Determination of antimony in wine by hydride generation graphite furnace atomic absorption spectrometry

 A method was developed for the determination of Sb in wine by electrothermal atomic absorption spectrometry, based on preconcentration by hydride generation with collection directly in the graphite furnace. Thiourea was added for prereduction of Sb(V) to Sb(III). The hydride was directly generated from diluted wine. Palladium was used as modifier in the collection step; the overall efficiency of the hydride/trapping system was found to be 67%. Sb was determined in several samples of red wine; the concentrations found were in the range 0.6 to 5.7 μg/L Sb. The detection limit of the method was 39 pg Sb, corresponding to 0.13 μg/L Sb in wine when 0.3 mL wine was analyzed. Received: 3 November 1995/Revised: 22 February 1996/Accepted: 24 February 1996     

Determination of antimony in wine by hydride generation graphite furnace atomic absorption spectrometry

 A method was developed for the determination of Sb in wine by electrothermal atomic absorption spectrometry, based on preconcentration by hydride generation with collection directly in the graphite furnace. Thiourea was added for prereduction of Sb(V) to Sb(III). The hydride was directly generated from diluted wine. Palladium was used as modifier in the collection step; the overall efficiency of the hydride/trapping system was found to be 67%. Sb was determined in several samples of red wine; the concentrations found were in the range 0.6 to 5.7 μg/L Sb. The detection limit of the method was 39 pg Sb, corresponding to 0.13 μg/L Sb in wine when 0.3 mL wine was analyzed. Received: 3 November 1995/Revised: 22 February 1996/Accepted: 24 February 1996     

石墨炉原子吸收法测定石脑油中微量砷

试样用四氢呋喃（THF）有机溶剂稀释,以硝酸镍为基体改进剂,研究采用石墨炉原子吸收法直接进样测定石脑油中的砷量。研究表明,砷量在0～50μg／L范围内线性关系良好,回收率93％～104％。     

Determination of antimony content in natural water by graphite furnace atomic absorption spectrometry after collection as antimony(III)-pyrogallol complex on activated carbon

Antimony(III) was preconcentrated on activated carbon (AC) as the antimony(III)–pyrogallol complex. Prior to the preconcentration, antimony(V) was reduced to antimony(III) with potassium iodide and ascorbic acid. The antimony adsorbed on the AC was determined by graphite furnace atomic absorption spectrometry as an AC suspension. The method was applied to differential determination of trace amounts of antimony in natural water.     

Determination of trace vanadium in sea cucumbers by ultrasound-assisted cloud point extraction and graphite furnace atomic absorption spectrometry

An ultrasound-assisted cloud point extraction (CPE) procedure was used for preconcentration and determination of vanadium by graphite furnace atomic absorption spectrometry. The vanadyl(IV) complex with ascorbic acid form a hydrophobic complex with 4-(2-pyridylazo) resorcinol (PAR) in a micelle medium, which is stable under our working conditions, and followed by its extraction into Triton X-100 surfactant-rich phase. The main factors affecting CPE efficiency, such as pH, concentrations of PAR, ascorbic acid and Triton X-100, incubation temperature, frequency and equilibration time of ultrasonic bath were investigated in detail. Under the optimum conditions, preconcentration of 10 mL sample gave a preconcentration factor of 36.4 and a detection limit of 4.0 µg kg^?1. The proposed method was successfully applied to determination of vanadium in sea cucumbers with satisfactory results.     

Determination of traces of molybdenum in sea water by combined anion-exchange — graphite furnace atomic absorption spectrometry

Summary Traces of molybdenum in sea water have been preconcentrated by anion-exchange from acidified samples in the presence of sodium azide. Molybdenum adsorbs strongly on a column of Bio-Rad AG 1 (Cl^–) and can be stripped easily by elution with 2 mol/l NH₄Cl — 2 mol/l NH₄OH solution. Molybdenum in the effluent is determined by graphite furnace atomic absorption spectrometry. The combined method allows to determine traces of molybdenum in sea water as well as non-saline water on a 100 ml sample basis. The method gives a relative standard deviation of better than 8% at a molybdenum level of 10 g 1^–1 of sea water.

