石墨炉原子吸收光谱法测定硒的研究进展

综述了石墨炉原子吸收光谱法测定硒的方法的进展,主次涉及基体改进剂的种类、用量、最佳灰化温度、原子化温度及测定过程中的基体干扰因素等(应用文献34篇)。     

石墨炉原子吸收光谱法测定虾酱中铅

通过硝酸铵作为虾酱的基体改进剂,建立了石墨炉原子吸收光谱法测定虾酱中铅的方法。方法具有试剂用量少,操作方便等优点,在最佳测试条件下,测得铅的检出限为6mg·kg-1。应用于虾酱中铅的测定,回收率为90.2%～101.8%,结果满意。     

石墨炉原子吸收光谱法直接测定血样中硒

用石墨炉原子吸收光谱法，以硝酸铜和硝酸铵为基体改进剂，塞曼效应扣背景，采用标准加入法可直接测定血样中硒，回收率为95％～105％，相对标准偏差为5．8％，检出限为96pg，测定结果准确可靠。     

石墨炉原子吸收光谱法测定灵芝饮料中痕量锗

研究了用石墨炉原子吸收光谱法测定灵芝饮料中痕量锗,提出了以NaOH、H_2O_2为消解液分解样品,采用NaOH+Ni(NO_3)_2混合基体改进剂在热解涂层石墨管中直接测定灵芝饮料中痕量锗的方法。该法简单、快速、灵敏度高、重现性好。     

石墨炉原子吸收光谱法测定废水中痕量镉

用石墨炉原子吸收光谱法测定环境废水中痕量镉时,锰、铬、镍、铜、钴、锌等共存元素干扰严重。以100 mg·L-1铁作为基体改进剂可消除干扰,加标回收率为94％～105％,RSD为5．92％～7．42％。     

石墨炉原子吸收法直接测定血清中硒,砷

选用Ｐｄ－Ｎｉ－Ｔｒｉｔｏｎ Ｘ－１００为基体改进剂，用石墨炉原子吸收法直接血清中砷、硒。该法具有操作简单、快速、灵敏度高的特点，为临床测定血清中砷、硒提供了一种新方法。     

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.     

Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry

A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH₄OH+0.05% w/v Triton X-100^®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO₃)₂ as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1⁻¹ Se, corresponding to 30 μg l⁻¹ Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l⁻¹, with a mean value of 114±22 μg l⁻¹.     

石墨炉原子吸收法测定钢中铅的干扰抑制

研究了石墨炉原子化法测定钢铁中痕量铅的干扰情况，并进行了干扰抑制实验。提出了抑制干扰的方法。     

石墨炉原子吸收光谱分析中的铋原子化机理研究

石墨炉原子吸收光谱法已广泛地应用于合金[1]、矿石[2]和水[3,4]等样品中铋的测定.铋是易挥发元素,为寻找有效的化学改进剂,了解其原子化机理是很有必要的.关于机理研究已有文献报道[5,6],但加入化学改进剂后在石墨管中形成的生成物的结构及其原子化机理的研究还少见报道[7].本试验以硝酸镍、氯化钯、氯化钯-硝酸镁和氯化钯-硝酸镍为化学改进剂,通过实验确定在本实验仪器条件下测定铋的最佳化学改进剂为氯化钯.进而研究铋在化学改进剂作用下的原子化机理,以达到提高原子化效率的目的.     

Evaluation of selenium behavior in thermospray flame furnace atomic absorption spectrometry

The behavior of selenium in thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was studied and the developed procedure was applied for selenium determination in biological materials after microwave-assisted sample digestion. A sample volume of 600 μL was introduced into the hot metallic Ni tube at a flow rate of 0.4 mL min⁻¹ using water as carrier. The limit of detection obtained for Se was 8.7 μg L⁻¹ (3s_blank/slope, n = 10), which is 95-fold better than that typically obtained using FAAS. The applicability of the TS-FF-AAS procedure was evaluated for selenium determination in biological materials. Certified reference materials of pig kidney (BCR 186) and mussel (GBW 08571) were analyzed and a t-test had not shown any statistically significant difference at a 95% confidence level between determined and certified values for both materials. The procedure was successfully applied for determination of Se in pig kidney and shellfish. It was demonstrated that TS-FF-AAS improved the performance of FAAS (flame atomic absorption spectrometry) for determination of Se.     

