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 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.     

Determination of trace elements in seawater samples by on-line column extraction/graphite furnace atomic absorption spectrometry

An innovative procedure for the on-line coupling of ion chromatography with graphite furnace atomic absorption spectrometry is described, which is particularly effective for the determination of trace metals in seawater samples. The Capillary Injection Device (CID) is used as an interface which allows the eluent to be transferred from the chromatographic column into the graphite tube at a flow rate of as high as 2 ml/min. The analytical procedure is based on the metal complex formation with 8-hydroxyquinoline in the sample solution, followed by the preconcentration of the complexes in a chromatographic column packed with XAD-2 resin. The complexes were then eluted from the column with methanol, and quantitatively injected into the furnace. The procedure was validated by determining cadmium and lead in certified reference seawater samples at a level of 30–40 pg/g, with a typical reproducibility of 10% and an accuracy of better than 5%. Finally, it was tested on a real sample of seawater. Due to the high reproducibility, a pg/g concentration level can be measured.     

Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of trioctylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 μg l^?1 of tin in the MIBK solution or 0.2–0.3 μg g^?1 in the rock. The concentration range is linear between 2.5 and 500 μg l^?1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 μg l^?1 level and < 7% at the 10–30 μg l^?1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 μg g^?1 or less.     

Determination of trace elements in automotive fuels by filter furnace atomic absorption spectrometry

The determination of Cd, Cr, Cu, Pb and Ni was performed in gasoline and diesel fuel samples by electrothermal atomic absorption spectrometry using the Transverse Heated Filter Atomizer (THFA). Thermal conditions were experimentally defined for the investigated elements. The elements were analyzed without addition of chemical modifiers, using organometallic standards for the calibration. Forty-microliter samples were injected into the THFA. Gasoline samples were analyzed directly, while diesel fuel samples were diluted 1:4 with n-heptane. The following characteristic masses were obtained: 0.8 pg Cd, 6.4 pg Cr, 12 pg Cu, 17 pg Pb and 27 pg Ni. The limits of determination for gasoline samples were 0.13 μg/kg Cd, 0.4 μg/kg Cr, 0.9 μg/kg Cu, 1.5 μg/kg Pb and 2.5 μg/kg Ni. The corresponding limit of determination for diesel fuel samples was approximately four times higher for all elements. The element recovery was performed using the addition of organometallic compounds to gasoline and diesel fuel samples and was between 85 and 105% for all elements investigated.     

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.     

Determination of trace elements in macrozoobenthos samples by total reflection X-ray fluorescence analysis

The paper describes the analysis of a set of metals in macrozoobenthos samples from a river in Western Austria by using total reflection X-ray fluorescence analysis (TXRF). Metal concentrations in aquatic insect larvae from an industrially contaminated site are significantly higher than in larvae from a reference site. Furthermore, species-specific differences in metal accumulation were found. TXRF allows multi-element analysis of very low metal concentrations in very small sample masses (e.g. single aquatic insect larvae with a dry weight of only a few milligrams). Due to its multi-element capability and high sensitivity total reflection X-ray fluorescence analysis is a valuable tool for biomonitoring studies of metal contamination in aquatic ecosystems.     

Determination of trace elements in Syrian medicinal plants and their infusions by energy dispersive X-ray fluorescence and total reflection X-ray fluorescence spectrometry

X-ray fluorescence (XRF) and total-reflection X-ray fluorescence (TXRF) techniques suited well for a multi-element determination of K, Ca, Mn, Fe, Cu, Zn, Rb, and Sr in some Syrian medicinal plant species. The accuracy and the precision of both techniques were verified by analyzing the Standard Reference Materials (SRM) peach-1547 and apple leaves-1515. A good agreement between the measured concentrations of the previously mentioned elements and the certified values were obtained with errors less than 10.7% for TXRF and 15.8% for XRF. The determination of Br was acceptable only by XRF with an error less than 24%. Furthermore, the XRF method showed a very good applicability for the determination of K, Ca, Mn, Fe, Cu, Zn, Rb, Sr, and Br in infusions of different Syrian medicinal plant species, namely anise (Anisum vulgare), licorice root (Glycyrrhiza glabra), and white wormwood (Artemisia herba-alba).     

