微波消解-石墨炉原子吸收法测定纸巾纸中砷含量

建立了石墨炉原子吸收光谱法测定纸巾纸中砷含量的方法。采用微波消解技术处理样品,加入基体改进剂硝酸镍,应用石墨炉原子吸收光谱法测定砷。结果表明,测定一次回归方程为Y=0.0025X+0.0004,相关系数r=0.9996。检出限为0.12 ug/L,回收率为95.8%～100.3%,相对标准偏差为2.37%。该方法具有快速、准确、灵敏度高等优点,适用于纸巾纸中砷含量的检测。     

石墨炉原子吸收光谱法测定大米中镉含量研究

目的:通过采用石墨炉原子吸收光谱法来对大米中镉的含量进行测量。方法:首先对所要进行试验的大米做实验前的处理,对大米采用湿法消解法进行处理,采用石墨原子吸收光谱法来测定大米中镉的含量,从而对大米中镉含量的最佳测定时间、重复性、回收率和精密度进行检测。结果:选用实验大米质量1g,采用消解剂为硝酸,实验时间13h,在该实验条件进行处理,然后对进行酸化处理的大米采用石墨炉原子吸收光谱法对镉含量进行测定。石墨炉原子吸收光谱法测定大米中镉含量的加标回收率为98.78%。结论:通过石墨炉原子吸收光谱法对大米中镉含量进行测量,具有测量准确、重复性好、误差小的特点,可以用于大米中镉含量的测定。     

石墨炉原子吸收光谱法测定蔬菜中铅和镉

目的:分析探讨蔬菜中铅、镉测定的最佳工作条件。方法:对西兰花与蒜苔蔬菜样品采用硝酸-高氯酸-硫酸消解,利用石墨炉原子吸收光谱法对蔬菜中的铅与镉进行测定。结果:在最佳条件下利用石墨炉原子吸收光谱法测定蔬菜中铅和镉,测得加标回收率铅98.90%,镉102.6%。结论:在对蔬菜中的铅和镉含量进行检测中,采用石墨炉原子吸收光谱法具有快捷、准确的优势,可得到满意的测定结果,满足分析要求。     

甲苯萃取-GFAAS法测定高盐食品中微量砷

建立甲苯萃取-石墨炉原子吸收测定高盐食品中砷的方法。用微波消解样品,甲苯萃取分离砷,硝酸镍作基体改进剂,钯涂层石墨炉原子吸收法测定高盐食品中微量砷。结果表明:用甲苯萃取砷提高了回收率,很好地消除基体干扰;用硝酸镍作基体改进剂,提高砷的灰化温度和灵敏度,方法的相对标准偏差≤1.12%(n=6);回收率达到97.5%~104.5%;检出限为0.038 mg/kg。该法灵敏、准确、可靠,可用于高盐食品中微量砷的测定。     

石墨炉原子吸收光谱法测定金银花中铅镉的研究

采用石墨炉原子吸收法(GFAAS)检测中药材金银花中微量重金属铅、镉的含量.考察了基体改进剂、灰化/原子化温度和常见共存离子等因素对测定的影响,建立以NH4H2PO4为基体改进剂石墨炉原子吸收光谱法测定金银花中微量铅、镉的方法.条件优化后的方法简便快速,重现性好,灵敏度、准确度高,铅的检出限为0.268 μg/L,镉的检出限为0.013 μg/L,回收率85%～110%.     

石墨炉原子吸收光谱法测定面制食品中的铝

目的:介绍并建立起面制食品中铝的石墨炉原子吸收光谱法。方法:将面制食品试验样品于85℃进行烘烤(4小时),然后经520℃进行灰化(6小时),采用0.5%HN03溶解并定容,采用石墨炉原子吸收光谱法测定铝。结果:测定线性范围为1.0~50μg/L,相对偏差在1.1%~4.3%,回收率为93.6%~98.2%。结论:在面制食品中铝的测定采用石墨炉原子吸收光谱法方便、快捷、准确,结果满意。     

