石墨炉原子吸收直接测定原油中痕量钒镍

石墨炉原子吸收光谱 ( GFAAS)直接进样技术在石墨炉原子吸收光谱仪问世不久就已开始出现[1 ] ,并随着石墨炉技术的发展而不断改进和完善。目前测定原油中痕量金属元素一般都需要对原油进行预处理后再测定。常用的干灰化[2 ] 等预处理方法 ,操作繁琐且费时。石墨炉原子吸收光谱直接进样技术充分利用了石墨炉本身对样品基体具有灰化处理能力这一特点 ,原油可不经预处理 ,直接进样分析 ,这样就大大简化了操作步骤 ,缩短了分析时间。虽然直接测定原油中痕量金属元素有许多优点 ,但是在实际应用中尚有一定难度 ,这除了因其操作难度大、校正困难…     

石墨炉原子吸收分光光度法测定大气颗粒物中的镍

用有机滤膜或有机滤筒采集大气颗粒物样品,以硝酸、高氯酸消解处理,用石墨炉原于吸收分光光度法测定大气颗粒物中的镍含量。方法的线性范围为0～0.50μg/L,线性回归方程为A=0.892c+0.0148,相关系数r=0.9994,相对标准偏差为3.9％～7.8％,回收率为90％～94％,检出限为7.00×10~(-3)μg/L。该方法的各项指标均符合环境监测的质控要求,适用于大气和固定污染源排气颗粒物中镍的测定。     

平台石墨炉原子吸收法直接测定高温镍基合金中硒

研究了基体改进剂及其用量,硒的灰化、原子化和出现温度,以及近20种共存离子的干扰。采用镍和钯混合液作基体改进剂,硒的灵敏度高,抗干扰能力强,不需要分离样品基体,可以采用平台石墨炉法直接测定高温镍基合金中硒。     

石墨炉原子吸收法测定食品中镍的研究

建立了测定食品中镍的石墨炉原子吸收法，方法的最低检出限为１．６０μｇ／Ｌ，标准参考物牡蛎镍的测定值怀保证值偏差小于５％，回收率在８６．０％￣１０３．０％之间，并对我国八大类食品中镍含量本底值作了调查。     

悬浮液进样石墨炉原子吸收测定钒钛磁铁矿中痕量镍

样品粒度不超过３８μｍ，以２０％乙醇－１％硝酸水溶液为介质，用与样品基体类似的一种标准矿样进行校正，可消除基体效应。样品浓度不超过７３ｍｇ／１０ｍｌ，含镍０－３５０ｎｇ．ｍｌ＾－１范围内呈良好线性关系。     

平台石墨炉原子吸收法测定高温镍基合金中砷

研究了基体改进剂，灰化，原子化温度和共存元素的干扰。采用钯作基体改进剂和匹配基体镍后，提高了灵敏度，增强了抗干扰能力。在波长１９７．２ｎｍ处，用平台石墨炉原子吸收法直接测定了高温镍基合金中砷。方法特征是为８８ｐｇ，检出限为０．２７μｇ．ｇ＾－１，相对标准偏差为３．１％－５．１％，回嵋率为８５％－１００％。     

石墨炉原子吸收法间接测定血清中的碘

１引言碘是人体中必需的微量元素，是甲状腺素的重要组分部分。缺碘易引发甲状腺肿大及克汀病等病症。碘的测定方法大都采用催化比色法和碘量法。其测定原理均是利用Ｉ－的还原性质，但这些方法大都具有操作复杂、反应条件要求苛刻、费时和不易掌握的缺点。本文利用Ｉ－与Ａｇ＋反应生成ＡｇＩ沉淀，测定样品中Ａｇ－浓度的减少值，间接求出Ｉ－浓度。干扰离子可借助其化学性质的差异和溶度积的不同加以消除。本法具有简单、快速、结果准确的特点。是测定Ｉ－的又一新方法。２实验部分２．１仪器与试剂岛津ＡＡ－６７０原子吸收分光光度计，…     

石墨炉原子吸收法连续测定气溶胶中重金属

提出了用石墨炉原子吸收法连续测定气溶胶中六种重金属的方法.气溶胶样品经处理后,直接用石墨炉原子吸收法测定其中的铜、钴、镍、镐、铅和铬.其检出限在 1.9×10~(-12)～1.6×10~(-10)g,仪器的精密度(RSD)<6.1%,标准加入回收率为90.4%～106.5%,已用于大批气溶胶样品的测定,结果令人满意.     

石墨炉原子吸收法直接测定水中硒

硒是人体必需的营养元素,可抑制癌肿瘤和心血管疾病的发生。体内硒含量过低能引起营养不良,导致心肌病变;过高则引起硒中毒。 硒作为重要的生物微量元素近十几年开始被研究。硒不仅被看成是生物体内所必要的微量元素之一,而且是目前已知微量元素中较重要的一种。近年来已证明硒是机体氧化还原系统中谷胱甘肽过氧化酶的活性元素。     