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Bestimmung von Molybdänspuren in Meereswasser mit Hilfe einer Kombination von Anionenaustausch und elektrothermischer Atomabsorptionsspektrometrie

     

Determination of antimony in solder alloy by hydride generation followed by graphite furnace atomic absorption spectrometry

Summary Antimony was determined in solder alloy (NBS; SRM 1276) by a combination of hydride generation with reducing tube, graphite furnace atomization and atomic absorption detection. Stibines were generated in a horizontal glass tube, in which a pellet of sodium borohydride was placed. 1.2–1.3 1/min of argon flow rate, 2,300° C of atomization temperature and 1.2–2.5 M of acids concentration were the best experimental conditions. The strong supression of the antimony signal by nickel, cobalt and copper was effectively eliminated with 1,10-phenanthroline. A detection limit of 1.2 ng was obtained with a precision of 4–5%. The reducing tube used in this technique is extremely simple and can be connected to all the types of graphite furnaces. Furthermore, this technique can be used for the determination of mercury [1].

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Bestimmung von Antimon in Lotlegierung durch Hydriderzeugung mit nachfolgender Atomisierung im Graphitrohr und AAS-Detektion

Zusammenfassung Antimon wurde nach diesem Verfahren in Lotlegierung NBS (SRM 1276) bestimmt. Die Stibine wurden in einer horizontalen Glasröhre erzeugt, die gekörntes Natriumborhydrid enthielt. Der Argonfluß betrug 1, 2–1,3 l/min, die Atomisierungstemperatur 2300° C und die Konzentration an Säure 1,2–1,5 M. Die starke Unterdrückung des Sb-Signals durch Ni, Co und Cu konnte erfolgreich mit Hilfe von 1,10-Phenanthrolin verhindert werden. Die Nachweisgrenze lag bei 1,2 ng, die Präzision betrug 4–5%. Die benutzte Reduktionsröhre ist sehr einfach und kann an alle Typen von Graphitöfen angeschlossen werden. Das Verfahren läßt sich auch zur Quecksilberbestimmung [1] einsetzen.

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Paper read at the meeting of the Japan Society for Analytical Chemistry, October 1983     

Determination of trace impurities in iron and nickel-base alloys by graphite furnace atomic absorption spectrometry

Five approaches to the determination of trace amounts of lead, bismuth, thallium, selenium, tellurium, and silver in iron and nickel-based alloys were investigated. While all procedures produced satisfactory results, direct techniques yielded a significant times advantage over separation schemes. Matrix effects made calibration curves an impractical approach. A spiking technique was used to generate data on a wide range of standard alloy samples.     

Preconcentration and determination of ultra trace amounts of palladium in water samples by dispersive liquid-liquid microextraction and graphite furnace atomic absorption spectrometry

A highly sensitive, simple and rapid method is presented for the determination of palladium using graphite furnace atomic absorption spectrometry after its separation and preconcentration by dispersive liquid-liquid microextraction. Ultra traces of Pd were extracted and preconcentrated in acidic water samples by using 2-amino-1-cyclohexene-1-dithiocarboxylic acid as a suitable chelating agent, and carbon tetrachloride and acetone as extraction and disperser solvents, respectively. The experimental parameters were optimized in order to enhance the extraction efficiency. After optimizing the extraction conditions and various instrumental parameters, an enhancement factor of 350 was obtained. The analytical curve absorbance vs. concentration was linear over the range 0.02–0.6 µg L^-1 Pd. The detection limit and relative standard deviation were 0.007 µg L^-1 and 4.2%, respectively. The method was successfully applied to the determination of palladium in roadside soil and several aqueous samples.     