石墨炉原子吸收光谱法直接测定纺织品萃取汗液中砷

本文采用石墨炉原子吸收光谱法直接测定纺织品萃取液中砷。通过在样品萃取液中加入基体改进剂,并对石墨炉原子化工作条件和基体改进剂用量进行优化。结果表明,加入4μL 50g/L硝酸镍基体改进剂,可以有效降低高浓度氯化钠基体的影响,样品检出限可达到0.05mg/kg,相对标准偏差为为1.65~3.44%,实际纺织品样品加标回收率为93.8%~103%。该方法具有快速、准确、灵敏度高等优点,适用于测定纺织品萃取汗液中砷含量的检测。     

石墨炉原子吸收光谱法测定六堡茶中的铅和镉

本文用石墨炉原子吸收光谱法测定六堡茶中的铅和镉含量,优化了样品前处理条件和光谱仪的各项技术参数。结果表明:应用微波消解-石墨炉原子吸收法测定六堡茶样品中的铅和镉时,铅的加标回收率在93.1%~99.2%之间,镉的加标回收率在92.3~97.3%之间,相对标准偏差均小于5%。方法准确、方便,可满足检测六堡茶中的铅和镉要求。     

微波消解-石墨炉原子吸收光谱法测定纳米二氧化钛中痕量砷

建立微波消解-石墨炉原子吸收光谱法(GF-AAS)测定纳米二氧化钛中痕量杂质砷的分析方法,以快速完全消解二氧化钛基体并且准确测定痕量杂质砷。方法采用氢氟酸、硝酸混合试剂结合高压密闭微波加热技术,解决二氧化钛难消解和低酸度溶液中高钛基体容易水解等难点。通过基体效应影响试验,优选采用热解涂层石墨管,优化石墨炉升温原子化控制程序以及原子吸收光谱仪工作条件等检测参数,消除热稳定性强的二氧化钛基体对测定易挥发痕量元素砷的影响。结果表明:方法检出限为0.02μg/L,回收率为93.0%~106.0%,相对标准偏差9.36%,与ICP-MS检测方法结果对照一致。     

火焰原子吸收光谱法测定肥料中重金属含量的不确定度评估

根据GB/T 23349—2009 《肥料中砷、镉、铅、铬、汞生态指标》中所规定的方法,采用火焰原子吸收光谱法测定肥料中重金属镉、铬和铅的含量,并建立了火焰原子吸收光谱法测定肥料中重金属含量的不确定度测量模型。测定肥料中重金属镉的含量为0. 003 6%(1±4. 2%),k=2;铬的含量为0. 006 3%(1±3. 8%),k=2;铅的含量为0. 005 0%(1±2. 1%),k=2。结果表明,对镉、铬和铅元素的测试而言,不确定度主要影响因素均来源于样品浓度测定中标准曲线的拟合及测量重复性引入的不确定度分量。     

Determination of gadolinium in biological materials using graphite furnace atomic absorption spectrometry with a tantalum boat after solvent extraction

A method was developed for the determination of gadolinium (Gd) in biological material using graphite furnace atomic absorption spectrometry (GFAAS). The element is first extracted into methyl isobutyl ketone and then reextracted into hydrochloric acid. Factors influencing the recovery of extraction such as pH, choice of chelating agents, and hydrochloric acid concentration have been investigated. The element is determined under STPF (stabilized temperature platform furnace) conditions with atomization from a tantalum boat. Under optimized furnace conditions, the use of the tantalum boat improved sensitivity substantially compared to the use of pyrolytically coated graphite tubes. Around 150 measurements could be performed with 1 boat. Memory effects, being a common problem in the GFAAS determination of lanthanoids, were no longer observed after insertion of the boat. The characteristic mass and detection limit (2SD; SD = standard deviation) of the Gd determination are 1000 and 2060 pg, respectively. The precision evaluated as the relative standard deviation (RSD) of six analyses was below 10% for tissue Gd concentrations ranging from 0.92 to 72.0 micrograms g-1. The recovery of added analyte ranged between 92.0% and 99.3%. The method was found to be suitable for studying the pharmacokinetics and biodistribution of Gd in rats.     

