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测定全血中铅的方法改进

针对不同的石墨管测定全血中铅时，用铅标准溶液制作的标准曲线和以全血为基体制作的标准工作曲线斜率的不一致，提出以磷酸氢二铵、磷酸氢二钠和硝酸铵作基体改进剂，以全血为基体制作标准工作曲线来测定全血中铅含量的方法。试验表明，此法基本消除了全血基体对血铅测定的影响，适应各种石墨管，可快速、准确地测定全血中铅。     

石墨炉原子吸收光谱法测定含盐食品中铅

含盐食品样品经硝酸和过氧化氢加热消解,采用石墨炉原子吸收光谱法测定其中铅的含量。以氯化钯-硝酸铵为混合基体改进剂,灰化温度为1 200℃,原子化温度为1 850℃。铅(Ⅱ)的质量浓度在25μg·L-1以内与其吸光度呈线性关系,检出限(3s/b)为26pg。应用此法分析了酱油样品,加标平均回收率为96.2%,相对标准偏差(n=5)为3.0%。     

石墨炉原子吸收光谱法测定尿中铅

提出了用石墨炉原子吸收光谱法测定尿中铅的方法.采用酒石酸和磷酸二氢铵的混合溶液作为基体改进剂,尿样加入酒石酸溶液后,原子化温度从1500℃降至1200℃,基体干扰明显减少;加入磷酸二氢铵溶液,吸光度明显增加.方法的检出限(3S/N)为30 Pg,回收率为99.1%～102.6%,相对标准偏差(n=6)小于6%.     

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)。     

微波消解-石墨炉原子吸收光谱法测定茶叶中的铅

<正>铅是一种严重影响人体健康的重金属元素,茶叶在生长及加工过程中不可避免的受到铅污染,因此,研究茶叶中铅的测定方法具有重要意义[1]。茶叶中铅的测定方法主要有:电化学法[2,3],分光光度法[4],原子光谱法[5-7]和质谱     

塞曼石墨炉原子吸收光谱法测定茶叶中镉

建立了石墨炉原子吸收光谱法测定茶叶中镉含量的分析方法。以1%磷酸二氢铵 1%硝酸镁的混合液为基体改进剂测定了茶叶中的镉,方法的回收率96.0%~103.0%,检出限为0.076ng/mL,测定结果令人满意。     

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％。     

石墨炉原子吸收光谱法测定氯化镁中铅

用石墨炉原子吸收光谱法测定了氯化镁中铅含量.试样经硝酸多次反复溶解转换成以硝酸镁为基体的试液,利用硝酸镁为基体改进剂,灰化温度可以提高到900℃.许多氯化物的干扰可以消除.方法的线性范围为0～80μg·L-1,检出限0.75 mg·kg-1,回收率(平均值)为89.5%,相对标准偏差为11.5%.     

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.     

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.     

Comparison of direct sampling and emulsion analysis using a filter furnace for the determination of lead in crude oil by graphite furnace atomic absorption spectrometry

The determination of trace elements in crude oil is difficult due to the complex nature of the sample and the various different chemical forms in which the metals can occur. The advantage of graphite furnace atomic absorption spectrometry is that only a minimum of sample pretreatment is required. In this work two techniques have been compared to establish a fast and reliable method for lead determination in crude oil. In the first one the crude oil samples were weighed directly onto solid sampling (SS) platforms and introduced into the graphite tube for analysis. In the second one the samples were prepared as oil-in-water emulsions and analyzed in a filter furnace (FF). Twenty μL of a mixture of 0.5 mg L^− 1 Pd + 0.3 mg L^− 1 Mg + Triton X-100 has been used as the modifier, and calibration against aqueous solutions has been used for both methods. The sensitivity obtained with the FF was more than a factor of two better than that with SS; however, as a larger sample mass could be introduced in the latter case, so that the limits of detection for both techniques were 0.004 mg kg^− 1. Seven crude oil samples were analyzed using the two procedures, and all results were in agreement at a 95% confidence level using a paired Student's t-test. For validation purposes, three crude oil samples have been mineralized using an open-vessel acid digestion, and the results were in agreement with those found with direct sampling and with emulsion sampling using FF according to ANOVA test. Both methods are simple, fast and reliable, being appropriated for routine analysis; however, the direct method using SS technology should be preferred because of its simplicity, speed and commercial availability.     

Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry

This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 g) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 °C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 °C. Structured background absorption also occurred after the analyte signal when atomization temperatures of >1600 °C were used, which arose from the electron-excitation spectrum (with rotational fine structure) of a diatomic molecule. Under optimized conditions (pyrolysis at 700 °C and atomization at 1500 °C), interference-free determination of cadmium in seven certified coal reference materials and two real samples was achieved by direct solid sampling and calibrating against aqueous standards, resulting in good agreement with the certified values (where available) at the 95% confidence level. A characteristic mass of 0.4 pg and a detection limit of 2 ng g^–1, calculated for a sample mass of 1.0 mg coal, was obtained. A precision (expressed as the relative standard deviation, RSD) of <10% was typically obtained when coal samples in the mass range 0.6–1.2 mg were analyzed.Dedicated to the memory of Wilhelm Fresenius     

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%。     

石墨炉原子吸收法测定肼类推进剂中九种金属杂质

建立了石墨炉原子吸收法测定肼类推进剂中锌、铁、铬、锰、铅、镍、铝、铜、钛等金属含量的检测方法 ,无需样品预处理过程 ,灵敏度高且快速、准确。各元素测定方法的精密度小于 1 0 % ,回收率在 82 %～ 1 1 6%之间。     

Cloud point extraction for the determination of lead and cadmium in urine by graphite furnace atomic absorption spectrometry with multivariate optimization using Box–Behnken design

Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Pb and Cd in undigested urine by graphite furnace atomic absorption spectrometry (GF AAS). Aliquots of 0.5 mL urine were acidified with HCl and the chelating agent ammonium O,O-diethyl dithiophosphate (DDTP) was added along with the non-ionic surfactant Triton X-114 at the optimized concentrations. Phase separation was achieved by heating the mixture to 50 °C for 15 min. The surfactant-rich phase was analyzed by GF AAS, employing the optimized pyrolysis temperatures of 900 °C for Pb and 800 °C for Cd, using a graphite tube with a platform treated with 500 μg Ru as permanent modifier. The reagent concentrations for CPE (HCl, DDTP and Triton X-114) were optimized using a Box–Behnken design. The response surfaces and the optimum values were very similar for aqueous solutions and for the urine samples, demonstrating that aqueous standards submitted to CPE could be used for calibration. Detection limits of 40 and 2 ng L^− 1 for Pb and Cd, respectively, were obtained along with an enhancement factor of 16 for both analytes. Three control urine samples were analyzed using this approach, and good agreement was obtained at a 95% statistical confidence level between the certified and determined values. Five real samples have also been analyzed before and after spiking with Pb and Cd, resulting in recoveries ranging from 97 to 118%.     

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。