Determination of antimony in geochemical samples by graphite furnace atomic absorption spectrometry using different matrix modifiers

Determination of antimony by graphite furnace atomic absorption spectrometry using five different matrix modifiers, viz. nitric acid, copper, nickel, molybdenum and palladium, together with L'vov platform was studied. Without matrix modification, antimony was lost in a 1.2-M HCl solution when the thermal pretreatment temperature exceeded 700°C. By using 1.4 M HNO₃ or $\text{1μg}\text{20μl}$ copper solution the thermal pretreatment temperature could be increased up to 900°C. The matrix modification with $\text{2μg}\text{20μl}$ palladium, $\text{4μg}\text{20μl}$ molybdenum, or $\text{20μg}\text{20μl}$ nickel allowed the use of 1300°C as the pretreatment temperature. The best results were obtained with palladium when its concentration exceeded $\text{0.8μg}\text{20μl}$. Chemical interferences were studied with standard solutions spiked with different metal chlorides. The severe interference caused by iron chloride was avoided with ascorbic acid (2.5 %, $\text{w}\text{v}$). The method was tested on some geochemical reference samples.     

石墨炉原子吸收光谱法测定中药漏芦中微量铅

中药漏芦具有抑制动脉粥样硬化、抗脂质过氧化、减弱血小板聚集和提高免疫力等作用[1]。测定中药中微量元素的含量,对于探讨中药药理、提高药效和降低毒副作用有重要的意义[2,3]。铅是一种毒性元素,它在人体中具有累积性,通过肠胃道吸收,严重损害神经系统、造血系统和消化系统,从而导致肌体免疫力降低。本文选用磷酸氢二铵为基体改进剂,采用石墨炉原子吸收光谱法,对漏芦中Pb的含量进行了测定,考察了影响测定结果的主要因素。样品分析结果表明,本法简便、快速、灵敏、准确。1　实验部分1 1　仪器及工作条件180 80型原子吸收分光光度计、…     

Preconcentration of lead in biological matrices for graphite furnace atomic absorption spectrometry

Lead was transferred by a two-step extraction procedure from complicated biological matrices into an aqueous solution. Thereafter, lead could be accurately determined in the aqueous solution without interference by graphite furnace atomic absorption spectrometry (GFAAS). Biological samples were digested sequentially by a mixture of sulphuric acid and nitric acids and a strong oxidant, potassium peroxodisulphate. Lead was extracted by dithiocarbamate in chloroform from the digest solution and subsequently back-extracted into a mercury(II) solution. Matrix materials such as chloride, phosphate and sulphate, which were known to cause serious interference in the determination of lead by GFAAS, could be eliminated in the preconcentration procedure. Close to 90% recovery of lead was achieved. The proposed procedure was applied for the analysis of several NBS biological standard reference materials containing lead in the mg kg^?1 range and satisfactory results were obtained.     

石墨炉原子吸收光谱法测定茶叶中的铅

采用石墨炉原子吸收光谱法测定茶叶中铅,以NH4H2PO4作为基体改进剂,提高了测定的灰化温度,消除了基体干扰.方法简便,快速,准确度高.通过对标准物质的多次测定,结果均在其保证值范围内,相对标准偏差为2.8%.对样品进行加标回收试验,回收率为96%～105%,方法检出限为0.12μg/L.     

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。     

浊点萃取-石墨炉原子吸收光谱法测定水样中痕量铝

提出了浊点萃取石墨炉原子吸收光谱法测定痕量铝的新方法。探讨了溶液pH、试剂浓度等实验条件对浊点萃取及测定灵敏度的影响。在最佳条件下,富集40 mL样品溶液,用石墨炉原子吸收光谱法测定,铝的检出限为0.045μg/L,铝的富集倍率为78.5倍。方法适用于自来水、河水及海水中痕量铝的测定。     

Determination of trace impurities in aluminum nitride by direct solid sampling graphite furnace atomic absorption spectrometry

