰＡＤＡＰ）测定钢中铌显色条件，所拟方法简捷实用，可测钢中０．０１０％～６．００％的铌。     

微分电位溶出法测定车间空气中镉的研究

以０．５０ｍｏｌ．Ｌ＾－１盐酸为底液，预镀汞膜的玻碳电极为工作电极，用微分电位溶出法对车间空气中镉进行测定，用标准加入法定量，在选定的条件下，线性关系良好，精密度ＣＶ为１．２５６％－２．２３％，平均回收率为９６％－１０７％，本法与原子吸收法对比，测定结果显著性差异，结果令人满意。     

ICP-AES法测定铜镍矿、铅锌矿中铜、镍、铅、锌、钴

用电感耦合等离子体发射光谱法测定铜镍矿、铅锌矿石中铜、镍、铅、锌、钴,样品用盐酸-硝酸溶解,在选定的测量条件下以ICP—AES测定溶液中的Cu、Ph、zn、Co、Ni的含量．对国家一级标准物质进行测定,方法精密度（RSD,n=12）为Cu 2．92％～6．62％,Pb 1．88％-2．61％,Zn 1．30％-2．05％,Co 6．90％,Ni 2．23％．本方法具有线性范围宽、干扰少、快速、简便、检出限低等优点．用于实际使用,结果满意．     

微乳液介质-二甲氧基羟基苯基荧光酮催化光度法测定合金中铌

1 引言 研究了以非离子微乳液介质，在稀硫酸体系中，用氨三乙酸作活化剂，铌催化溟酸钾氧化二甲氧基羟基苯基荧光酮褪色的新指示反应，据此建立了催化动力学光度法测定铌的新方法。非离子型微乳液有明显提高了体系的灵敏度和稳定性，检出限达到0．15μg/L。该方法应用于样品中痕量铌的测定，其相对标准偏差小于6．8％。     

The separation of niobium from tantalum by extraction with tributyl phosphate and determination of niobium as the thiocyanate complex

A method is proposed for the rapid extraction and separation of microgram amounts of niobium(V). The niobium is extracted quantitatively by 100 % TBP from 7.7-9.4 M (initial) hydrochloric acid and determined spectrophotometrically as the thiocyanate in TBP-acetophenone solution. Beer's Law is obeyed at 430 mmu over the range 0.8-9.0 mug ml . The system is stable for 72 hr. Caesium, calcium, strontium, barium, aluminium, titanium(IV), zirconium(IV), cerium(TV), fluoride, thiocyanate and oxalate do not interfere (1 mg). Niobium(V) can be determined in a niobium(V)-tantalum(V) mixture. The method is accurate and reproducible to within +/-2%.     

Liquid-liquid extraction of niobium(V) in the presence of other metals with high molecular mass amines and ascorbic acid

A novel method is proposed for the solvent extraction of niobium(V). A 0.1M solution of Aliquat 336S in xylene quantitatively extracts microgram quantities of niobium(V) from 0.01M ascorbic acid at pH 3.5-6.5. Niobium from the organic phase is stripped with 0.5M nitric acid and determined spectrophotometrically in the aqueous phase as its complex with TAR. The method permits separation of niobium not only from tantalum(V) but also from vanadium(IV), titanium(IV), zirconium(IV), thorium(IV), chromium(III), molybdenum(VI), uranium(VI), iron(III), etc. Niobium from stainless steel was determined with a precision of 0.42%.     

Arsenazo III and its analogues-V Complex formation of niobium with o,o'-dihydroxyazo compounds

A new group of reagents-the 2,7-bisazo derivatives of chromotropic acid-has been synthesized and the reaction of these compounds with niobium studied. Reaction with niobium occurs in strongly acidic medium (1-3N) and is characterized by high sensitivity ( = 30-50 x 10(3)). The functional grouping responsible for the reaction was shown to be the o,o'-dihydroxyazo group. The analytical usefulness of the reagents is determined by the presence of the electron-withdrawing substituents and the nature of the diazo coupling component. Niobium reacts in partially hydrolysed form with these reagents, to give 1:1 complexes.     

Analysis of lead titanate-zirconate ceramics: Determination of lead,titanium and niobium by differential cathode-ray polarography

Differential cathode-ray polarography is applied to the direct determination of lead, titanium and niobium in lead titanate-zirconate solid-solution ceramics containing small additions of niobium pentoxide. Titanium and niobium are determined in buffered EDTA solution at pH 4.0 and lead in 1 M hydrochloric acid. With the high precision comparative technique, relative standard deviations of 0.11% and 0.31% for lead and titanium respectively are obtained. Niobium is determined by the subtractive technique.     

