能量色散-X射线荧光光谱测定中草药痕量镉、铅、铜

为寻求一种能够直接对中草药中重金属进行快速检测的方法,采用压片法对样品进行前处理,建立了能量色散-X射线荧光光谱法快速检测中草药中痕量重金属镉、铅、铜元素的方法。在20 min即可完成检测,镉、铅、铜检出限分别为0.072、0.207、0.340 mg/kg,测试结果表明与原子吸收和ICP-MS相比,本方法数据稳定性和准确度良好,具有快速、准确、简单的优点,能够满足药典中对重金属元素的限量要求,适用于现场快速检测与质量控制检测。     

Elemental analysis in solutions by radioisotope excited X-ray fluorescence

The problem of spectrochemical analysis of elements in solutions has been investigated for a number of elements across the periodic table using radioisotope-induced energy dispersive X-ray fluorescence method. In this study a low intensity¹⁰⁹Cd X-ray source was used for characteristic X-ray excitation. Experimental parameters such as saturation thickness and critical thickness have been studied to evaluate their role in this method. Minimum detection limits, sensitivities and the nature of concentration calibration at critical thickness have been obtained as a function of Z to find the limits of the method. Results obtained have been discussed in the light of theories and potential areas of applicability of the method have been indicated.     

Determination of lead in metallic reference materials by laser ablation combined with laser excited atomic fluorescence

Concentrations of lead in the range 0.15–750 μg⁻¹ were measured in metallic matrices (copper, brass, steel, and zinc) by laser excited atomic fluorescence combined with UV laser ablation in a low-pressure (130 mbar) argon atmosphere. The mass of material ablated was determined by repetitive weighing of the target prior to and after approximately 10 000 ablating shots. The fluorescence was excited after a 100 μs delay relative to the ablation pulse. A long integration time of 200 s was used to provide a representative determination of bulk concentrations. No matrix effect was observed, providing a universal calibration curve for all samples with relative standard deviations of about 20%. The relative and absolute limits of detection were 72 ng g⁻¹ and 0.5 fg, respectively.     

Determination of silver in lead by neutronactivation analysis

Submicrogram amounts of silver have been determined in lead by neutron-activation analysis. The activity of the ¹¹⁰Ag isotope was measured by following the decay of the 0·66-MeV gamma ray. Reproducibility was generally better than 10%. The smallest amount of silver determined was approximately 0·02 μg. The analyses were completed within 15 min.     

Determination of lead in household refuse fly-ash by X-ray fluorescence spectrometry and a modified standard-addition technique

Lead in fly-ash from a garbage incinerator has been determined by X-ray fluorescence spectrometry (XRFS) and a modified standard-addition method. To keep the attenuation properties of the spiked samples constant, decreasing amounts of an attenuation modifier [mercury (II) acetate] were added together with increasing amounts of the standard (lead nitrate). Linearity between fluorescence intensity and amount of lead was thus obtained, so the amount of lead in the sample could be evaluated by linear regression. The amount of modifier needed could be calculated from a simple expression. The method was validated by comparison with the results obtained by applying atomic-absorption spectrometry (AAS) to solutions made by leaching the fly-ash with strong acid. For 8 fly-ash samples, containing between 0.8 and 1.35% lead, the largest absolute difference between the two sets of results was 0.03%. Theoretical calculations based on a simplified version of the Sherman equation were performed to confirm the linearity of the modified standard-addition curves.     

Determination of lead concentration and film thickness in electroluminescent calcium sulfide thin films by X-ray fluorescence

Summary For the analysis of electroluminescent thin films, X-ray fluorescence (XRF) provides a convenient method as both the concentration of the dopant and the film thickness can be determined rapidly and non-destructively. An XRF method for the determination of thickness and lead concentration in lead doped calcium sulfide thin films was developed. Calibration standards made of polyvinyl alcohol and gelatin as well as filter paper standards were used. In addition, the applicability of a fundamental parameter program UniQuant was investigated. For comparison, the concentrations of lead and calcium were determined after dissolution by atomic absorption spectrometry. Generally, the correlation between the different methods excluding the use of filter paper standards was satisfactory. When the dopant concentration was very low or very high, however, the fundamental parameter program yielded best results. Determination of thicknesses by XRF was made by comparing the sulfur K intensities of the sample and those of a zinc sulfide standard. A correction factor for molar masses and densities was applied. The thicknesses obtained were compared to those measured with a profilometer after etching and the deviations were found to be less than 10%.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

