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1.
建立了电感耦合等离子体原子发射光谱(ICP-AES)测定超导粉中痕量铁的新方法。优化了仪器工作参数,对痕量铁测定时的基体干扰及消除干扰的方法进行了系统研究,结果表明:大量存在的基体元素产生一定基体效应,并使重现性变差,且由于铁含量甚微,仪器灵敏度不能满足测定的要求,需采用分离富集方法以提高测定结果的准确度和精密度。以三乙醇胺掩蔽基体元素铋和铜,在适宜的酸度条件下,铁与邻二氮菲生成配合物,以活性炭定量吸附,用1∶1硝酸解吸,并对分离富集条件进行了优化。对模拟标准样品进行测定,分析结果与理论值一致,相对标准偏差为2.4%,方法检出限为0.033μg.g-1。该方法已用于超导前驱粉样品中痕量铁的分析,结果令人满意,并进行了回收实验,回收率为95.6%~98.0%。  相似文献   

2.
研究了以强碱性阴离子交换树脂为固定相的离子交换色谱法分离富集土壤中钼,实现了钼与其他常见金属元素离子的选择性分离,富集在色谱柱上的钼以0.5mol.L^-1NH4NO3+2mol.L^-1HNO3洗脱并用富氧火焰原子吸收光谱法进行测定,钼的回收率为99%—101.3%。  相似文献   

3.
选用331弱碱性阴离子交换树脂,对微污染水体中的Cr(Ⅵ)和有机态Cr(Ⅲ)进行了分离富集作用研究,考察了酸度、富集时间、洗脱液类型、洗脱液浓度及溶液中共存离子对分离富集过程的影响。研究表明,分别用1.0 mol·L-1 HCl和2.0 mol·L-1 NH4NO3+0.5 mol·L-1 NH3·H2O可以很好分步洗脱有机态Cr(Ⅲ)和Cr(Ⅵ),利用ICP-AES测定, 该方法对Cr(Ⅲ)和Cr(Ⅵ)的检出限分别为1.1和 1.4 μg·L-1,相应的相对标准偏差RSD(n=6)平均值分别为3.8%和5.6%。该方法适用于自来水、地下水、地表水及生活污水中痕量Cr(Ⅵ)和有机态Cr(Ⅲ)的分离富集及测定。  相似文献   

4.
在10%盐酸介质中,采用717阴离子交换树脂富集金、钯和铂,从而与大部分基体分离。被吸附的金、钯和铂用硫脲解脱后以发射光谱法测定。检出限分别为金:0.04μg,钯:0.04μg,铂:0.09μg。相对标准偏差在11.2%-18.5%之间。  相似文献   

5.
辛仁轩  吴伟 《光谱实验室》2001,18(6):711-714
采用大孔阴离子换换树脂D296分离净化30%TRPO(三烷基氧膦)-煤油中酸性有机杂质,再用甲醇将TRPO-煤油淋洗干净而与脂肪酸分离。最后将脂肪酸等酸性杂质用四甲基氯化铵解吸。柱穿透容量为0.97mmol/g混合脂肪酸。  相似文献   

6.
利用ICP-AES法测定了铋系超导前驱粉(BSCCO)中Fe,Cr,Ni,Si,Al和Ba等微量杂质元素,优化了仪器测定参数并研究了酸的种类及浓度对测定结果的影响。系统研究了BSCCO基体元素Bi,Sr,Pb,Ca和Cu对微量杂质元素测定的干扰,分别测定了每个基体元素对测定元素的校正系数并组成交互干扰校正矩阵,采用全选主元高斯消去法计算出基体元素产生的背景等效浓度,再计算出样品的真实浓度。用此方法对合成标样中的上述微量杂质元素进行了测定,分析结果的回收率99.5%~100.5%,测定了实际样品中的杂质元素,并与ICP-MS法进行了对比,二者结果一致。  相似文献   

7.
建立了ICP-AES同时测定铋系超导材料中Bi、Pb、Sr、Ca、Cu5种金属元素含量的分析方法,优化了仪器的最佳工作条件。该方法无需复杂的前处理,没有谱线和基体干扰,检出限Bi为0.01699μg.mL^-1、Pb为0.02121μg.mL^-1、Sr为0.002854μg.mL^-1、Ca为0.007401μg.mL^-1、Cu为0.003726μg.mL^-1。该法相对误差均小于1.0%,RSD均小于1.0%,简便,快捷,完全满足铋系超导材料中各元素含量的测定。  相似文献   