The trace impurities Cr, Cu, Fe, K, Mn, Sb and Zn were determined in powdered aluminum nitride by direct solid sampling graphite furnace atomic absorption spectrometry using a ZEEnit 60 atomic absorption spectrometer. This spectrometer features inverse Zeeman-effect background correction and a variable magnetic field enabling measurements in two sensitivity modes over a concentration range of three orders of magnitude. The measurement sensitivity can be adjusted to the analyte concentration in the sample. The use of chemical modifiers was not necessary. Calibration was carried out by means of calibration curves obtained with aqueous standard solutions. Accuracy was checked mainly by comparison of the results with those obtained by instrumental and radiochemical neutron activation analysis whereby, excluding the results for potassium, no significant differences were found by carrying out the t-test at the significance level 0.05. The limits of detection were between 0.05 ng g⁻¹ (Zn) and 80 ng g⁻¹ (Fe) and the relative standard deviations below 11 %. With the proposed method, up to ten measurement cycles can be carried out in one hour.     

Determination of arsenic content in natural water by graphite furnace atomic absorption spectrometry after collection as molybdoarsenate on activated carbon

A sample solution containing less than 0.5 μg of As was adjusted to pH 2. As in the solution was collected on activated carbon (AC) as molybdoarsenate. The AC was directly introduced as an AC suspension into a graphite furnace atomizer, and the concentration of As was determined by atomic absorption spectrometry (AAS). This method is relatively free from interference caused by coexisting ions. The calibration curve was linear up to 0.1 mg l⁻¹, and limit of detection of As was 0.004 mg l⁻¹. When 1000 ml of sample solution is preconcentrated to 5 ml (enrichment factor is 200-fold) 0.02 μg l⁻¹ of As could be determined, and relative standard deviation was below 4.0% (by the deuterium background correction system). The method was applied to sea water and well water, and the sum of As(III) and As(V) was determined with satisfactory results.     

Determination of trace elements in Antarctic krill samples by inductively coupled atomic emission and graphite furnace atomic absorption spectrometry

Analytical methods were developed for the determination of trace elements in Antarctic krill samples applying inductively coupled plasma atomic emission spectrometry (ICP-AES) and graphite furnace atomic absorption spectrometry (GF-AAS). Cu, Fe, Mn and Zn were determined by ICP-AES, while Cd and Pb by GF-AAS technique. Two microwave assisted digestion procedures were elaborated for the preparation of 0.5-g krill samples using open and closed vessel systems. The efficiency of the digestion processes was checked by measurements of the total organic carbon content of the solutions obtained. The deviations of the analytical data from the certified values and the relative standard deviations of the concentration measurements were lower for all six elements investigated applying the closed vessel digestion system.     

石墨炉原子吸收法测定中药百里香中微量镉

百里香(ThymusSerpyllumL.)异名地椒、地花椒、山椒等,属唇形科小灌木植物。我国主要分布在西北、河北、内蒙古和东北等地,可全草入药。主治小儿百日咳、风寒咳嗽、胃痛、泄泻、外伤疼痛、牙疼等疾病[1,2]。本文以NH4H2PO4为化学改进剂,GFAAS法直接测定百里香中微量镉。对化学改进剂及其用量,石墨炉工作条件以及共存离子的影响等进行了研究。优化实验条件下,精密度(RSD)2 2%,检出限0 6pg,试样加入回收率96 5%～106%,测定值与参考值基本符合。1　实验部分1 1　仪器及操作条件180 50型原了吸收光度计(日本日立公司),170 0126型自动…     

Determination of cadmium in orthophosphoric acid by graphite furnace atomic absorption spectrometry

Summary Cadmium has been determined in analytical-reagent grade orthophosphoric acids by direct graphite furnace atomic absorption spectrometry with Zeeman background correction. The detection limit was 3.0 pg cadmium, corresponding to 1.0 g/l of cadmium in the concentrated acid. Most of the acids analyzed contained 2–5 g/l of cadmium. The method was checked using electrochemical preconcentration of cadmium, followed by flame atomic absorption spectrometry.