微波消解——石墨炉原子吸收光谱法测定紫菜中的铅

应用石墨炉原子吸收光谱法测定紫菜中铅含量,以HNO3-H2O2为氧化剂,微波消解处理样品,磷酸二氢铵作测铅基体改进剂,考察了基体改进剂浓度、灰化温度、原子化温度对吸光值的影响。在最优条件下,低浓度的铅与吸光值具有良好的线性关系,线性方程为：A=0．0058C＋0．0052,r=0．9994,检出限为1．0μg／L。运用该方法测定10次加标样的RSD为1．512％～2．469％,加标回收率为98．4％～101．1％。该方法简单、快速、重现性好,适合日常批量检测。     

用石墨炉原子吸收光谱法测定次磷酸钠中微量铅

试样直接用水溶解,以磷酸氢二铵作测铅基体改进剂,考察了基体改进剂用量,原子化温度以及基体元素对测定的影响,在最佳测定条件下,用石墨炉原子吸收光谱法测定了次磷酸钠中微量铅,测试结果为:线性范围为0～60×10-3μg/mL,检出限为1.6×10-3μg/mL,回收率为94.0%～102.6%,RSD<5%。方法简便,灵敏度高,重现性较好。     

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。     

平台石墨炉原子吸收光谱法测定土壤保水剂中铅、镉

提出在不用任何基体改进剂的条件下,用平台石墨炉原子吸收法测定土壤保水剂中铅、镉的方法。经加标准回收实验表明铅平均回收率101%,镉平均回收率98.4%。本方法切实可行。     

微波消化石墨炉原子吸收光谱法测定中成药中痕量铅、镉方法研究

本文建立了微波消化石墨炉原子吸收光谱法测定中成药中铅、镉方法。方法的相对标准偏差对铅为5.1％,镉为7.0％。回收率铅在94—110％之间,镉在99—112％之间,检出限分别为铅0.6ng/mL、镉0.02ng/mL。     

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茶叶中铅的不确定度评定

通过石墨炉原子吸收光谱法测定茶叶样品中Pb的含量,分析了测试过程中的不确定度的影响因素,并对各不确定度的影响分量进行评定。实验结果显示不确定度的主要来源为称量、容量器具的体积、标准曲线拟合、标准溶液、重复性测定和仪器示值误差等。茶叶中铅的测试结果为:WPb=(1.68±0.014)mg/kg,k=2(置信水平约为95%)。     

微波消解石墨炉原子吸收法测定土壤中铅镉策略探析

本文使用了微波消解法对土壤样品进行前处理,采用了石墨炉原子吸收分光光度法对土壤中的铅、镉进行测定。本方法消解效率高、消解速度快,能够满足土壤中铅、镉的监测分析要求。     

Determination of gallium in human urine by supercritical carbon dioxide extraction and graphite furnace atomic absorption spectrometry

This study presents supercritical carbon dioxide (scCO(2)) extraction as an inherently safer and cleaner sample treatment method for identifying trace gallium in urine samples. Extraction is performed in the presence of a fluorinated beta-diketones chelating agent, 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octanedione (HFOD), by unmodified scCO(2). Quantitative extractions are conducted at 80 degrees C and 20.7 MPa with 15 min static plus 15 min dynamic extractions, and are followed by analysis via graphite furnace atomic absorption spectroscopy (GFAAS). The proposed procedure is successfully applied to determine the concentrations of gallium in real urine samples spiked with various levels of gallium with satisfactory recoveries of 90.8-100.3% (n=6) and relative standard deviations <10%. A standard reference material (SRM), Seronorm Trace Elements Urine, is used to validate the accuracy of the proposed method.     

石墨炉原子吸收法测定头发中硒

利用优级纯硝酸浸润,放置过夜,适当水浴加热的方法,将头发样品制备成溶液,用石墨炉原子吸收法测定头发中硒,在选定的测定条件下检出限0．004mg／l,精密度3．7％,回收率在91．1％-98．2％之间。     

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.     

石墨炉原子吸收法测定废水中铅的不确定度分析

对石墨炉原子吸收法测定废水中铅的不确定度进行评定,系统分析不确定度的来源,计算出该方法的不确定度,为评价方法的可靠性和分析的准确性提供参考。     

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.     

Continuum source atomic absorption spectrometry in a graphite furnace with photodiode array detection

A graphite furnace continuum source atomic absorption spectrometer using a photodiode array detector is described that provides high-resolution wavelength versus absorbance spectra over a 2.5-nm range for a single atomization step. The multiwavelength detection power allows the simultaneous determination of several elements, reduces problems caused by spectral interferences, and automatically corrects for nonzero background absorbance. Each spectrum is acquired in 0.33 s, and several successive spectra can be obtained during a single run. Three-dimensional wavelength-absorbance-furnace temperature spectra can be obtained by using ramped heating steps to provide a rough separation of elements in a mixture. Limits of detection calculated for 19 elements range from 0.1 pg for magnesium to 700 pg for arsenic. The sampling precision was found to be better than 10% relative standard deviation in all cases, with the precision for a single atomization being greatly increased when multiple absorption lines for a single element are observed in the spectrum. The error found for the measurement of the iron concentration in an NBS standard bronze was 8.5%, with the calculated concentration agreeing with the certified concentration within 95% confidence limits.     

Determination of trace aluminum in biological and water samples by cloud point extraction preconcentration and graphite furnace atomic absorption spectrometry detection

A cloud point extraction (CPE) method for the preconcentration of trace aluminum prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) has been developed. The CPE method is based on the complex of Al(III) with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), and then entrapped in non-ionic surfactant Triton X-114. PMBP was used not only as chelating reagent in CPE preconcentration, but also as chemical modifier in GFAAS determination. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PMBP and Triton X-114, equilibration temperature and time, were investigated in detail. An enrichment factor of 37 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of this method for Al(III) is 0.09 ng mL(-1), and the relative standard deviation is 4.7% at 10 ng mL(-1) Al(III) level (n=7). The proposed method has been applied for determination of trace amount of aluminum in biological and water samples with satisfactory results.