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1.
根据卡托普利与醋酸铅反应定量生成沉淀的特点,通过用氢化物发生原子吸收法测定沉淀中的铅,可间接测定卡托普利的含量。平均回收率99.8%,RSD值为1.6%。  相似文献   

2.
电热开缝石英管氢化物发生—原子吸收法测定锗   总被引:4,自引:0,他引:4  
谢凤宏  朱英杰 《分析化学》1991,19(12):1445-1447
  相似文献   

3.
顺序注射-氢化物发生原子吸收法测定砷   总被引:6,自引:0,他引:6  
殷学锋  张建君  王小芳 《分析化学》2004,32(10):1365-1367
通过在气液分离器的液体出口处增置微型电磁阀,延长样品和还原剂NaBH4在气液分离器中的反应时间,实现了单注射泵顺序注射-氢化物发生原子吸收法测定砷。本法自动化程度高,分析速度112次/h,样品消耗量为0.4mL;4μg/L As测定10次的相对标准偏差为2.0%;检出限0.09μg/L。用于标样中砷的测定,结果满意。  相似文献   

4.
氢化物发生辅助雾化火焰原子吸收法测定水中铅   总被引:3,自引:0,他引:3  
研究了一种提高火焰原子吸收测定铅灵敏度的新方法——氢化物发生辅助雾化的火焰原子吸收法;方法采用硼氢化钠与铅(Ⅳ)在原火焰原子吸收雾化器喷口处反应生成氢化物,以提高火焰原子吸收法的雾化效率;采用重铬酸钾一酒石酸预处理体系,重铬酸钾氧化样品中铅(Ⅱ)为铅(Ⅳ),酒石酸稳定铅(Ⅳ)的亚稳态化合物;对各种实验参数和干扰情况也进行了研究;方法操作简单、快速,灵敏度比通常的火焰原子吸收法提高了6.8倍;检出限(K=3,n=11)为6.64μg/L,线性范围为0.021~3.2mg/L;测定水样的回收率达94%~99%。  相似文献   

5.
氢化物发生石墨炉原子吸收进展   总被引:1,自引:0,他引:1  
在氢化物发生原子吸收光谱中,石英管是使用较为广泛的原子化器,但由于其气相干扰比较严重,石英管表面性质对分析灵敏度影响较大,因而又发展了石墨炉原子化器。自提出涂钯石墨管原位富集氢化物以后,氢化物发生石墨炉原子吸收受到人们的重视。现将氢化物发生石墨炉原于吸收的主要方法分述如下: 1 石墨炉在线原子化法 所谓石墨炉在线原子化法,是将生成的氢化物直接通入已经达到原子化温度的石墨管里的方法。氢化物可以从石墨炉内气路通入石墨管,也可以从石墨管进样孔进入石墨管。由于石墨炉原子化的温度较高,因而能大大减小可以形成氢化物元素的气相干扰。文献[1]比较了石英管和石墨管两种原子化器的抗干扰能力,其中有关砷和硒的干扰情况见表1。  相似文献   

6.
氢化物发生-原子吸收法测定饮用水中的砷、硒   总被引:4,自引:0,他引:4  
建立了测定饮用水中砷、硒的氢化物发生-原子吸收法,探讨了盐酸、硼氢化钠溶液的浓度以及样品还原处理对测定结果的影响,测定结果的相对标准偏差(n=7)小于3%,回收率为89.1%-110.7%,测定砷的线性范围为0-40ug/L(r=0.9990),测定硒的线性范围为0-50ug/L(r=0.9990),砷、硒的检出限分别为1.06,0.78ug/L。  相似文献   

7.
介绍简易的氢化物发生原子吸收测砷的方法。喷雾器负压将KBH_4吸入反应器,并将生成的AsH_3吸入乙炔-空气焰原子化。石英缝管使灵敏度提高3.5倍。方法的检测限(3σ)为1.8ng/mL(5mL试样)。20ng/mLAs(Ⅲ)标准液10次测定的RSD为3.8%。本法成功地应用于钢铁和地质标样中微量砷的测定。  相似文献   

8.
本文将电热氢化物原子吸收光谱技术应用于食品中微量锑铋测定,检出限可达ppb级。探讨了被测元素价态、预还原条件等因素对测定灵敏度的影响,并应用于罐头食品中微量锑铋分析。  相似文献   

9.
应用氢化物电热原子化装置测定了血清中的硒。采用这种技术可减少试样的基体干扰,提高分析灵敏度,而且具有良好的线性关系。方法测定灵敏度为1.2μg/L(1%吸收),检出限0.4μg/L变异系数6.3%,具有血量少、成本低、方法简便、精度好等优点。  相似文献   

10.
介绍简易的氢化物发生原子吸收测砷的方法,喷雾器负压将KBH5吸入反应器,并将生成的AsH3吸入乙炔-空气焰原子化。石英缝管使灵敏度提高3.5倍,方法的检测限为1.8ng/mL(5mL试样)。20ng/mL As(Ⅲ)标准液10次测定的RSD为3.8%。本法成功地应用于钢铁和地质标样中微量砷的测定。  相似文献   

11.
Berkkan A  Ertaş N 《Talanta》2004,64(2):423-427
Flow injection hydride generation atomic absorption spectrometry (FI-HGAAS) was used for determination of lead in dialysis concentrates. The parameters such as acidity, concentration of oxidising and reducing agents and argon gas flow rate were investigated to reach the best peak height sensitivity. No significant background signal was observed at high salt concentrations. The detection limit, concentration giving a signal equal to three times standard deviation of the blank signal, was 0.7 ng ml−1 for a 500 μl injection volume. Precision of the measurements at the 20 ng ml−1 level was 3.7% R.S.D. The dialysis concentrates analysed by FI-HGAAS were found to have 10-70 ng ml−1 of lead. The same samples were analysed by ETAAS after removing the matrix using solid phase extraction with Chelex 100. The results were in agreement with those obtained by FI-HGAAS.  相似文献   

12.
This paper proposes a method for the determination of lead in aluminum and magnesium antacids employing electrothermal atomic absorption spectrometry (ET AAS). The pyrolysis and atomization temperatures established during the optimization step were 700 and 2200 °C, respectively, using phosphate as the chemical modifier. Under these conditions, a characteristic mass of 25 pg, and limits of detection and quantification of 0.40 and 1.35 μg L−1, respectively were obtained. Some experiments demonstrated that the calibration can be performed employing the external calibration technique using aqueous standards. The precision expressed as relative standard deviation (RSD %) was 4.03% for an antacid sample with lead concentrations of 284.5 μg L−1. The proposed method was applied for the determination of lead in five antacid samples acquired in Salvador City, Brazil. The lead content was varied from 87 to 943 μg g−1. The samples were also analyzed after complete dissolution by inductively coupled plasma mass spectrometry (ICP-MS). No statistical difference was observed between the results obtained by both of the procedures performed.  相似文献   

13.
Hao DQ  Xie GH  Zhang YM  Tian GJ 《Talanta》1996,43(4):595-600
Serum is rapidly digested with a mixture of nitric and perchloric acids at a temperature of 180 +/- 10 degrees C, and hydrochloric acid is used to reduce selenium(VI) to selenium(IV). Selenium is determined by hydride generation flame atomic absorption spectrometry. The results show that this method has the advantages of being sensitive, accurate, rapid and simple. After the serum is digested and diluted, 4.0 ml is taken for the determination. The characteristic concentration, detection limit, variation coefficient, recovery rate and linear range are 2.93 mug 1(-1), 1.55 mug l(-1), 1.6-5.0%, 97.3-99.2% and 0.0-320.0 mug l(-1) respectively. Serum at 4 degrees C and in frozen state can be preserved for at least 7 and 14 days, respectively.  相似文献   

14.
采用HNO3/HClO4(体积比10∶1)消解冶金废水样品,经6mol.L-1 HCl溶液酸化后,加入碘化钾(3%)、抗坏血酸(1%)及硫脲(1%)混合溶液进行还原,用氢化物-原子吸收光谱法(HG-AAS)测定了样品中的As含量.结果表明,该方法的检出限为0.297μg/L,相对标准偏差RSD为5.463%,样品加标回收率为93%~108%;其操作方便、选择性好、灵敏度高、干扰少,适合于复杂废水中微量和痕量As的测定.  相似文献   

15.
L Hansson  J Pettersson  A Olin 《The Analyst》1989,114(4):527-528
Selenium was determined in freeze-dried fish flesh from perch, pike-perch and the fish flesh reference materials MA-A-2 No. 1174 and MA-B-3 No. 151 (both from the International Atomic Energy Agency) by hydride generation atomic absorption spectrometry. Four different decomposition procedures were tested. They yielded consistent results for the four specimens, but the certified concentration level of selenium in the reference material MA-A-2 was not reached. This indicated losses or the presence of very stable selenium-containing compounds in this fish flesh. Neutron activation analysis of the reference material, however, was in agreement with those results obtained.  相似文献   

16.
J Cacho  V Ferreira  C Nerín 《The Analyst》1992,117(1):31-33
The optimization of lead hydride generation in aqueous ethanolic media and the influence on its generation of the wine components, both white and red, have been studied. These interferences were overcome by careful control of the parameters affecting hydride generation and the procedure was applied to the determination of Pb in wines. The method is fast, accurate and sensitive and can be used to quantify 24 ppb of Pb in wines.  相似文献   

17.
氢化物发生-原子荧光光谱法测定中草药中的微量铅   总被引:1,自引:0,他引:1  
采用水煎煮法提取中草药,HNO3-H2O2密闭消解体系消解样品,应用氢化物发生-原子荧光光谱法测定中草药及其提取液中的微量铅;优化了仪器工作及实验条件,荧光强度与Pb质量浓度在0.49~400 μg/L范围内呈线性关系,相关系数:0.9996,检出限:0.49 μg/L;发现部分提取液中Pb量比原中草药样品中Pb量有明显降低.  相似文献   

18.
 A method was developed for the determination of Sb in wine by electrothermal atomic absorption spectrometry, based on preconcentration by hydride generation with collection directly in the graphite furnace. Thiourea was added for prereduction of Sb(V) to Sb(III). The hydride was directly generated from diluted wine. Palladium was used as modifier in the collection step; the overall efficiency of the hydride/trapping system was found to be 67%. Sb was determined in several samples of red wine; the concentrations found were in the range 0.6 to 5.7 μg/L Sb. The detection limit of the method was 39 pg Sb, corresponding to 0.13 μg/L Sb in wine when 0.3 mL wine was analyzed. Received: 3 November 1995/Revised: 22 February 1996/Accepted: 24 February 1996  相似文献   

19.
The possible benefits of the addition of an anionic surfactant, didodecyldimethylammonium bromide, in the determination of arsenic, by flow injection hydride generation atomic absorption spectrometry using a flame-heated quartz tube atomizer, were studied in the light of previous reports concerning the effects of surfactants on chemical vapor generation procedures. Concentrations of arsenic between 5 and 30 μg l−1 were used. Calibrations in the presence and absence of the surfactant in the sample solution were not significantly different, either for the case where vesicles were formed in the presence of the analyte or where they were preformed in the surfactant solution and then added to the analyte. The surfactant had no effect on recoveries in the presence of copper, nickel or bismuth. The addition of the surfactant to the acid carrier and/or borohydride streams had no effect. It is proposed that there may be a greater role for surfactants in the improvement of the processes by which the hydride is transferred to the bulk gas phase than has been attributed in previous reports on this subject.  相似文献   

20.
 A method was developed for the determination of Sb in wine by electrothermal atomic absorption spectrometry, based on preconcentration by hydride generation with collection directly in the graphite furnace. Thiourea was added for prereduction of Sb(V) to Sb(III). The hydride was directly generated from diluted wine. Palladium was used as modifier in the collection step; the overall efficiency of the hydride/trapping system was found to be 67%. Sb was determined in several samples of red wine; the concentrations found were in the range 0.6 to 5.7 μg/L Sb. The detection limit of the method was 39 pg Sb, corresponding to 0.13 μg/L Sb in wine when 0.3 mL wine was analyzed. Received: 3 November 1995/Revised: 22 February 1996/Accepted: 24 February 1996  相似文献   

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