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建立了微波消解-石墨炉原子吸收光谱法测定土壤样品中的镉元素含量的方法。采用微波消解和HNO3-HF-H2O2酸系消解样品的前处理方法效果相对较好,消解速度快,能很好地处理土壤中有机质。通过正交实验优化了升温程序,灰化温度选择680℃,原子化温度选择1 600℃,同时通过对基体改进剂的比选,选择0.50μg/mL氯化钯溶液作为基体改进剂时效果相对较好。该方法镉的检出限为0.018 ng/mL,测定下限为0.072 ng/mL,方法精密度(RSD值)为0.9%~2.4%,加标回收率为97.0%~102.7%,符合岩石矿物分析规范的要求。微波消解-石墨炉原子吸收光谱法测定土壤中镉含量的方法具有操作简便、检出限低、干扰少、精密度高、准确度好的特点。 相似文献
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建立了石墨炉原子吸收法快速测定丹参药材中铅和镉元素含量的方法。利用微波消解样品,选择1.0%磷酸二氢铵和0.2%硝酸镁作为基体改进剂,用石墨炉原子吸收方法完成铅镉元素测定。结果表明,方法线性关系良好,铅和镉的相关系数分别为0.9995和0.9992;检出限分别为0.427μg/L和0.082μg/L;精密度分别为7.44%和10.97%;加标回收率分别为90.5%和104.0%。该方法是一种简便、快捷、准确的分析方法,可为丹参的进一步研究提供科学依据。 相似文献
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本文建立了石墨炉原子吸收法测定土壤样品中痕量铊的方法。样品经盐酸-硝酸-高氯酸-氢氟酸分解后,以抗坏血酸作基体改进剂消除基体影响,用石墨炉原子吸收进行痕量铊测定。方法测定痕量铊的方法检出限为0.2ng/g,精密度(RSD)为3.19%,结果令人满意。 相似文献
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钼是饮用水、地表水和地下水水质的控制指标之一。当硫酸盐(以SO2-4计)浓度达到500 mg/L时,对钼的石墨炉原子吸收分析法产生显著干扰。考察了氯化钙、硝酸铵、硝酸镁、硝酸钯、磷酸二氢铵和抗坏血酸几种基体改进剂对石墨炉原子吸收法测量钼的干扰研究。结果表明,硝酸钯-硝酸镁混合基体改进剂消除硫酸盐干扰效果最佳,其他基体改进剂虽能不同程度地提高测量准确度,但灵敏度下降、背景吸收较大、测量精度不高。通过对石墨炉升温程序的优化,采用硝酸钯-硝酸镁基体改进剂,灰化温度可达1 400℃,利于基体驱除,而且背景值小、吸收峰形好。钼的线性测量范围为0~50μg/L,方法检出限为0.6μg/L;实际样品测量的相对标准偏差为5.7%~14.8%(n=6),加标回收率为81%~96%。与MIBK萃取GFAAS法和ICP-MS法相比,该方法操作简便、分析成本低,易于推广应用。 相似文献
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研究了利用硝酸作消解试剂微波消解饲料,在赶剩余酸和氮氧化物过程中,添加1~3 mL氢氟酸除去饲料中的硅,得到清澈消解溶液。磷酸二氢铵为基体改进剂,石墨炉原子吸收光谱法测定饲料中镉的含量,结果表明,该法准确度较高,效果良好。 相似文献
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Determination of copper, lead, and nickel in edible oils by plasma and furnace atomic spectroscopies
Lori B. Allen Paul H. Siitonen Harold C. Thompson Jr. 《Journal of the American Oil Chemists' Society》1998,75(4):477-481
An atmospheric pressure microwave digestion procedure is described for the determination of copper, lead, and nickel in edible
oils. The digestion procedure is compatible with either inductively coupled plasma atomic emission spectrometry (ICP-AES)
or graphite furnace atomic absorption spectrometry (GFAAS). Instrument conditions are specified to allow the simultaneous
determination of all three metals for each sample introduction. Method detection limits were element-specific but equal to
or less than 50 ng/g with ICP-AES and 30 ng/g with GFAAS. Results from spike and recovery experiments at levels of 50, 100,
and 200 ng/g are reported for corn and soybean oil. For soybean oil, recoveries at 100 ng/g were 90, 100, and 106%, respectively,