Separation of niobium and tantalum by extraction chromatography with bis(2-ethylhexyl)phosphoric acid

A novel method is developed for the reversed-phase extractive chromatographic separation of niobium and tantalum with bis(2-ethylhexyl)phosphoric acid. Niobium is extracted from 1-10M hydrochloric acid and can be stripped with 3M sulphuric acid containing 2% hydrogen peroxide. Tantalum is extracted from 0.1-2M hydrochloric acid and can be stripped with 0.1M hydrochloric acid containing 2M tartaric acid. It is possible to separate niobium and tantalum, in different ratios, from multicomponent mixtures.     

Determination of niobium in rocks, ores and alloys by atomic-absorption spectrophotometry

Niobium, in concentrations as low as 0.02% Nb(2)O(5), is determined in a variety of materials without separation or enrichment. Chemical and ionization interferences are controlled, and sensitivity is increased, by maintaining the iron, aluminium, hydrofluoric acid and potassium content within certain broad concentration limits. There is close agreement with the results of analyses by emission spectrographic, electron microprobe and X-ray fluorescence methods.     

X-ray fluorescence analysis of titanium alloys

An X-ray solution method is proposed for determining major amounts of Mo, Sn and Zr in Ti alloys. The method utilizes adjacent elements in the periodic table as internal standards and has been successfully applied to levels of 3-10% Sn, 11-40% Mo and 6-20% Zr. The procedure involves three steps: dissolving the sample with a suitable acid mixture; adding the suitable internal standard at the concentration levels experimentally found to give optimum accuracy and precision; analysing the resulting solution mixture by X-ray fluorescence. Antimony was found to be a suitable internal standard for its adjacent element tin at a concentration ratio of 3:1 Sb:Sn. Niobium was successfully used for both its adjacent elements, molybdenum and zirconium, at 2:1 concentration ratios, Nb:Mo and Nb:Zr. A number of elements non-adjacent to tin, molybdenum and zirconium (i.e., copper, bromine, titanium, bismuth and tantalum) were experimentally found unsuitable as internal standards. Concentration factors of the internal standard and the adjacent elements sought were found to affect significantly the precision of analysis.     

Spectrophotometric determination of zirconium in steels with xylenol orange

Zirconium (0.005–0.25%) is determined after acid dissolution of the steel, and fusion of insoluble matter with sodium carbonate and sodium hydrogensulphate. Niobium and other interfering ions are removed by mercury cathode electrolysis. Residual small amounts of iron(III) are masked with ascorbic acid.     

油酸新戊二醇己二酸复合酯的合成及其润滑性能

新戊二醇(NPG)和己二酸(AA)通过酯化反应合成了"低聚物"中间体(1).当n(NPG):n(AA)＝1.5～3.0时,1的聚合度(m)在4.34～2.10,收率97%.以对甲苯磺酸为催化剂,甲苯为带水剂,1与油酸进行酯化得到复合酯(2),收率83%～89%.测定了2的黏度、黏度指数、氧化稳定性、生物降解率、摩擦磨损性能和热稳定性.结果表明,2的黏度和氧化稳定性随着m的增大而增大,100 ℃时的黏度在18.3 mm~2·s~(-1)～30.1 mm~2·s~(-1),黏度指数均超过200,凝点低于-43 ℃,生物降解率＞96%,最大无卡咬负荷(P_B)为784 N,磨斑直径0.40 mm,热分解温度＞300 ℃.1和2的结构经IR表征.     

Dosage d'oxydes de tantale,niobium et titane dans leurs mélanges par radioactivité

The oxides of niobium, tantalium and titanium can be determined in their mixtures by means, of radioactive tracers. Two methods have been studied.1st method. On irradiation of the mixture with slow neutrons and measuring the activity of the ¹⁸²Ta formed, tantalium can be determined within about 10% in mixtures poor in this element.2nd method. It is an improvement of the classical method of separation of these oxides by tannin. ⁹⁵Nb of known specific activity is added to the solution, to be determined, then tantalium, together with a part of the niobium, is precipitated by tannin at ph 3.8. Niobium is then precipitated in the filtrate at a higher pH. The activity measurement of the two fractions allows the determination of how the partition is effected and the introduction of the necessary correction. Titanium is determined by colorimctry after calcination of the redissolvcd oxides.