Determination of trace molybdenum in biological and water samples by graphite furnace atomic absorption spectrometry after separation and preconcentration on immobilized titanium dioxide nanoparticles

A new method has been developed for the determination of trace molybdenum based on separation and preconcentration with TiO₂ nanoparticles immobilized on silica gel (immobilized TiO₂ nanoparticles) prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS). The optimum experimental parameters for preconcentration of molybdenum, such as pH of the sample, sample flow rate and volume, eluent and interfering ions, have been investigated. Molybdenum can be quantitatively retained by immobilized TiO₂ nanoparticles at pH 1.0 and separated from the metal cations in the solution, then eluted completely with 0.5 mol L^?1 NaOH. The detection limit of this method for Mo was 0.6 ng L^?1 with an enrichment factor of 100, and the relative standard deviation (RSD) was 3.4% at the 10 ng mL^?1 Mo level. The method has been applied to the determination of trace amounts of Mo in biological and water samples with satisfactory results.     

Determination of trace elements in sea water by graphite-furnace atomic absorption spectrometry after preconcentration by tetrahydroborate reductive precipitation

A method is described for the preconcentration of 16 elements from coastal and deep ocean sea water based on their reductive precipitation by sodium tetrahydroborate. The enrichment factors obtained were sufficient to permit the analysis of a near-shore sea-water reference material (11 elements) and an open ocean sea-water reference material (9 elements). Recoveries from 900 ml of sea water ranged from 80 to 107% (100-ml sample for Mn) with absolute blanks between <1.0 ng (Se) and 20 ng (Cu). Estimated detection limits varied from 0.3 ng l ^?1 (Pb) to 19 ng l^?1 (As) based on a 36-fold concentration of a 900-ml sample.     

Determination of mercury by atomic absorption spectrometry using a platinum-lined graphite furnace for in situ preconcentration

Mercury in water samples was reduced by tin(II) chloride and the generated vapour swept in a flow of argon through a platinum-lined graphite tube to permit in situ preconcentration. Subsequent atomization of the mercury was then carried out under essentially gas-stop conditions to maximize sensitivy. The system was optimized with respect to argon gas flow and time of mercury generation/deposition using response surface methodology. Synthetic sea-water samples were analysed to test the applicability of the method. For 50-ml sample volumes, detection limits below 2 ng 1^?1 mercury could be obtained, based on twice the standard deviation of the blank. The most favourable aspect of the procedure is its simplicity, since the mercury generator can be easily constructed and connected to commonly available graphite furnace atomic absorption spectrometers.     

Determination of trace metals in seawater by graphite furnace atomic absorption spectrometry with preconcentration on silica-immobilized 8-hydroxyquinoline in a flow-system

Summary A flow-system utilizing a miniature column packed with silica-immobilized 8-hydroxyquinoline (I-8-HOQ) was used for the preconcentration of Cd, Pb, Zn, Cu, Fe, Mn, Ni, and Co from seawater prior to their determination by graphite furnace atomic absorption spectrometry (GFAAS). Enrichment factors sufficient to permit the analysis of an open ocean seawater reference material using 50 ml sample volumes (100 ml for Co determinations) were obtained. Recoveries of the above elements from seawater averaged 93% (range 87–97%) with absolute blanks ranging between 0.04 ng (Ni) and 4.0 ng (Fe). Estimated detection limits for these elements vary from 0.2 ng l^–1 (Co) to 40 ng l^–1 (Fe) based on a 50 ml sample volume (100 ml for Co).

