共查询到19条相似文献,搜索用时 93 毫秒
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采用同一种前处理方法即硝酸和高氯酸消解处理烟草样品后,氢化物发生-原子荧光光谱法测定烟叶中砷、铅;原子吸收光谱法测定烟叶中镉。样品溶液介质为10%的盐酸,对7个样品平行3次重复实验,其相对标准偏差为砷:0.81%—4.96%、铅:2.82%—5.83%、镉:0.96%—4.60%,砷、铅、镉的检测线性范围分别为:0.0—120.0、0.0—60.Oμg·L-1和0.0—800.0μg·L-1,加标回收率:砷在94.5%—96.9%之间、铅在92.7%—101.6%之间、镉在102.2%—110.9%之间。 相似文献
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通过对不同产地几种中药材中砷、铅、镉、铜以及无机砷、三价砷含量的分析测定,得出样品中砷、铅、镉、铜以及无机砷、无机三价砷的测定RSD〈3%,加标回收率在91.32%—109.7%之间。11个样品的总砷含量在0.047—1.681μg/g之间,均低于2μg/g;无机砷含量为0.023—1.294μg/g;无机三价砷含量为0.019—0.918μg/g;铅含量两份样品未检出,其余样品为0.007—0.786μg/g,均低于5μg/g;镉的测定,两份样品未检出,其余样品含量为0.007—2.129μg/g,其中两份样品大于0.3μg/g;铜含量为4.441—14.07μg/g,均低于20μg/g。研究发现同种药材不同产地的重金属含量差异较大,部分产地金银花中镉含量超标严重,无机砷和三价砷含量相对较高,需引起重视。 相似文献
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用ICP-AES方法测定淀粉中铅、砷的含量 总被引:4,自引:3,他引:1
采用ICP-AES(电感耦合等离子体发射光谱)法,以硝酸镍作为基体改进剂,对淀粉中的铅、砷含量进行了测定;探讨了样品灰化方法及灰化原子化温度、基体改进剂对测定结果的影响.实验结果表明,用ICP-AES方法测定淀粉样品中铅、砷一类有害重金属含量,数据、结果的重现性好,方法简便易行、测定结果准确. 相似文献
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电感耦合等离子发射光谱法用于植物油多元素同步测定研究 总被引:2,自引:0,他引:2
用全谱直读电感耦合等离子体发射光谱法同步测定了植物油中的铁、铜、钴、镍、铅、铝、锌、镉、铬、锰和镁11种金属元素,考察了硫酸炭化灰化法、硝酸炭化灰化法、微波消解法、活性炭炭化灰化法以及燃烧炭化灰化法五种样品前处理方法对测定结果的影响,最后采用硫酸炭化灰化法处理样品,在0.1和0.5mg·kg-1两个浓度水平对实际样品加标的平均回收率为70.4%~113%,相对标准偏差1.01%~10.6%,11种元素的方法检出限在0.1~3.6 μg·kg-1之间.方法应用于豆油、花生油、芝麻油、菜籽油、茶油、精炼油、调和油等植物油样品中11种金属元素的测定,结果令人满意. 相似文献
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消化-石油醚提取氢化物-原子荧光光谱法测定食用油中砷 总被引:5,自引:0,他引:5
采用消化 -石油醚提取方法处理食用调味油样品 ,以氢化物 -原子荧光光谱法测定砷 ,研究了样品的处理方法、线性关系及检出限 ,建立了快速测定食用调味油中砷含量的原子荧光光谱法。相对标准偏差小于1.79% ,加标回收率 96 .7%— 10 3.8%。 相似文献
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研究了微波灰化法处理渣油,试验了微波灰化的恒温时间、灰化温度及取样量对样品处理效果的影响。结果表明,微波灰化温度800℃、恒温1.5h、样品量5g左右时,样品灰化完全。用原子吸收光谱法测定样品中的微量金属元素Fe、Na、Ni、V、Cu、Ca的含量,精密度在2.2%—5.5%之间、相对误差小于7.1%、回收率在91.2%—110.0%之间。与传统的灰化法相比,没有显著性差异,灰化时间由十几个小时缩短为1.5h左右。微波灰化具有升温速度快、易控制,最高温度可达1200℃;灰化时间短,冷却速度快;精确、安全等特点。 相似文献
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飞灰含碳量的定量分析需要不同含碳量梯度的飞灰样品作为定标之用。通常做法是用煤粉按照快速灰化法的要求灼烧得到不同含碳量的灰样,用于定标分析。但是这与实际锅炉飞灰的成分存在一定差异,需要对光谱特性的差异进行研究来指导实际定标工作。因此,对比了快速灰化法制备的不同含碳量的煤灰样品与锅炉飞灰在特征谱线强度、等离子温度等等离子光谱特征方面的差异。实验证明快速灰化法制备的煤灰样品的Fe,Mg和Al谱线强度强于锅炉飞灰样品,飞灰等离子温度低于所制备的煤灰样品的等离子体温度,这可能是不同处理过程的物理化学特性差异造成的。用主成分分析法考察了导致光谱差异的主要原因,认为Fe,Mg,Al和Si等元素是导致二者在光谱特性差异的主要因素,这可能因为实验室内按照快速灰化法进行制样的飞灰相应矿物质组成不同所导致的。在用灼烧后的煤灰定标未燃碳时,应注意由于成灰过程不同所造成的Fe,Mg,Al和Si等元素含量和形态不同所带来的影响。 相似文献
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《光谱学快报》2013,46(4-5):405-417
Abstract Digestion methods such as dry and wet ashing and microwave oven were examined at various conditions to determine a rapid, reliable, and simple digestion procedure for yogurt. Digestion by microwave oven was found to be an excellent method in comparison with dry and wet ashing methods when only Al and Zn in yogurt samples were determined. Iron in this matrix is not completely digested by the microwave oven method at the examined conditions. From the obtained results, yogurt can also be a good source of essential nutrients such as minerals in human diet, especially zinc. Aluminum concentrations in yogurt samples fermented in Al containers were found to be significantly higher than in plastic containers. Al concentrations of yogurt taken from the bottom of the container were found to be higher than from the center and top of Al containers. The determinations of metals were carried out via an atomic absorption spectrophotometer using calibration curve and standard additions methods. Aluminum concentrations in yogurt samples produced in big production centers were found to be significantly higher than the other yogurt samples produced in‐house when plastic containers were used. 相似文献