8.
制备了以Dowex1-X10阴离子交换树脂为填料的固相萃取小柱,建立了固相萃取、全反射X射线荧光分析法(TXRF)测定高冰镍中微量贵金属钯、铱、铂和金含量的新方法,解决了复杂体系中微量贵金属检测前的分离富集难的问题.在0.5mol/L盐酸体系中,TXRF测定高冰镍中钯、铱、铂和金的相对标准偏差(RSD)均小于3.4%,其仪器检出限分别为0.015、0.011、0.013μg/mL和0.01 5μg/mL,方法检出限分别为0.050、0.036、0.043μg/g和0.050μg/g.实际样品的测定结果与ICP-MS基本一致.用TXRF可以同时、快速地测定高冰镍中的贵金属,样品测定结果可靠.  相似文献   

9.
原子光谱法直接测定纯铝材中的砷,受到铝基体的干扰。实验表明,当被测试液中Al的质量浓度大于等于As的5 000倍时,测量误差大于5%。为了降低被测试液中铝的浓度以消除干扰,利用对Al3+吸附作用强的强酸型阳离子交换纤维作为固相萃取剂,通过对萃取剂用量、萃取温度、pH值等条件的研究,得到以下方法:0.900 0 g强酸型阳离子交换纤维在55 ℃,pH 2.0的试液中,对Al3+进行超声辅助萃取5 min,此时以砷酸形式存在的砷不被萃取而留在试液中供测定。结果表明,10.00 mL含砷1.00 μg,铝20.0 mg的试液经过分离后,其中砷未见损失,而残留铝质量浓度约为砷的2 000倍,已不干扰ICP-AES测定As。方法检出限(3 s)为0.027 μg·mL-1,方法定量下限(10 s)为0.091 μg·mL-1。本方法已用于合成样、铝制饮料易拉罐和烘烤食品用铝箔等样品中As的测定,标准加入的回收率98.3%~105%;RSD(n=3) 0.1%~4.3%;结果显示,在本实验所测的铝易拉罐和烘烤用铝箔样品中,砷的含量均低于国家标准(GB/T 3190—2008)的限定值。  相似文献   

10.
建立了离子交换树脂-固相萃取富集-电感耦合等离子体光谱(ICP-AES)联用测定水中的重金属元素Zn,Mn,Cu,Co,Ni,Cd,Pb的方法。实验采用Dowex50WX8强酸型阳离子交换树脂,通过优化富集分离条件和排除共存离子的干扰,最终确定最佳的样品pH,样品流速,洗脱液种类和浓度,样品体积分别为3.0~4.0,3.0 mL·min-1,3.0 mol·L-1 HNO3,200 mL。方法中各元素的检出限和定量限范围分别为0.09~0.45和0.31~1.50 μg·L-1,加标回收率和相对标准偏差RSD(n=6)分别为95.3%~104.2%和1.25%~4.12%。采用该方法测定不同地区的样品,并与直接采用ICP-MS法进行对比,其测定结果基本吻合。实验表明该方法的检出限,定量限可以满足水中重金属元素Zn,Mn,Cu,Co,Ni,Cd,Pb的检测要求,准确性和精密度好,结果可靠,适用于测定水中Zn,Mn,Cu,Co,Ni,Cd,Pb。  相似文献   

11.
从元素检出限、基体效应、ICP稳健性及记忆效应方面实验研究了双铂网雾化与超声雾化两种进样方式对ICP-AES分析性能的影响。结果表明,在超声雾化进样条件下,Cu,Pb,Zn,Cr,Cd,Ni的检出限较双铂网雾化的检出限降低了6~23倍;在基体效应方面,超声雾化进样时基体对元素原子及离子谱线强度的影响均较双铂网雾化系统明显,元素谱线增强/减弱的幅度受元素谱线、基体组成和浓度的影响;Ca和Mg基体对谱线强度的影响强于K和Na基体;离子谱线受基体的影响明显强于原子谱线。超声雾化系统进样时ICP的稳健性要劣于双铂网雾化系统,而且超声雾化系统的记忆效应较双铂网雾化器严重。  相似文献   