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Bestimmung von Spurenmetallen in Meereswasser durch Graphitofen-AAS mit Anreicherung an Kieselgel-immobilisiertem 8-Hydroxychinolin in einem Durchflu\system

     

Determination of trace amounts of cadmium by modified graphite furnace atomic absorption spectrometry after liquid phase microextraction

A simple and powerful microextraction technique was used for determination of cadmium in water samples using liquid phase microextraction (LPME) followed by graphite furnace atomic absorption spectrometry (GF-AAS). In a preconcentration step, cadmium was extracted from a 2 mL of its aqueous sample in the pH = 6 as cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) cationic complex into a 4 µL drop of nitrobenzene and ammonium tetraphenylborate as counter ion. In the drop, the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) ammonium tetraphenylborate ion associated complex was formed. After extraction, the microdrop was retracted and directly transferred into a graphite tube modified by [Pd_(c) + Pd_(i)]. Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent and counter ion, extraction time and stirring rate were optimized. Under the optimum conditions, the enrichment factor and recovery were 390 and 78%, respectively. The calibration graph was linear in the range of 0.01–1 µg L^− 1 with correlation coefficient of 0.9952 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0065 µg L^− 1 and relative standard deviation (RSD) for eight replicate measurements of 0.1 µg L^− 1 and 0.4 µg L^− 1 cadmium was 6.4 and 5.8% respectively. The characteristic concentration was 0.0014 µg L^− 1 equivalent to a characteristic mass of 5.6 fg. In order to evaluate the accuracy and recovery of the presented method the procedure was applied to the analysis of reference materials and seawater.     

Differential determination of arsenic(III) and total arsenic using flow injection on-line separation and preconcentration for graphite furnace atomic absorption spectrometry

Arsenic(III) can be quantitatively extracted using sodium diethyldithiocarbamate (NaDDTC) as the complexing agent and C18 reversed phase packing as the column material for solid phase extraction. Arsenic(V) must be reduced to its trivalent oxidation state prior to extraction. A mixture of sodium sulphite, hydrochloric acid, sodium thiosulphate and potassium iodide was found to be optimum for on-line reduction. When the sorbent extraction is carried out without and with the addition of the reduction mixture, arsenic(III) and total arsenic can be determined sequentially by graphite furnace atomic absorption spectrometry with detection limits (3 σ) of 0.32 ng for As(III) and 0.43 ng for total arsenic. A 7.6-fold enhancement in peak area compared to direct injection of 40 μl samples was obtained after 60 s preconcentration. Results obtained for sea water standard reference materials, using aqueous standards for calibration, agree well with certified values. A precision of 5.5% RSD was obtained for total arsenic in a sea water sample (1.65 As). Results obtained for synthetic mixtures of trivalent and pentavalent arsenic agreed well with expected values.     

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、…     

Determination of trace elements in bee honey,pollen and tissue by total reflection and radioisotope X-ray fluorescence spectrometry

Multielemental determinations in samples of various types of bee honey, pollen and bee tissue have been carried out using total reflection X-ray fluorescence spectrometry (TXRF) and radioisotope excited X-ray fluorescence spectrometry (XRF). The objective was to establish whether the elemental content of bee honey, in particular, correlates with any useful information about the environment, variety of honey, etc. An attempt has also been made to determine the X-ray techniques' ability to compete with atomic absorption spectrometry (AAS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES), with regard to elemental sensitivity, accuracy, sample preparation procedures, and in particular, economic performance, which is very important in selecting an appropriate technique for the analysis of large numbers of samples. The results confirm the advantages of the TXRF method for trace element analysis, but only when utilising monochromatic excitation and selecting a proper sample preparation procedure. The radioisotope XRF technique, which does not require any sample preparation, is still very competitive in analysis of elements with concentrations above a few ten ppm. Preliminary results also confirm some correlations between the elemental content of honey and the status of the environment, and encourage further work in this direction     

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。     

Determination of fluorine by total reflection X-ray fluorescence spectrometry

There is a growing interest in determination of low Z elements, i.e. carbon to phosphorus, in various samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as a suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon).