阀切换-离子色谱法测定高纯硼酸中的痕量阴离子

研究了高纯硼酸中痕量阴离子的离子色谱测定方法.建立了使用阈切换技术联合离子色谱同时测定高纯硼酸中痕量阴离子的检测方法.样品经水溶解后,通过阀切换技术,使用蠕动泵和IonPac TAC-ULPI超低压浓缩柱,消除基体中硼酸根的干扰,同时在线富集样品中的阴离子,最后使用IonPac AS15分析柱进行分离.在20～500μg/L浓度范围内,7种常见阴离子的工作曲线的线性相关系数r均优于0.995,对硼酸样品进行加标,7种阴离子的平均回收率为90%～106%.该方法可应用于高纯硼酸中痕量阴离子的检测.     

Determination of indium in high purity antimony by electrothermal atomic absorption spectrometry (ETAAS) using boric acid as a modifier

The use of boric acid as a modifier for the determination of trace amount of indium in high purity antimony by electrothermal atomic absorption is described. It was found that the negative influence of the hydrofluoric acid, used for the digestion could not be eliminated by using stabilized temperature platform furnace (STPF) alone. Due to the high dissociation energy (D₀ = 506 kJ mol⁻¹) of indium fluoride, it is difficult to dissociate in the gas phase and hence is lost. In presence of HF (used for the dissolution of antimony), the universal Pd-Mg modifier does not work satisfactorily. Additionally, rising corrosion and reduced tube lifetime were observed when the acid digested (HF-HNO₃) antimony solution was injected in to the platform. Improvement in platform life and elimination of interferences were achieved by the addition of boric acid as a chemical modifier together with ruthenium coating of the platform. Corrosive changes of the transversely heated graphite atomizer (THGA) platform surface were examined by scanning electron microscopy. The standard addition method was applied. A characteristic mass of 36 pg was obtained. The detection limit of the proposed method is around 0.04 μg g⁻¹. The developed method was applied to the determination of indium in real samples. The data obtained by this method were in good agreement with those obtained by ICP-MS.     

石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙

以甘露醇为基体改进剂,建立石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙含量的方法。考察基体改进剂用量、灰化温度、原子化温度、基体干扰以及共存离子干扰对测定结果的影响,确定最佳测定条件:以硼含量为1000 mg/kg的硼酸为背景基体,加入适量甘露醇,样品作酸化处理,灰化温度为1700℃,原子化温度为2450℃。钙含量在8~32 μg/kg范围内与光谱强度成良好的线性关系,相关系数为0.9996,方法检出限为1.79 μg/kg。对于硼基体含量为0~2500 mg/kg的样品,测定结果的相对标准偏差为0.5%~7.5%(n=6),相对误差不大于13.2%,加标回收率为93.9%~113.3%。该方法检测速度快,结果准确,能满足实际生产要求。     

Thermodynamics of aqueous solutions of boric acid

Vapor pressures of aqueous solutions of boric acid over a wide range of acid concentrations were measured from 40 to 100°C. The results, together with solubility data taken from the literature, can be described with a thermodynamic model which uses the Wilson equations to express the activity coefficients of water and boric acid. Only three temperature independent adjustable parameters are required; one of these represents the entropy of fusion of boric acid, data which are not available in the literature.     

Determination of traces of rubidium in high purity cesium chloride by electrothermal atomic absorption spectrometry (ETAAS) using boric acid as a modifier

The use of boric acid as a modifier for the determination of trace amount of rubidium in high purity cesium chloride matrix by electrothermal atomic absorption is described. It was found that the negative influence of the chloride matrix could not be eliminated using stabilized temperature platform (STPF) alone. Due to the high dissociation energy (D₀ = 427 kJ mol⁻¹) of rubidium chloride, it was difficult to dissociate in the gas phase and hence is lost. Elimination of interferences was achieved by the addition of boric acid as a chemical modifier. Diluted cesium chloride samples (5%, m/v) were analyzed applying the standard addition method. The characteristic mass of 24 pg was obtained. The detection limit of the proposed method is around 26 ng g⁻¹. The developed method was applied to the determination of traces of rubidium in high purity cesium chloride samples. The data obtained by this method were in good agreement with those obtained by other independent method like FAAS.     

Determination of the hydrogen content in Nigeria palm oil by the neutron moderation method

The thermal neutron moderation analysis facility at the Institute of Experimental Physics, Debrecen, Hungary has been used to determine the weight percent of total hydrogen content in Nigerian palm oil. The facility utilizes the fast neutron moderation technique in which the intensity of reflected thermalized neutrons is proportional to the hydrogen content of the sample exposed to fast neutrons. Using a 100 cm³ sample the total hydrogen content in the oven-dry palm oil sample was found to be 12.0±0.1% within a measuring time of 5 minutes. The method is fast and can be used in plant quality control where the hydrogen content must be determined within specific limits.     

微波消解-电感耦合等离子体原子发射光谱（ICP-AES）法测定镍基耐蚀合金中镍

采用微波消解法与电感耦合等离子体原子发射光谱(ICP-AES)法相结合的方式,建立了镍基耐蚀合金中镍元素含量的测定方法。试样在浓硝酸和浓盐酸中微波消解后,用电感耦合等离子体原子发射光谱仪在优化的工作参数下测定,结果表明,稀释的消解液可直接用于镍含量的测定,光谱干扰少。对镍基耐蚀合金中镍含量进行多次平行测定,相对标准偏差(RSD,n=7)为0.29%,且测得值与标准值结果一致。对不同的镍基耐蚀合金样品进行加标回收实验,加标回收率在98.5%~102%。标准物质验证实验表明,测得值与标准值一致。     

Effect of boric acid on tetrafluoroborate ion hydrolysis in solutions of tetrafluoroboric acid

The presence of boric acid in tetrafluoroboric acid solutions enhances the BF₄^- ion hydrolysis. An increase of the boric acid content in a 32% HBF₄ solution from 0.1% to 3.8% is accompanied by a simultaneous increase of the degree of hydrolysis from 4.8% to 30.5%.     

