衬钽石墨炉原子吸收分光光度法测定水中痕量钡

石墨炉原子吸收分光光度法广泛地应用于痕量分析,但常局限于测定低温和中温元素。相当多的元素与石墨管形成稳定的碳化物,测定灵敏度低,常伴有记忆效应,石墨管也易损坏。钡属于形成碳化物的元素之列,而且特征波长在可见区,石墨管在高温下的背景发射影响测定。为了克服碳化物的影响,通常采用以下解决办法。常用的碳化物涂层法,虽然文献报导较多,但处理过程比较麻烦,而且结果重现性差,对钡的效果并不明显。也有使用热解石墨管测钡的,灵敏度有不同程度的提高。用金属原子化器。测定钡,灵敏度有所提高,但在通常的石墨炉上直接采用有一定的困难。还有在标准石墨管中衬入高熔点的金属     

石墨炉原子吸收测定硅酸盐岩石样品中铍时各种石墨管的应用

石墨炉原子吸收测定铍,由于基体的影响,常常采用标准加入法,预先分离基体和在标准溶液中加入基体元素等方法,这些方法比较费时,给分析带来许多不便。近年来,由于等温平台石墨炉和加基体改进剂等方法,对消除基体元素的干扰比较成功,因此被人们普遍采用。本工作不用平台,不加基体改进剂,而采用最大功率加热方式,分别利用热解镀层石墨管(简称PGT),普通石墨管(简称GGT)和衬钽管(简称TaT),直接分析岩石样品中     

基质效应对有机磷农药测定的影响及其解决方法

该文以液液萃取-气相色谱法探讨了基质对乐果、甲基对硫磷、马拉硫磷和对硫磷4种有机磷测定的影响以及解决方法.研究表明,气相色谱法测定有机磷农药的过程中基质效应显著存在,其基质增强比例为1.01 ～3.46.基质效应由基质种类及含量、有机磷农药种类及浓度等因素决定,同时与萃取溶剂、测定条件(如衬管、进样口温度等)有关.不同萃取溶剂对有机磷农药的萃取效率不同,但均存在基质增强效应;当进样口温度为260 ℃时,可最大程度降低基质在衬管中的残留,且不造成有机磷农药的分解;衬管则应首选带玻璃棉的.实际样品/标准样品的交替进样方式可以降低基质效应强度,但难以达到回收率要求,而校正因子校正法及分析保护剂法则是降低或消除基质效应的可行办法.     

超纯气体中微量水的气相色谱分析

超纯气体制备和用超纯气体做保护气的许多工业部门,对气体中微量水是需要经常分析的。目前常用的大都是露点法,其缺点是仪器只能专用;而用高灵敏度热导检测器气相色谱仪,不但可方便地测出超纯气体中的微量水,而且还可以测定超纯气体中的微量气体杂质及作其它有机物分析之用。气相色谱仪操作简单,定量也较方便准确。     

衬钽管石墨炉原子吸收法测定痕量镓时基体改进剂的研究及应用

提出用钒和铜混合基体改进剂衬钽管石墨炉原子吸收测定镓的方法。衬钽管使镓的灵敏度提高6倍左右,钒和铜混合基体改进剂不仅能进一步提高灵敏度,而且能提高灰化温度,降低原子化温度,增强抗干扰能力。测定 GSD 标准样品中的镓时,不需对样品进行预分离即可直接进行测定,结果与参考值相符。     

新型透水坩埚在红外线吸收法测定连铸保护渣游离碳含量中的应用

准确分析连铸保护渣中的游离碳成分 ,对提高连铸坯质量和连铸操作的稳定性都起着非常重要的作用。近年奉冬文[1] 及杜建民[2 ] 曾分别发表了难熔碳化物中游离碳的快速测定及铁沟料中游离碳和碳化硅的高频炉燃烧红外光谱测定。但关于连铸保护渣中游离碳的测定迄今尚未见报道。作者等于1998～ 2 0 0 1年间 ,按冶信标院的要求起草了连铸保护渣游离碳化学分析行业标准。其方法是将试样经酸溶分解 ,以玻璃漏斗加衬瓷滤片和酸洗石棉过滤 ,转移至瓷舟或坩埚中 ,用管式炉内燃烧气体容量法或红外线吸收法进行测定。1　仪器与试剂ＣＳ 4 44型红外线吸…     

气相耗材对系统性能的影响

 叙述了气相耗材如气体过滤器、柱卡套、进样口密封垫、衬管等的性能及其选择和安装对系统运行的影响 ,指出要想使气相系统保持最佳运行状态 ,必须有性能优良、干净及选择得当的耗材作保证。     