12.
纺织品在加工的过程中会引起多种有害元素的污染,为了监控纺织品的质量,建立了微波辅助稀硝酸萃取结合电感耦合等离子体发射光谱同时测定纺织品中砷、锑、铅、镉、铬、钴、铜、镍、汞等九种有害元素的检测新方法。通过萃取剂的筛选和萃取条件的优化,最终确定了用5%的硝酸30mL作为萃取剂,萃取时间为5min,萃取温度为120℃,仪器功率为400W作为微波辅助萃取条件。并用电感耦合等离子体发射光谱对萃取出的九种有害元素总量进行检测。结果显示:本方法的检出限在2.25~112.5μg.kg-1之间,对加标样品的萃取率为73.6%~105%,相对标准偏差(RSD,n=3)为0.2%~1.7%。本方法已成功用于棉布、毛料、涤纶、腈纶四种纺织品样品的检测。  相似文献   

13.
摘要高铬铸铁样品经微波消解,以氧化钇为内标,用电感耦合等离子体发射光谱法同时测定样品溶液中的铬、镍、铜、锰、磷、硅、钼和钛.分析了3种有证国家标准物质,测定值同证书值吻合,验证了方法的准确性.  相似文献   

14.
Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry as well as the high costs of other sensitive methods in compared to flame atomic absorption spectrometry.In this study,thiol-containing sulfonamide resin was synthesized,characterized and applied as a new sorption material for solid phase extraction of nickel in drinking water samples.After preconcentration procedure,flame atomic absorption spectrometry was used for determinations.Optimum parameters were found to be pH=3.2,contact time =20 min and eluate volume=3 mL.The limit of detection was found to be 0.75 ng · mL-1.The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent,high sorption capacity as well as the relatively fast extraction rate.The Ni concentrations in the studied 21 kind of water samples were found to be in the range of BDL-4.0 ng ·mL-1.  相似文献   

15.
Microwave and ultrasound procedures for samples preparations were adopted and the elements were determined by validated flame atomic absorption and inductively coupled plasma–optical emission spectrometry. Student’s t-test was established whether there was a difference between the sample preparation methods. Trueness of certified values by all methods was ensured which were not differing significantly at 95% level of confidence interval. The highest intensity ratio of magnesium (II)/magnesium (I) was obtained at 1120 radiofrequency value to achieve accurate and reproducible results by inductively coupled plasma–optical emission spectrometry. The value of corresponding correlation coefficient (r2) were obtained as >0.990 indicating the excellent linearity for concentration range chosen for each element to be determined in commercial samples. Results showed that concentrations of calcium, magnesium, potassium, sodium, chromium, copper, iron, manganese, selenium, and zinc found in commercially available products are in good agreement with label as declared by the manufacturers. Exposure to aluminum, cadmium, and lead from consumption of products under evaluation was estimated and it was in compliance with permissible level suggested by European Commission regulations. Regarding the food safety monitoring, the proposed methods are rapid and met green chemistry approach so that can be implemented in laboratories easily for routine analysis.  相似文献   

16.
In the present study, a method for determination of BrO3- and Br- using ion chromatograghy coupling with inductively coupled plasma mass spectrometry (IC-ICP-MS) was developed. BrO3- and Br- were separated on a Hamilton PRP X-100 (150 x 4.1 mm, 10 microm) column guarding with a On-guard II RP (4 x 50 mm) column with 10 mmol x L(-1) NH4NO3 eluent solution at 2 mL x min(-1). By using 200 microL sample loop, the detection limits for BrO3- and Br were 0.35 and 0.36 microg x L(-1), respectively. BrO3- had good linearity in the range 4.8-160.0 ng x L(-1). The standard solution linear equation was y = 250.31x-45.43, and R2 = 0.9999. Br had good linearity in the range 4.2-140.0 ng x L(-1). The standard solution linear equation was y = 186.84x-127.10, and R2 = 0.9994. Recoveries of spiked samples were 98.9%-109.5% and 97.4%-106.1%, respectively. The samples included various kinds of Chinese patent drugs, waters, and beverages. Among them, 14 bottled drinking waters and 2 kinds of tap waters were found containing BrO-, while other samples were under BrO3- detection limit. Br- was detected in all samples.  相似文献   

17.
探讨不同种类生物样品中Si和Al等10种元素的测定方法,采用干灰化结合偏硼酸锂碱熔灰分的前处理方法,用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定试样中Si和Al以及Ca,Mg,Fe,Na,P,Mn,Sr,Ti。方法检出限Si为0.15μg·mL-1,Al为0.03μg·mL-1。用国家一级标准物质GBW07604(杨树叶),验证了方法的准确度及精密度,Si和Al的测定的准确度(RE)分别为-0.03%和-3%,Si和Al测定的方法精密度均小于3%,该方法已用于新研制的系列生物标准物质的定值,并取得满意结果。  相似文献   

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