Determination of uranium at ultratrace levels by time-resolved laser fluorimetry

Uranium at ultratrace levels in the pelleted cake from a NaF/Na₂CO₃/K₂CO₃ (10:45:45) fusion is determined by laser fluorimetry. Light scattering and fluorescence from impurities are greatly reduced by time-resolved fluorimetry. The optimum excitation wavelength is shown to be 360 nm from the signal-to-background ratio spectrum; emission is measured at 555 nm. The detection limit is 9 ng kg^?1 for a standard uranium sample. Relative standard deviations in the determination of ca. 50 ng kg^?1 uranium in silica samples are about 10%.     

Direct determination of uranium in seawater by laser fluorimetry

A method for estimation of uranium in seawater by using steady state laser flourimetry is described. Uranium present in seawater, in concentration of approximately 3 ng ml⁻¹ was estimated without prior separation of matrix. Quenching effect of major ions (Cl⁻, Na⁺, SO₄⁻, Mg⁺, Ca⁺, K⁺, HCO₃⁻, Br⁻) present in seawater on fluorescence intensity of uranium was studied. The concentration of phosphoric acid required for maximum enhancement of fluorescence intensity was optimized and was found to be 5%. Similarly the volume of concentrated nitric acid required to eliminate the quenching effect of chloride and bromide completely from 5 ml of seawater were optimized and was found to be 3 ml. A simple equation was derived using steady state fluorescence correction method and was used for calculation of uranium concentration in seawater samples. The method has a precesion of 1% (1 s, n = 3). The values obtained from laser fluorimetry were validated by analyzing the same samples by linear sweep adsorptive stripping voltametry (LSASV) of the uranium-chloranilic acid (2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone) complex. Both the values are well in agreement.     

Estimation of uranium in bioassay samples of occupational workers by laser fluorimetry

A newly established uranium processing facility has been commissioned at BARC, Trombay. Monitoring of occupational workers is essential to assess intake of uranium in this facility. A group of 21 workers was selected for bioassay monitoring to assess the existing urinary excretion levels of uranium before the commencement of actual work. Bioassay samples collected from these workers were analyzed by ion-exchange technique followed by laser fluorimetry. Standard addition method was followed for estimation of uranium concentration in the samples. The minimum detectable activity by this technique is about 0.2 ng. The range of uranium observed in these samples varies from 19 to 132 ng/L. Few of these samples were also analyzed by fission track analysis technique and the results were found to be comparable to those obtained by laser fluorimetry. The urinary excretion rate observed for the individual can be regarded as a ‘personal baseline’ and will be treated as the existing level of uranium in urine for these workers at the facility.     

Uranium/plutonium and uranium/neptunium separation by the Purex process using hydroxyurea

Hydroxyurea dissolved in nitric acid can strip plutonium and neptunium from tri-butyl phosphate efficiently and has little influence on the uranium distribution between the two phases. Simulating the 1B contactor of the Purex process by hydroxyurea with nitric acid solution as a stripping agent, the separation factors of uranium/plutonium and uranium/neptunium can reach values as high as 4.7·10⁴ and 260, respectively. This indicates that hydroxyurea is a promising salt free agent for uranium/plutonium and uranium/neptunium separations.     

Uranium/plutonium and uranium/neptunium separation by the Purex process using hydroxyurea

Hydroxyurea dissolved in nitric acid can strip plutonium and neptunium from tri-butyl phosphate efficiently and has little influence on the uranium distribution between the two phases. Simulating the 1B contactor of the Purex process by hydroxyurea with nitric acid solution as a stripping agent, the separation factors of uranium/plutonium and uranium/neptunium can reach values as high as 4.7·10⁴ and 260, respectively. This indicates that hydroxyurea is a promising salt free agent for uranium/plutonium and uranium/neptunium separations.     

A comparative analysis of uranium in potable waters using laser fluorimetry and ICPMS techniques

The main objective of this work is the accurate measurement of uranium in the potable water sources of Muktsar district of Punjab, India. In the present work, a laser fluorimetry technique was used for the analysis of uranium. Inductively coupled plasma mass spectrometry (ICPMS) technique was also applied to verify and compare the uranium content analyzed using laser technique. About 16 samples from waterworks, bore wells, and hand pumps that supply the drinking water to local population were collected for this purpose. An indigenous laser fluorimeter supplied by RRCAT, Indore was employed for the analysis. Uranium concentrations obtained were in the range from 0 to 10???g?L^?1 in ten samples, 11?C30???g?L^?1 in three samples, and more than 100???g?L^?1 in three samples namely Channu ground water, Warning Khera pump, and Killanwale village hand pump. The USEPA guideline value for uranium in safe drinking water is 30???g?L^?1. Also, a data comparison with similar studies carried out in other countries is presented.     

An improved laser fluorimeter for the detection of traces of uranium

An improved laser fluorimeter and its application for the determination of ultratrace concentrations of uranium are described. The system developed uses a collecting lens-filter system, by which the density of laser radiation on the sample is increased greatly and the interfering stray light can be reduced to a great degree. In addition, both laser and lamp sources are joined together in the instrument. A strong green phosphor from uranium-doped sodium metaphosphate (NaPO₃: U) has been found suitable and has been used for the determination of ultratraces of uranium. A detection limit (3) of 0.36 pg of uranium (in 30 mg NaH₂PO₄ per pellet) was obtained. In the case of peak-to-background intensity ratios relative standard deviations (RSD) are 6.4% and the linear dynamic range extends from 1 pg to 10³ ng of uranium.     