Determination of gold in silver, copper, lead, selenium and anode slime by atomic-absorption spectrometry

A simple and sensitive combined solvent-extraction and atomic-absorption spectrometric method has been developed for the determination of gold in silver, copper, lead, selenium and anode slime. Samples are decomposed with hydrochloric and nitric acids, and gold is extracted as the trioctylmethylammonium-gold bromide complex and determined by atomic-absorption spectrometry by direct spraying of the extract into the flame. Optimal conditions for the extraction and determination of gold have been established. As little as 0.5 mug of gold in a sample can be determined. The extraction of gold from hydrochloric or hydrobromic acid solution with trioctylamine or trioctylmethylammonium chloride (or bromide) has also been investigated.     

Determination of copper,iron and zinc in spirituous beverages by total reflection X-ray fluorescence spectrometry

The concentration of copper in traditional homemade alcoholic distillates produced in Venezuela (Cocuy de Penca) were determined by total reflection X-ray fluorescence (TXRF) using vanadium as internal standard. The results were compared to those obtained by flame atomic absorption spectrometry (FAAS). Three preparative methods of addition of vanadium were compared: classical internal standard addition, ‘layer on layer’ internal standard addition and in situ addition of internal standard. The TXRF procedures were accurate and the precision was comparable to that obtained by the FAAS technique. Copper levels were above the maximum allowed limits for similar beverages. Zinc and iron in commercial and homemade distilled beverages were also analyzed by TXRF with in situ addition of internal standard demonstrating the usefulness of this technique for trace metal determination in distillates.     

波长色散X射线荧光光谱法测定钴精矿中钴、铜和锰含量

采用高纯氧化物经四硼酸锂和偏硼酸锂熔融制备人工标准样品,以氧化镱为内标,制作校准曲线,建立了波长色散型X射线荧光光谱法测定钴精矿中钴、铜、锰元素的分析方法。重点研究了混合熔剂、试样稀释比、氧化剂和内标选择、方法检出限、方法准确度和精密度等,结果表明,各元素校准曲线线性范围宽,相关系数均大于0.999, 钴、铜、锰元素检出限分别达到0.002%、0.001%和0.001%,测试准确度和精密度可靠,方法满足行业检测需求。     

The simultaneous determination of gold and silver in blister copper and speiss products

A method for determination of silver and gold (concentration ranges of 0.1–0.4% and 8·10^–4–3·10^–3% respectively) in blister copper and speiss is described. Silver is determined directly in the solution after dissolution of the sample and appropriate dilution. The amount of gold is determined in an aliquot of the same solution after extraction with methyl isobutyl ketone. The relative standard deviation of the method described is 3.3% for speiss and 4.4% for blister copper for gold and 1.6% and 2.5% for silver respectively.     

Extraction-spectrophotometric determination of traces of gold in copper in silver, lead, blister copper, copper concentrate and anode slime with 4,4'-bis(dimethylamino)-thiobenzophenone

A sensitive spectrophotometric method has been developed for the determination of gold in copper, silver, lead, blister copper, copper concentrate and anode slime. Optimal conditions have been established for the extraction and determination of gold. Gold is extracted as its bromo complex with tri-n-octylamine and determined photometrically with 4,4'-bis(dimethylamino)thiobenzophenone; the absorbance of the organic phase is measured at 540 nm and the apparent molar absorptivity is about 1.2 x 10(5) 1.mole(-1). cm(-1). As little as 0.1 or 0.2 ppm of gold in these materials can be determined.     