Separation and preconcentration of cadmium ions using octadecyl silica membrane disks modified by methyltrioctylammonium chloride

A simple and selective method for the determination of cadmium in water samples by FAAS after solid phase extraction has been developed. The method is based on the sorption of cadmium as CdI(4)(2-) on octadecyl silica membrane disks modified by cationic surfactant of methyltrioctylammonium chloride in the pH range of 1-8. The sorbed cadmium is then eluted with 10ml of 1moll(-1) nitric acid in ethanol and is measured by flame atomic absorption spectrometry. The influence of flow rates of eluent and sample solution, iodide concentration and amount of surfactant in retention and elution of cadmium from disks was also investigated. A preconcentration factor of 100 was achieved by passing 1000ml of sample through the membrane disk. The limit of detection (LOD) of cadmium was found to be 0.014ngml(-1). Precision at 2.5mugl(-1) was 1.2% (n=8). The method was successfully applied to the determination of cadmium in some natural water samples. The accuracy was assessed through recovery experiment, independent analysis by graphite furnace atomic absorption spectrometry, and analysis of certified reference waters.     

石墨炉原子吸收光谱法测定超高纯试剂中钙的研究．

研究了超高纯试剂异丙醇中痕量钙的石墨炉原子吸收光谱测定法。制定了石墨炉原子吸收光谱法测定痕量钙的分析程序，试样经挥发浓缩，采用标准曲线法测定；还确定了仪器最佳工作条件，原子化条件等，研究了共存离子的干扰，回收试验及实测样品等。同时将石墨管用氯氧化锆进行适当的处理，并控制合适的仪器操作条件及升温程序，即可提高石墨炉原子吸收法测钙的灵敏度，获得了较满意的结果。     

原子吸收法测定白酒中铅和锰的方法改进

目的:本文以简化操作步骤,改进实验方法为目的,着重研究利用原子吸收光谱法直接测定白酒中的铅和锰。方法:直接对样品进行稀释,用火焰原子吸收法测定锰。以磷酸氢二铵为基体改进剂,用石墨炉原子吸收光谱法测定铅。结果:该方法操作简单快速,减少了试剂用量,而且精密度和准确度都能满足实验要求。结论:该方法是可行的,值得推广使用。     

石墨炉原子吸收分光光度法测定水中硒的不确定度评定

参照JJF 1059-1999<测量不确定度评定与表示>的技术规范,通过对石墨炉原子吸收分光光度法测定水质硒标准样品过程的分析,阐明了硒不确定度的评定步骤和评定方法。     

Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni2+ with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni2+ with 10 mL solution. Under the optimal conditions, the detection limit of Ni2+ is 0.12 ng mL(-1) with R.S.D. of 4.3% (n = 10, c = 100 ng mL(-1)). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.     

电感耦合等离子体发射光谱法测定矿石中银的研究

目前,实验室测定矿石中银的方法主要有银的光度法、火焰原子吸收光谱法、石墨炉原子吸收光谱法等等,为了更好的简化测量过程、提高工作效率,本文旨在建立更适宜的、能满足于高中低含量银的测试方法,采用电感耦合等离子体光谱法测定金属矿中银的含量.样品采用氢氟酸、硝酸、硫酸(体积比10∶5∶1)溶解,赶净氟和破坏有机物后,经(1+1...     

Speciation of chromium in water samples with cloud point extraction separation and preconcentration and determination by graphite furnace atomic absorption spectrometry

A novel method has been developed for the speciation of chromium in natural water samples based on cloud point extraction (CPE) separation and preconcentration, and determination by graphite furnace atomic absorption spectrometry (GFAAS). In this method, Cr(III) reacts with 1-phenyl-3-methyl-4-benzoylpyrazol-5-one (PMBP) yielding a hydrophobic complex, which then is entrapped in the surfactant-rich phase, whereas Cr(VI) remained in aqueous phase. Thus, separation of Cr(III) and Cr(VI) could be realized. Total chromium was determined after the reduction of Cr(VI) to Cr(III) by using ascorbic acid as reducing reagent. PMBP was used not only as chelating reagent in CPE procedure, but also as chemical modifier in GFAAS determination of chromium. The detection limit for Cr(III) was 21 ng L(-1) with an enrichment factor of 42, and the relative standard deviation was 3.5% (n=7, c=10 ng mL(-1)). The proposed method has been applied to the speciation of chromium in natural water samples with satisfactory results.     

石墨炉原子吸收法直接测定饮用水中的铍

采用石墨炉原子吸收法,使用热解涂层石墨管,加上硝酸镁作基体改进剂,直接测定水中的铍。