Determination of cadmium in zinc ores by thermal neutron absorption analysis

A method has been developed for routine determination of cadmium in zinc ores by thermal neutron absorption analysis, based on the attenuation of a thermal neutron flux passing through a neutron absorbing material. The thermal neutron flux is related to the⁵²V-activity induced in a vanadium detector, surrounded by pellets pressed from a mixture of powdered material with graphite. Besides cadmium, also the major constitutents zinc, iron and sulfur contribute significantly to the total attenuation of the thermal neutron flux. Calibration lines for these elements are worked out. All irradiations are carried out for 200 s in the partially thermalized neutron flux of a 5 Ci²²⁷Ac—Be isotope neutron source. After a decay of 30 s, the⁵²V-activity of the vanadium detector is measured for 400 s with a NaI(T1) scintillation detector. The analysis sequence, including the computation of the results from the counting data, is automated by means of a LSI—11 microprocessor with 12K×16 bit memory. Zinc ores, containing 0.02 to 1.45% cadmium, have been analyzed with a precision ranging from 12.6% to 0.54% relative. As a test for the reliability of the method, two NBS standard reference materials were analyzed in the same way as the zinc ore samples.     

石墨炉原子吸收测定模拟体液中的镍

人工关节置换手术的出现是外科手术治疗软骨病损的一次巨大的进步。但人工关节假体的后期松动是长期困扰其发展的难题。镍钛合金人工关节假体材料在体液中的腐蚀与磨损,以及磨损颗粒引起周围组织的异物反应,是造成晚期关节假体松动的主要原因。另一方面,镍钛合金植人体在体液腐蚀下释放的镍离子对人体有害,而且还可能致癌。因此,对镍钛合金进行表面改性,以提高其耐磨与耐腐蚀性能很有必要。     

Determination of the bitumen content in asphalt concrete using a neutron reflection method

A neutron physical method for the fast, nondestructive determination of the bitumen content in asphalt concrete has been developed. The determination is performed on cylindrical asphalt concrete samples containing desiccated rubble matrix. Using samples of ～1000 g and measuring times of 20 min, the reproducibility of the bitumen determination is ±0.15 w%, the sensitivity is 3·10^?3 g/g.     

Separation of fission and corrosion products from boric acid solutions by solvent extraction

Extractive purification of boric acid from radioactive corrosion and fission products dissolved in aqueous solutions modelling nuclear reactor coolants has been studied. Aliphatic 1,3-diols containing 8 and 9 carbon atoms per molecule were used as extractants fro boric acid. The behaviour of some representative corrosion and fission products as well as various factors affecting their distribution between the organic and aqueous phases have been investigated under the conditions of boric acid extraction. Conditions for the effective separation of boric acid from most of the radioactive contaminants are presented.     

Determination of structures of cupric-chloro complexes in hydrochloric acid solutions by UV-Vis and X-ray absorption spectroscopy

Structural Chemistry - Ultrahigh-purity metals are indispensable to understanding the nature of materials, but the purity of contemporary metals is insufficient for determining their intrinsic...     

Determination of boron in glass by neutron transmission method

Neutron transmission method has been used for the determination of boron in borosilicate glasses. The method is sensitive and rapid to control the spatial homogeneities of glass-product in the melting furnace.Dedicated to Academician J. Csikai on his 60th birthday.This work was supported by the National Foundation for Research (Contact No. 259).     

高频燃烧红外吸收法测定钢铁中超低碳硫

通过对气体净化,坩埚处理,试样处理及称样量选择,助熔剂种类及用量等因素的优化,建立了钢铁中超低含量碳硫的测定方法,实验结果表明：比较器水平设为1%,分析时间设为45 s,坩埚在1350 ℃下预烧45 min,选择钨作为助熔剂且使用前在140 ℃烘3 h,助熔剂用量为1.5 g,称样量为0.5 g时,是分析钢铁中碳硫含量在0.01～0.001 %的最佳条件,方法重复性好,准确度高,在实际操作中切实可行。     

Electronic absorption spectrum of perylene radical cation trapped in boric acid film

A detailed spectroscopic analysis of the electronic absorption spectrum of the perylene radical cation, produced in a boric acid film by photo-oxidation is reported. To interpret the experimental spectrum, the electronic energy levels and oscillator strengths have been calculated using the Pariser—Parr molecular orbital method with limited configuration interaction. The effect of variation of solute concentration and irradiation time of the films has also been studied. It is found that the agreement between experimental and theoretical results in excellent.     

高效液相色谱法测定松针中莽草酸的含量

松针为我国传统中药,<本草纲目>曰:松针,味苦温、无毒,久服令人不老,轻身益气,主治风湿疮,生毛发,安五脏,守中,不饥,延年[1].历代均入药用,民间用于治疗神经衰弱、维生素丙缺乏症、营养性水肿、风牙肿痛、阴囊湿痒、腰痛、跌打损伤和预防钩虫病[2].现代临床医学上常用以治疗慢性气管炎、预防流脑和感冒.