纤维素衬层压片-X射线荧光光谱法测定砂岩型铀矿中9种主次元素

目的是采用粘结性强、腐蚀性低有机纤维素替换粉末压片法中硼酸衬层,降低硼酸衬层在样品分析过程中受热挥发,分散的硼酸粉末附着于仪器金属部件、滤光片、准直器,硼酸粉尘累积,增加仪器维护保养成本甚至会影响仪器运行和检测结果等不良影响。方法研究其有机纤维素作为衬层可能性及对样品检测结果的影响,微晶纤维粉改善砂岩型铀矿样品的过程中会出现样品粘结性差、分层和裂纹的效果。结果该方法测定砂岩型铀矿中9种主次元素的精密度(RSD,n=11)为0.34-4.76%,准确度为0.06-5.52%,相较于硼酸衬层和未添加辅助粘结剂样品的测定值,应用格拉布斯法检验各元素统计量G均在1.25-1.40%之间。结论采用羟甲基纤维素作为衬层可用于砂岩型铀矿中主次元素的测定,添加微晶纤维素0.5g可改善矿石粘结性能,提升实验制备样片的稳定性,降低了样品分析对仪器金属部件及检测效果的影响。     

用衬钨钽金属热解石墨管原子吸收法测定稀土等十七个元素

用热解石墨管(PGT)测定稀土等高温元素存在着严重困难。为此,曾在石墨管中衬钽片测定了一些高温元素,但是未报道钽片的寿命和测定精密度。文献[2,3]采用上述方法测定稀土元素和铀,     

测定甲醇合成气中微量硫化物的注意事项

根据微量硫分析仪测定人工煤气中微量硫化物的原理和仪器本身的特点，分析了用该法测定甲醇合成气中微量硫化物时，温度、气体配比等因素对测定结果的影响，指出了测定时应注意的事项。     

Thermodynamic simulation and experimental investigation of reactive chemical vapor deposition in the Ta–C–Si–O–F system

Reactive deposition processes of tantalum carbide are studied experimentally and theoretically in the Ta–C–Si–O–F system. It is shown that Sio₂ substantially affects the carbide formation process. This is expressed in a decreased efficiency of tantalum transfer from the source zone to the crystallization zone, the possibility of bilateral transport of tantalum to carbon and carbon to tantalum, the complicated composition of condensed phases in the equilibrium with the gas phase. Aspects of preparing single crystal tantalum oxyfluoride are considered.     

钽丝圈原子化器原子吸收光谱法的研究

用自制的钽丝圈原子化器与原子吸收光谱仪联用,以氩气为保护气,测定了Ｃｄ、Ｃｕ和Ｚｎ,研究了这一原子化器的性能。在选定的仪器工作条件下,测定Ｃｄ,Ｃｕ和Ｚｎ的特征浓度分别为２、３０和７ｎｇ／ｍＬ。对实际样品中的Ｃｕ、Ｚｎ和Ｃｄ进行测定,其结果令人满意。     

Colorimetric determination of tantalum in titanium alloys

Experimental work on tantalum-titanium alloys has been handicapped by the lack of accurate methods for the determination of the tantalum. In this paper a colorimetric procedure is proposed for the determination. The tantalum is separated completely from the titanium by two tannin precipitations with an intervening digestion with tannin. The tannin precipitate is ignited, fused with potassium bisulfate and the melt taken up with ammonium oxalate solution. Pyrogallol is then added and the intensity of the yellow color is measured. A study was made of the tantalum pyrogallol color to obtain optimum conditions. Elements that would be found in the usual tantalum-titanium alloys do not interfere with the method. More than 0.0025 gram of niobium interferes by cauaing occlusion of titanium by the tannin precipitate. This causes high results for tantalum, since titanium reacts with pyrogallol to produce a yellow color. The presence of more than 0.0050 gram of tungsten causes high results for tantalum because tungsten is partially precipitated by the tannin and reacts with pyrogallol to produce a yellow color. The proposed method is recommended for tantalum-titanium alloys containing 0.05 to 5 percent, tantalum.     

