APDC和MIBK萃取富集石墨炉原子吸收法测定天然水、废水中的硒

本文研究了天然水及废水中痕量硒的石墨炉原子吸收测定方法。天然水、废水等经硝酸—高氯酸进一步消化后,用APDC和MIBK萃取富集,用原子吸收石墨炉法测定。检出限0.7μg·L~(-1)。结果令人满意。     

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。     

石墨炉原子吸收光谱法测定高纯三甲基铝 三乙基铝中痕量有害元素杂质

用石墨炉原子吸收光谱法测定了高纯三甲基铝和三乙基铝中痕量Fe、Cu、Mg、Au、Cd和Ga,样品处理安全可靠,测定限在0.1～1μg/g之间。对方法的准确度和产品纯度控制标准进行了讨论。     

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痕量金—测量方式对分析准确度的影响

本文报道了用不同厂家的仪器、不同种类的石墨管,不同测量方式对石墨炉原子吸收测定地球化学样品中痕量金分析准确度的影响,研究了其影响的主要原因。     

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。     

石墨炉原子吸收法测定洗涤剂中砷含量

建立了石墨炉原子吸收光谱法测定洗涤剂中砷含量的方法。采取硝酸及高氯酸法处理样品,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=0.0012X+0.0009,相关系数r=0.9994。检出限为0.16 ug/L,回收率为92.9%～101.4%,相对标准偏差为1.42%～3.18%。该方法具有快速、准确、灵敏度高等优点,适用于洗涤剂中砷含量的检测。     

原子荧光法测定饲料添加剂中的砷

砷广泛存在于自然界中，为有毒有害元素之一，必须严格限量。传统的理化法：二乙氨基二硫代甲酸银分光光度法测砷操作繁琐费时，灵敏度低，试剂毒性大且测试周期长。石墨炉原子吸收光谱法和氢化物发生原子吸收光谱法存在仪器要求较高、操作条件要求严格等问题。而近年来获得迅猛发展的氢化物-非色散原了荧光光洁分析是我国具有自主知识产权的分析仪器，     

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。     

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。     

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。     

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.     

乳浊液进样-石墨炉原子吸收法快速测定牛奶中的铬

目的:快速准确测定牛奶中的铬含量。方法:前处理采用稀释液超声处理牛奶样品,并用石墨炉原子吸收法测定铬,对稀释液的配比浓度,超声时间等条件进行优化。结果:在优化后的条件下,对牛奶样品进行处理分析,测定的相关系数r=0.9997,方法检出限为0.18 ug/L,加标回收率在96.1%~102.9%。结论:本方法操作简单、快捷,具有良好的准确性和可靠性。     

Slurry analysis after lead collection on a sorbent and its determination by electrothermal atomic absorption spectrometry

In this study, in order to eliminate the drawbacks of elution step and to reach higher enrichment factors, a novel preconcentration/separation technique for the slurry analysis of sorbent loaded with lead prior to its determination by electrothermal atomic absorption spectrometry was described. For this purpose, at first, lead was collected on ethylene glycol dimethacrylate methacrylic acid copolymer (EGDMA-MA) treated with ammonium pyrolidine dithiocarbamate (APDC) by conventional batch technique. After separation of liquid phase, slurry of the sorbent was prepared and directly pipetted into graphite furnace of atomic absorption spectrophotometer. Optimum conditions for quantitative sorption and preparation of the slurry were investigated. A 100-fold enrichment factor could be easily reached.

The analyte element in certified sea-water and Bovine-liver samples was determined in the range of 95% confidence level. The proposed technique was fast and simple and the risks of contamination and analyte loss were low. Detection limit (3δ) for Pb was 1.67 μg l⁻¹.     

Determination of trace lead in water samples by continuous flow microextraction combined with graphite furnace atomic absorption spectrometry

A new method of continuous flow microextraction (CFME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of trace lead in water samples. A drop of 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) dissolved in benzene is injected into a glass chamber by a microsyringe and held at the outlet tip of a PTFE connecting tube, the sample solution flows right through the tube and the glass chamber, the solvent drop interacts continuously with the sample solution, and the analyte was extracted into the drop and concentrated. After extracting for a period of time, the drop was retracted into the microsyringe and directly injected into graphite furnace for determination of Pb. Several factors affecting the extraction efficiency, such as solution pH, sample flow rate, drop volume and extraction time, were optimized. Under the optimized conditions, a concentration factor of 45 was achieved, and the detection limits for Pb were 12 pg mL(-1). The relative standard deviation for six replicate analyses of 10 ng mL(-1) Pb was 6.8%. The proposed method was applied to determine of trace Pb in water samples with satisfactory results.     

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.     

Preliminary kinetic study on the degradation of nitrobenzene by modified ceramic honeycomb-catalytic ozonation in aqueous solution

In this study three major types of preconcentration methods based upon different principles (cation exchange, physical absorption and hydrophobic extraction) were evaluated and optimized for the extraction and determination of three highly toxic heavy metals namely Cd, Pb and Sn by graphite furnace and hybrid generation atomic absorption spectrometry in real samples. The optimum analytical conditions were examined and the analytical features of each method were revealed and compared. Detection limits as low as 0.003-0.025 microg L(-1) for Cd(2+), 0.05-0.10 microg L(-1) for Pb(2+) and 0.1-0.25 microg L(-1) for Sn(4+) depending on the extraction method were obtained with RSD values between 3.08% and 6.11%. A preliminary assessment of the pollution status of three important natural ecosystems in Epirus region (NW Greece) was performed and some early conclusions were drawn and discussed.     

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。