石墨炉原子吸收光谱法测定食盐中钡

建立了石墨炉原子吸收光谱法测定食盐中钡的方法,不需要对石墨管做任何处理,也无需对样品进行除盐处理,通过优化石墨炉升温程序,极大改善了食盐样品中钡测定的灵敏度和峰型。钡在0.00~50.0 μg/L浓度范围呈现良好的线性关系,相关系数优于0.999,检出限为0.650 mg/kg(以称样量0.200 g,定容至50 mL计算)。食盐样品钡加标回收率范围为81.3%~105.1%,相对标准偏差在8.9%以内。方法稳定可靠,准确度较高,适用于食盐中钡的测定。     

Effectiveness of linearization of calibration curves in Zeeman graphite furnace atomic absorption spectrometry

A theoretical analysis is made of the effect of analytical line broadening and of non-absorbable radiation in the light source on the shape of concentration curves in Zeeman graphite furnace atomic absorption spectrometry. These results have been used in a systematic study of the effect of spectrometer slit width and hollow-cathode lamp (HCL) current on linearization of calibration graphs for 11 elements: Ag, Au, Bi, Cd, Co, Cu, Fe, Mn, Ni, Pb, and Sb. The effectiveness of linearization throughout the analytical range covered was estimated experimentally on series of 25–30 solutions. Three solutions in each series were used as standards for constructing the calibration graph, the others serving to evaluate the linearization effectiveness. Increasing the slit width and decreasing the HCL current compared to the standard measurement conditions have permitted us to reach a sufficiently high effectiveness of linearization for all the elements studied, with the exception of Ni. The maximum deviation of experimental points from the linear graph under optimum conditions does not exceed 6%. The effect of the Δ parameter used in the computational algorithm on linearization effectiveness is investigated.     

石墨炉原子吸收光谱法测定锌基体物料中微量铊

采用B-HNO3-A溶解样品,硝酸钯作基体改进剂,通过优化仪器分析条件,灰化温度为500℃,原子化温度为1 800℃,成功实现了石墨炉原子吸收光谱法测定湿法冶炼锌基体物料锌精矿、锌焙砂、氧化锌、锌粉等物料中微量铊。方法对照实验结果与电感耦合等离子体质谱法(ICP-MS)测定值基本一致。方法的相对标准偏差(RSD,n≤8)为1.7%~7.8%,加标回收率为99%~103%。     

Determination of organotin compounds in marine sediments using graphite furnace atomic absorption spectrometry

Organotin compounds, especially tributyltin, began to cause concern 10 years ago due to a high toxicity towards marine organisms. Several methods of analysing organotin compounds in various matrices have already been developed to determine organotin species simultaneously, but these are quite expensive as special equipment and specialized staff are needed. A simple screening method, which determines the organic tin compounds in the sediment, has therefore been developed and validated. The method can easily be implemented in laboratories accustomed to tracelement analyses; the sediment is extracted by a two-phase extraction and the organic extract is analysed using graphite furnace atomic absorption spectrometry (GF AA.) The screening method has been validated using high-pressure liquid chromatography-inductively coupled plasma mass spectrometry (HPLC–ICP MS).     

Determination of osmium in waste water by graphite furnance atomic absorption spectrometry

The determination of osmium in waste water by electrothermal atomic absorption spectrometry (AAS) with a graphite furnace atomiser has been investigated. The atomisation characteristics of osmium on the atomiser were found to result in optimal ashing and atomisation temperatures of 300–500 and 3180 °C, respectively.The characteristic mass (the mass of element giving 0.0044 abs.) of osmium after optimization was found to be 1.6ng, which is better than obtained with flame AAS and ultraviolet/visible (UV) absorption spectrophotometry. The detection limit (s/n = 3) was 3.6ng (or 0.36 (g ml^–1). The relative std. deviation obtained with graphite furnace AAS was 3.0%.The interference caused by large amounts of common cations and anions in waste water were evaluated and thiourea as matrix modifier was shown to be able to eliminate many interferences. The recovery of osmium spiked in waste water was considered almost satisfactory at the 1–50 g ml^–1 range and the results were shown to well agree with the analytical values obtained by UV absorption spectrophotometry.     

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.     

石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙

以甘露醇为基体改进剂,建立石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙含量的方法。考察基体改进剂用量、灰化温度、原子化温度、基体干扰以及共存离子干扰对测定结果的影响,确定最佳测定条件:以硼含量为1000 mg/kg的硼酸为背景基体,加入适量甘露醇,样品作酸化处理,灰化温度为1700℃,原子化温度为2450℃。钙含量在8~32 μg/kg范围内与光谱强度成良好的线性关系,相关系数为0.9996,方法检出限为1.79 μg/kg。对于硼基体含量为0~2500 mg/kg的样品,测定结果的相对标准偏差为0.5%~7.5%(n=6),相对误差不大于13.2%,加标回收率为93.9%~113.3%。该方法检测速度快,结果准确,能满足实际生产要求。     

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％。     

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、…     

石墨炉原子吸收法测定3-苯基丙烯酸酯类化合物中微量钯

利用高灵敏的石墨炉原子吸收法,在V(HCl):V(HNO3):V(H2O)＝5:1:94混合酸介质中测定苯基丙烯酸酯类化合物中的钯量.已纯化样品钯量的平均值是6.76 μg/g,标准相对偏差是4.8%,平均回收率为99.3%;未纯化样品钯量的平均值是121.2 μg/g,平均相对偏差是5.4%.还讨论酸介质对测定钯吸光度的影响,通过比较找到了合适的酸介质组成.