简便、廉价的电热原子化器的应用研究

将自制钽丝圈原子化器与原子吸收光谱仪联用,以氩气作保护气,测定了Ｃｄ、Ｃｕ、Ｍｎ、和Ｐｂ,研究这一原子化器的性能。在选定的仪器工作条件下,测定Ｃｄ、Ｃｕ、Ｍｎ和Ｐｂ的特征质量浓度分别为０．７μｇ／Ｌ、１７μｇ／Ｌ、２８μｇ／Ｌ和３１μｇ／Ｌ。对实际样品中的Ｃｕ和Ｍｎ进行了测定,其结果令人满意。该法具有简便、廉价的特点。     

Application of on-line HPLC-ICP-MS for the determination of the nuclide abundances of lanthanides produced via spallation reactions in an irradiated tantalum target of a spallation neutron source

An analytical procedure has been developed for the determination of spallation nuclides in an irradiated tantalum target using HPLC coupled on-line to ICP-MS after dissolution and separation of the tantalum matrix. Pieces of tantalum were taken from different locations of the irradiated tantalum target which had been used as the target material in a spallation neutron source. Tantalum was dissolved in a HNO₃/HF mixture and the tantalum matrix was separated by liquid-liquid extraction so that only the spallation nuclides were left in the sample solutions. The major fraction of the spallation nuclides in the tantalum target are lanthanide metals in the μg g^–1 concentration range determined in the present study. Additional reaction products are formed by the irradiation of trace impurities in the original tantalum target. The nuclide abundances of the lanthanide metals measured in the tantalum target differ significantly from the natural isotopic composition so that a lot of isobaric interferences of long-lived radionuclides and stable isotopes in the mass spectrum are to be expected. Therefore, all the lanthanide metals had to be separated chemically prior to their mass spectrometric determination. The separation of all rare earth elements was performed by ion chromatography on-line to ICP-MS. The nuclide abundances of each lanthanide were determined using a sensitive double-focusing sector field inductively coupled plasma mass spectrometer. The nuclide abundances of the lanthanides in the irradiated tantalum target calculated theoretically and the experimental results obtained by on-line HPLC-ICP-MS proved to be in good agreement.     

Interaction of tantalum fluoride with organic solvents

A systematic study on the extraction of tantalum fluoride from various acidic solutions and mixed media has been given using HDEHP, TBP and LA-2 as solvents. The results obtained for these three solvents clarify the ionic behaviour of tantalum. The separation of tantalum from other elements is discussed.     

Determination of niobium and tantalum in binary alloys and zirconium alloys

Recent developments in the metallurgy of niobium, tantalum and zirconium have necessitated provision of analytical procedures for determining niobium and tantalum in the presence of each other and in the presence of zirconium. For this purpose, absorptioinetric procedures based on the formation of yellow coloured complexes, between pyrogallol and niobium or tantalum, have been critically examined. Direct absorptiometric procedures are described, which are suitable for determining niobium or tantalum in the range 2 to 7%; when either of these metals exceeds 7%, differential absorptiometric procedures are recommended. Corrections must lie made for absorption due to the presence of other metals which form complexes with pyrogallol. In tlie determination of niobium or tantalum up to 5%, the precision of the method is about ±0.05%. About 12 determinations can be made in a day, by one analyst.     

Separation and determination of tantalum and niobium by precipitation from homogeneous solution

An attempt to separate niobium and tantalum by precipitation from homogeneous solution by thermal decomposition of their peroxy complexes, in the presence of tannin and oxalate, has been only moderately successful. A more satisfactory separation of tantalum and niobium for ratios from 50:1 to 1:30 is obtained by extracting the bisulphate melt with ammonium oxalate before adding hydrogen peroxide, hydrochloric acid and tannin. For a tantalum/niobium ratio of 1:1 the niobium coprecipitation is reduced to 5 %. Furthermore, two alternative possibilities are presented: (1) a quantitative recovery of a tantalum precipitate at small oxalate and high tannin concentration, leaving 90% of the tantalum-free niobium in solution; (2) an 85 % recovery of niobium-free tantalum at high oxalate and small tannin concentration. A study of the coprecipitation process of niobium shows that the distribution coefficients follow a logarithmic pattern, true homogeneous mixed crystals being formed.     

Separation of trace concentrations of tantalum from niobium and some other heavy metal ions by extraction with N-oxide of trioctylamine

The distribution of tantalum(V) between 0.1M trioctylamine oxide dissolved in xylene and sulphuric acid solutions has been studied. On the basis of results on the distribution, it is concluded that at sulphuric acid concentration 0.5M, tantalum is probably extracted by a solvate mechanism as the complex Ta(OH) (SO₄)₂·3TOAO. It has also been shown that tantalum can be quantitatively separated from niobium, uranium, thorium and rare earth elements by extraction with N-oxide of trioctylamine from 0.5M sulphuric acid solution.