Surfactant/oil/water system for the determination of selenium in eggs by graphite furnace atomic absorption spectrometry

An oil-in-water formulation has been optimized to determine trace levels of selenium in whole hen eggs by graphite furnace atomic absorption spectrometry. This method is simpler and requires fewer reagents when compared with other sample pre-treatment procedures. Graphite furnace atomic absorption spectrometric (GF AAS) measurement was carried out using standard addition calibration and Pd as a modifier. The precision, expressed as relative standard deviation, was better than 5% and the limit of detection was 1 µg L^− 1. The validation of the method was performed against a standard reference material Whole Egg Powder (RM 8415), and the measured Se corresponded to 95.2% of the certified value. The method was used for the determination of the Se level in eggs from hens treated with Se dietary supplements. Inorganic and organic Se sources were added to hen feed. The Se content of eggs was higher when hens were fed with organic Se compared to the other treatments. The proposed method, including sample emulsification for subsequent Se determination by GF AAS has proved to be sensitive, reproducible, simple and economical.     

Preconcentration of palladium in a flow-through electrochemical cell for determination by graphite furnace atomic absorption spectrometry

An electrochemical preconcentration at a controlled potential on the electrode in a flow-through mode followed by graphite furnace atomic absorption spectrometric (GFAAS) detection is proposed for determination of trace amounts of palladium. After electrolysis the polarization of the electrodes was changed and deposited metal was dissolved electrochemically in the presence of an appropriate stripping reagent. Conditions for the electrodeposition, such as pH of the solutions, a deposition potential, dissolution potential and a composition of stripping solution were optimised. The graphite electrode (GE) and glassy carbon electrode (GCE) were tested for the palladium reduction process. The detection limit of 0.05 ng ml⁻¹ Pd (1 pg) was obtained after palladium preconcentration on the GCE and dissolution with 0.2 mol l⁻¹ thiourea in 0.1 mol l⁻¹ HCl followed by GFAAS detection. The method was applied for the determination of palladium in spiked tap water and road dust samples.     

Ammonium fluoride as a novel chemical modifier for the elimination of magnesium chloride interference on the determination of lead by graphite furnace atomic absorption spectrometry

Ammonium fluoride was found to be very efficient modifier for the elimination of MgCl₂ interference on Pb determination. Ammonium fluoride probably converts strongly interfering volatile MgCl₂ to less volatile MgF₂ matrix that makes possible the release of Pb analyte at lower temperature, before the matrix starts to vaporize. It was observed likewise that NH₄F removes the interferences mentioned, i.e. caused by MgCl₂ presence, much more effectively as compared with some modifiers, before now recommended for this purpose. The application of this modifier to the determination of Pb in 2% (m/v) MgCl₂ has ensured the characteristic mass and LOD value in the original sample of 12 pg and 60 ng g⁻¹, respectively (10 μl aliquots of sample). Applying the modifier to standards and samples enables the use of matrix-free standard solutions for attaining accurate analysis as verified by recovery studies.     

样品基体化学改进剂-石墨炉原子吸收光谱法测定镍合金中痕量铋

镍基合金是航空工业的重要金属材料,合金中铋、铅、锡等易挥发元素的含量对合金材料性能影响很大[1,2].原子光谱法常被用于分析镍基合金中的痕量元素,如火焰原子吸收光谱法(FAAS)、氢化物发生-原子吸收(荧光)光谱法(HG-AAS/AFS) [3]、电感耦合等离子体-质谱法(ICP-MS).     

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…