X射线荧光光谱法测定除尘灰中砷、铅含量

以熔融制样法,采用X射线荧光光谱对除尘灰中的有害元素：砷、铅含量进行了测定。对样品的烧失温度进行了讨论,发现在950℃灼烧温度下灼烧2h时除碳完全。砷和铅的相对标准偏差为0.15 %和0.20 %。测试结果与化学分析法、原子吸收光谱法等相吻合。该方法制作工艺简单,分析速度快,样品可长期保存,还能满足其他元素的日常分析。     

X-ray fluorescence analysis of lead in leaves

The analysis of samples by means of X-ray fluorescence spectrometry has been used to monitor environmental pollutants in a collaborative project between the Department of Physics, the Centre for Materials Science of the University of Birmingham and latterly the University of Manitoba. Lead was chosen as the element of greatest environmental interest and the abundance of tree linedroads in the vicinity of the University suggested that leaves would be a conveninent sampling medium for the investigation of atmospheric lead concentration in areas of high traffic density.     

Determination of calcium in uranium by X-ray fluorescence

Summary An X-ray fluorescence method for the analysis of calcium in uranium in the range of 20 to 500 ppm is described. U₃O₈ samples are mixed with boric acid binder and double-layer pellets are prepared. The pellets are analysed using Philips PW 1220 semi-automatic X-ray spectrometer. Calculated lower limits of detection are better than 5 ppm for calcium in uranium.

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Bestimmung von Calcium in Uran durch Röntgenfluorescenz

Zusammenfassung Ein Verfahren für den Bereich von 20–500 ppm wird beschrieben. Die U₃O₈-Proben werden mit BorsÄure als Bindemittel vermischt zu Doppelschicht-Tabletten gepre\t, die mit Hilfe eines halbautomatischen Philips PW 1220 Röntgenspektrometers analysiert werden. Die untere Nachweisgrenze liegt bei 5 ppm Ca.

     

Determination of gold by X-ray fluorescence methods

X-ray fluorescence methods for the determination of gold in silver beads and in hydrochloric acid solutions are described. These techniques may be applied to silver containing 0.2-5 % of gold and to solutions containing 0.004-0.1% of gold. Platinum, palladium, rhodium and indium do not interfere.     

X-ray fluorescence spectrometry of copper intermediates

Iron, magnetite, copper, copper(II) oxide, calcium carbonate, sulphur, silicon dioxide and aluminium oxide as components of copper intermediates (concentrates, slags, mattes, calcines and fluxes) in powdered (300-400 mesh) binary mixtures obey the Lachance-Traill equation, so the coefficients alpha(AX) of interelement effects can easily be determined experimentally. They show a reasonable agreement with the theoretical values calculated from mass absorption coefficients. This fact can be the basis of a convenient routine method for the determination of intermediates. Since the intermediates exhibit differences in the distribution of their atoms (microcosmic inhomogeneity) a correction factor k(dist) has to be used. Its value for the main components (concentrations > 5%) is in the range 0.92-1.24 The highest relative average deviation of the results from those of the classical "wet" methods is 2.7% for the major and 30% for the minor components.     

Determination of lead in fresh and canned pineapple by isotope dilution mass spectrometry and isotope systematics

Pineapple stored in welded and soldered can was analysed for lead to assess the extent to which it is contaminated during processing and storage. To avoid contamination during analysis the samples were prepared in clean laboratory using ultra-clean procedures. The lead concentration was determined by isotope dilution mass spectrometry and the sources of lead were identified by their isotopic signature and quantified by isotope systematics. The results showed that the lead concentration in pineapple stored in the soldered cans (ca. 150 ng g^?1) was about 2.5 times that found in the welded cans and 60–80% of this lead was traced to the soldered joint using isotope systematics. The edible portion of a fresh pineapple contained < 0.85 ng g^?1 lead, showing that even pineapple in welded cans may be contaminated 80 times more than the natural level.     

Investigation of adsorbed mercury distribution in silver coated filters by X-ray fluorescence

We have been working on mercury collection from flue gas by amalgamation and subsequent XRF analysis. Previous results showed unexpectedly high relative standard deviation (30%) in collection efficiency when silver-coated filters were exposed to gas phase mercury in a pilot-scale test chamber. Filters were analyzed by micro-XRF, TXRF and conventional XRF to explore the source of scattering. It was concluded that mercury had inhomogeneously adsorbed in the filter as the cause of this variation, leading to a positive bias of 50% in efficiency value. Results reported in this paper suggest the TXRF method is accurate to within ±10% when X-ray counting statistics are not the limiting factor. Application of this filter in flue gas measurement will be presented.