for copper, lead, and nickel with ICP-AES, and 89, 106, and 96%, respectively, with GFAAS. Recoveries for corn oil spiked
at 100 ng/g were 93, 95, and 103%, respectively, for copper, lead, and nickel with ICP-AES, and 90, 117, and 100%, respectively,
with GFAAS. Day-to-day reproducibility was demonstrated by similar method recoveries and reproducibilities in independent
analysis of two canola oil sample sets that were spiked at 100 ng/g. 相似文献
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石墨炉原子吸收光谱法是一种操作简便、灵敏度高、检出限低的元素测定方法,但测砷时有较为严重的基体干扰。本研究采用不同基体改进剂以消除基体干扰,优化了原子化温度,对比了不同的消解方法,建立了海洋产品中砷的石墨炉原子吸收的测定方法。最佳原子化温度为2750℃,以氯化钯与硝酸镍混合液为基体改进剂,可以得到较好结果。高氯酸浓度升高,虾粉的测量结果下降,盐酸浓度小于等于1%,对虾粉的测定结果影响不显著,达到3%后,虾粉的测定结果显著下降。砷与钠、钾、钙、镁的比例为1∶400,结果显示离子没有干扰,砷与铁的比例为1∶200,结果显示没有干扰。 相似文献
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研究用火焰与石墨炉原子吸收分光光度法测定美国NSI公司的能力测试样品中痕量金属元素:Mn、Fe、Pb、Zn、Ag、Cu、Cd.采用加标回收试验判断样品基体干扰程度,加入磷酸二氢胺和硝酸镁作为基体改进剂,降低了石墨炉测定Ag、Cd时的背景吸收,在工作曲线最佳测定范围内提高了测定准确度.该方法测定结果的相对误差<±4%,用于能力检测结果满意。 相似文献
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石墨炉原子吸收光谱法测定茶叶中铅 总被引:1,自引:0,他引:1
目的:探讨茶叶中铅的检测方法,并用该法测定10个样品(含2个标准样品)的Pb含量。方法:应用基体改进剂,用石墨炉原子吸收光谱法测定茶叶中铅。结果:(1)茶叶中Pb含量的测定适宜条件为:磷酸二氢铵作为基体改进剂,灰化温度700℃,原子化温度2000℃;(2)本法铅的检出限为1.1μg.L-1,回收率为94.0%~108.8%;(3)抽检的市售8种茶叶种有2种铅含量大于5mg.kg-1。结论:该法准确灵敏,回收率好,可满足实际检测要求。 相似文献
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This paper proposes a low cost, simple, fast method for determining Ni and Cd in biodiesel samples by graphite furnace atomic absorption spectrometry (GFAAS). The method was evaluated in biodiesel from different sources. Tungsten was used as a permanent modifier and the samples were prepared in the form of microemulsions, by mixing about 0.5 g of biodiesel with 5 g of surfactant (Triton X-100) in volumetric flasks and completing the volume with HNO3 1% (v/v). The detection limits obtained for Ni and Cd in microemulsions were ≤0.9 and 0.1 μg L−1, respectively. The relative standard deviation (% R.S.D., n = 12) was ≤8.20% for Ni (washed animal fat sample) and ≤4.71% for Cd (sunflower oil sample). Accuracy was checked based on addition and recovery experiments, which yielded recovery rates varying from 93% to 108% for Ni and from 98% to 116% for Cd. Sample preparation is rapid and easy, and the use of an inorganic standard for calibration makes this sample preparation procedure suitable for routine applications. 相似文献