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高压消解-ICP-AES测定木材及木制品中的铜铬砷 总被引:1,自引:0,他引:1
研究了木材及木制品的制备,样品被制成锯末,过孔径为0.5mm的筛,在105℃烘干4~5 h,采用方差分析法进行样品均匀性试验.比较了湿法、干法、高压消解(包括密闭微波消解系统和钢衬聚四氟乙烯消解罐消解)样品的前处理方法.从比较结果来看,湿法消解适用于测定样品中可溶性的铜铬砷,干法消解和高压消解适用于测定样品中总的铜铬砷,但干法消解使砷有挥发损失.探讨了酸度效应和基体效应.建立了高压消解-ICP-AES测定木材及木制品中铜铬砷总量的方法.铜铬砷的检出限(3σ)分别为:1.2,0.2,7.1 mg·kg-1,相对标准偏差为0.2%~1.5%,回收率为92%~106%.该方法为控制木材、木制品及其废弃物中有害物质提供了更为合理的结果,已应用于实际的检测工作. 相似文献
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采用干灰化法、HNO_3-H_2O_2湿法消解法和HNO_3-HClO_4湿法消解法分别处理枸杞子样品,利用原子吸收光谱法测定各组样品中Na,K,Ca,Mg,Fe,Cu,Zn,Ni,Pb,Cd十种元素的含量,探讨简单、快捷、准确地测定枸杞子中矿物质元素的前处理方法。结果表明:干灰化法的回收率范围为89.88%~102.15%,标准偏差(RSD)3.037%;HNO_3-H_2O_2湿法消解法的回收率范围为92.34%~103.21%,标准偏差(RSD)2.751%;HNO_3-HClO_4湿法消解法的回收率范围为94.52%~102.10%,标准偏差(RSD)2.496%;三种方法均具有较好的准确度和精密度,但相对于干灰化法和HNO_3-H_2O_2湿法消解法,HNO_3-HClO_4湿法消解法回收效果较好,精密度更高。HNO_3-HClO_4湿法消解法测得Na,K,Ca,Mg元素含量的平均值高于干灰化法和HNO_3-H_2O_2湿法消解法,差异有统计学意义(p0.05)。此外,HNO_3-HClO_4体系湿法消解法耗时短、消耗试剂量少、消解完全。因而,HNO_3-HClO_4体系湿法消解法可作为原子吸收光谱法测定枸杞子矿物质元素含量较好的前处理方法。 相似文献
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A procedure has been developed for the direct determination of cadmium in whole blood by furnace atomic absorption spectroscopy. No ashing procedures are necessary thus avoiding positive errors caused by contamination in wet ashing or negative errors caused by volatilization of the cadmium during dry ashing techniques. The whole blood samples are immobilized on a pretreated small filter paper disk which is then dropped into a carbon bed atomizer, heated with an RF coil. Decomposition and atomization take place in the carbon bed and the combustion products are drawn into the optical light path for absorption measurements. In contrast to commercial furnace atomizers, there is no atomization program which thereby avoids loss of cadmium by volatilization and greatly reduces the background and chemical interference effects due to the highly variable matrix of blood. Typical results are reported. 相似文献
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植物标样多元素测定的五种前处理方法比较 总被引:22,自引:1,他引:21
本文采用植物样品的五种前处理方法,即干灰化法,硝酸+硫酸+高氯酸法,硝酸+硫酸+高氯酸+氢氟酸法、硫酸+过氧化氢法、灰化+碱熔法,对植物标样GBW07603作样品分解,试液用ICP-AES法进行十九种常量及微量元素的测定。 相似文献
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《Current Applied Physics》2007,7(2):211-214
Homogeneous glow plasma at atmospheric pressure without streamers and arcing was generated by making use of a radio-frequency (RF, 13.56 MHz) power supply. Oxygen gas was added to Ar/He gas as reactive agents for photo-resist (PR) ashing. The input power, flow rate, oxygen concentration, treatment time, substrate temperature are controlled for high ashing rate and uniform ashing. Thickness of PR film was measured by NANOSPEC (AFT200) and α-Step (P-10). An unstable discharge occurs destroying the uniformity, when the input power exceeds a threshold value determined from the distance between the substrate and plasma source. An increase of oxygen quantity or temperature increase makes high ashing rate, but the ashing surface is rugged. The PR ashing rate was related to oxygen atom in plasma. The number of treatment may not be important in PR ashing at the atmospheric pressure. 相似文献
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悬浮进样探针原子化石墨炉原子吸收法测定地质样品中的铬 总被引:3,自引:0,他引:3
本文应用探针恒温原子化技术 ,系统研究了铬的分析性能 ,应用固体悬浮进样 ,直接测定了地质样品中的痕量铬 ,方法的 RSD为 3.0 %~ 6 .5 % ,检测限为 5 .1× 10 - 1 2 g铬 ,标准物质的测定结果满意 相似文献