荧光法测定尿中的富马酸比索洛尔

建立了直接测定尿中富马酸比索洛尔的荧光分光光度法。荧光强度与富马酸比索洛尔含量在100－1000ng/mL范围内呈线性关系。检测限20ng/mL。对浓度100ng/mL与500ng/mL的标准溶液进行测定,其回收率分别为95．6％和99．6％,相对标准偏差为5．6％和2．3％,可用于 尿中富马酸比索洛尔含量的测定。     

Cold dissolution method for the determination of uranium in various geological materials at trace levels by laser fluorimetry

A cold dissolution procedure for the determination of uranium in various geological materials like rocks, minerals, soils etc., has been described. Samples are allowed to react with HF and HNO(3) at room temperature overnight. Boric acid is added to complex excess fluoride ions. From the clear solution thus obtained, uranium is determined directly in laser fluorimeter after the addition of fluorescence enhancing reagents. The results of few standard reference materials analysed by the present method agree with the certified values. This methodology does not require platinum or teflon ware, exhaust system and time consuming solvent extraction step. Hazardous acid vapours are not left in air, so there is no air pollution. Chemicals consumption is minimal. Therefore the method is economical. The method can be employed for high sample throughput which is the prerequisite for exploration geochemists.     

荧光光谱法测定奶制品中的三聚氰胺

三聚氰胺能够与荧光素在水溶液中发生作用,使荧光素的荧光强度增强,且在一定浓度范围内,荧光强度与三聚氰胺的浓度成线性关系,据此建立了一种新的测定奶制品中三聚氰胺的荧光分析方法。方法的回归方程为ΔI=178.2ρ(10-6g/L),r=0.9977,线性范围5.00×10-7~1.00×10-5g/L,RSD为1.9%(n=10),检出限为9.85×10-8g/L。采用该方法测定奶粉和液态奶中三聚氰胺的含量,测得的平均回收率分别为95.1%和95.8%。     

Determination of gentamycin by synchronous derivative fluorimetry

Use of synchronous first-derivative fluorimetry for determination of gentamycin is described. Gentamycin reacts with acetylacetone and formaldehyde in pH 5.6 HOAc/NaOAc buffer solution to form N-gentamyl-2,6-dimethyl-3,5-diacethyl-1,4-dihydropyridine[I] which is a fluorescent substance. Spectra of [I] and the reagent blank can be separated with synchronous derivative fluorimetry, and gentamycin can be determined directly. The synchronous spectral peaks of [I] and the reagent blank are at 434 and 411 nm, respectively. The first-derivative peak of [I] is at 425 nm. Effects of pH, foreign ions, buffer system, and heating time on the determination of gentamycin have been examined. The linear regression equation of the calibration graph is C=0.0513H-0.0416, with a correlation coefficient of linear regression of 0.9978. C means total potency of gentamycin: U ml(-1); H means peak height in the linear regression equation calibration graph. The linear range for the determination of gentamycin is from 0.00 to 3.00 U ml(-1). Recovery is from 95.06 to 112.0%, R.S.D. of 3.8%. The results determined by the fluorimetric method agreed roughly with those by the microbiological method. The method is simple and has low detection limit.     

催化荧光法测定痕量硒

基于稀硝酸介质中溴酸钾氧化藏红T,使其荧光猝灭,硒(Ⅳ)对此反应具有阻抑作用,使荧光强度增大,建立了催化荧光法测定痕量硒(Ⅳ)的新方法。方法检出限为0.12μg L,线性范围为0.5～10μg L。方法可用于测定水样中的硒(Ⅳ)。     

胶束增敏荧光法测定盐酸沙拉沙星

在pH 5.3的乙酸-乙酸钠缓冲溶液中,十二烷基苯磺酸钠能够敏化盐酸沙拉沙星的荧光,使λex=335 nnq、λem=450 nm的荧光增强.盐酸沙拉沙星质量浓度在0.10～6.99 mg/L范围内与荧光强度呈线性关系,方法检出限为9.16μg/L.6次平行测定方法回收率为91.8%～107.2%,相对标准偏差为1.6%～3.7%.常见金属离子及药物敷料对测定无干扰,不经分离直接用于兽药中盐酸沙拉沙星的测定.     

Determination of traces of rare earth elements in high-purity uranium by ion-exchange separation and neutron activation γ-spectrometry

Neutron activation γ-spectrometry is sufficiently sensitive for the determination of traces of rare earth elements but quantitative separation from uranium is essential. The rare earth elements in 0.2 M ammonium carbonate medium are quantitatively retained on Chelex-100, and are quantitatively separated from uranium by recycling the eluate. When 10-g samples are used, neutron activation provides detection limits of 1–20 μg kg^?1. Recoveries of rare earths, checked by spiking with radiotracers, are essentially complete.