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1.
汪正  陈天裕等 《分析化学》2002,30(10):1222-1225
端视电感耦合等离子体原子发射光谱在分析过程中易电离元素引起的非光谱干扰,常常使分析结果产生偏差,就不同浓度Na基体对分析谱线产生的干扰进行了实验和研究,并用Y作为内标元素来补偿钠基体的干扰。得出在Robust条件,即高功率和低载气流速条件下,选择合适的离子线,并且离子线的总能量大于10eV下,用内标Y437.494nm可以很好的补偿不同Na含量的干扰。  相似文献   

2.
端视ICP-AES中用铟内标校正钠基体干扰的研究   总被引:5,自引:0,他引:5  
端视电感耦合等离子体原子发射光谱中易电离元素引起的非光谱干扰,常使分析结果产生偏差。本文就不同浓度钠基体对分析谱线产生的干扰进行了试验和研究,并用铟作为内标元素来补偿钠基体的干扰。得出选择用几个内标元素和多条内标谱线时可以校正钠基体的干扰。  相似文献   

3.
电感耦合等离子体质谱法测定高纯氧化钆中痕量稀土杂质   总被引:7,自引:3,他引:4  
刘湘生  蔡绍勤 《分析化学》1997,25(4):431-434
考察了起因于钆基体的多原子离子干扰,当基体浓度为1g/L时,基体质谱对相邻低质量同位素产生严重的峰前沿干扰,基体的多原子离子也会对待测稀土杂质同位素产生严重的谱干扰。研究了Ga,In,I,Cs和Tl内标对基体抑制效应的补偿作用,加入内标元素Tl后,基本上克服了基体效应。  相似文献   

4.
选择不同电离电位的基体元素K、Na、La、Y和Mg,比较研究了它们对分析元素谱线强度的影响,其影响程度与谱线激发电位及基体元素电离电位有定量的相关关系。碱金属基体(K、Na)和非碱金属基体(La、Y和Mg)对分析元素检出限、背景强度及其相对标准偏差的影响显著不同,后者的记忆效应也大于前者。La的电离电位与Na相差不大。但其基体效应与Y相似,表明墓体效应与基体元素的化学性质有关。  相似文献   

5.
ICP-AES中内标法的应用研究 Ⅲ.用内标法校正基体干扰   总被引:1,自引:0,他引:1  
通过观测基体对分析元素发射强度的干扰情况,分析干扰机制,从而确定用来校正基体干扰的内标元素与分析元素的匹配条件。实验结果表明,只要选择合适的内标元素,可以校正基体干扰。  相似文献   

6.
以高纯氧化钇中稀土杂质的ICP-AES测定为例, 研究了基体对分析元素谱线强度的影响及基体效应与工作条件的关系, 指出基体效应除主要来自分析物进样效率的降低外, 大量基体进入ICP降低了激发温度并对分析物的电离产生抑制作用, 提出用Se内标法代替通常的基体匹配法来补偿基体效应。进行了折衷条件选择及联样量确定等研究。实样分析表明, 内标法和基体匹配法所得结果一致, 加入回收率为87-120%, 精度也符合分析要求。  相似文献   

7.
ICP—AES中内标法的应用研究:Ⅲ.用内标法校正基体干扰   总被引:13,自引:0,他引:13  
通过观测基体对分析元素发射强度的干扰情况,分析了扰机制,从而确定用来正基体干扰的内村元素与分析元素的匹配条件。实验结果表明,只要选择合适的内标元素,可以校正基体干扰。  相似文献   

8.
从同位素的选择、基体效应,内标元素的选择及仪器工作条件等方面对实验参数进行了优化,重点研究了等离子体功率及仪器分辨率的改变对铒基体所形成的氢化物多原子离子干扰的影响。通过提高等离子体功率、改变仪器分辨率及数学方程校正等方法,减少和剔除了ErH对Ho和Tm测定的干扰。实验中选取Cs为内标元素,测定了不同含量的高纯氧化铒样品。分析结果与标准加入法结果进行了比较,之间无显著性差异。  相似文献   

9.
刘湘生  蔡绍勤 《分析化学》1997,25(6):652-655
考察了基体对待测稀土杂质元素信号的影响,研究了内标对基体效应的补偿作用。对于不同的基体元素最佳的内标元素是不一致的,Ga、In、I、Cs和Tl是稀土纯度分析中合适的内标元素。内标法简便易行,效果好,其测定方法的精度和回收率令人满意。  相似文献   

10.
建立了ICP-OES内标法同时测定纺织品中砷、锑、铅、镉、铬、钴、铜、镍、汞等9种有害元素的检测方法.采用钇(Y)作为内标添加物,有效补偿了酸性汗液中钠元素造成的背景干扰.结果表明:砷、锑、铅、镉、铬、钴、铜、镍、汞等9种元素的谱线强度与其浓度在(0.03~0.30)~10 mg/L范围内均具有良好的线性关系,检出限分...  相似文献   

11.
Colon M  Hidalgo M  Iglesias M 《Talanta》2011,85(4):1941-1947
The determination of arsenic by inductively coupled plasma mass spectrometry (ICP-MS) in natural waters with high sodium and chloride content has been investigated. The instrument used is equipped with an octopole collision/reaction cell to overcome spectroscopic interferences. Thus, the optimization of collision/reaction gas flow rates is required when using a pressurized cell. A mixture of 2.9 mL min−1 of H2 and 0.5 mL min−1 of He has been found to be suitable for the removal of 40Ar35Cl+ interference.The effect of the introduction of small amounts of alcohol has also been studied in this work under both vented and pressurized cell conditions. It has been observed that the presence of 4% (v/v) of ethanol or methanol results in an increase in arsenic sensitivity. Moreover, under vented cell conditions the addition of alcohol also decreases the formation of polyatomic interference. However, this decrease is not observed under pressurized cell conditions.Different elements have been studied as possible internal standards for arsenic determination in presence of high amounts of sodium. Good results have been obtained for rhodium and yttrium under both vented and pressurized cell conditions. Although the presence of alcohol in the sample matrix also affects their behaviour, rhodium and yttrium are still the most suitable elements to correct for these matrix effects.Different experimental conditions have been compared for arsenic determination in spiked, certified and natural waters with high sodium and chloride content. The best results have been obtained under pressurized cell conditions, in the presence of ethanol and using rhodium as internal standard.  相似文献   

12.
ICP-AES法测定铁矿中的CaO、MgO、Al2O3和MnO   总被引:4,自引:0,他引:4  
用电感耦合等离子发射光谱仪(ICP-AES)测定了铁矿中的CaO、MgO、Al2O3和MnO,用钇内标元素校正基体干扰,对分析谱线、共存元素、酸性条件等进行了讨论。  相似文献   

13.
An evaluation of precision improvements using real-time internal standardization with an axially-viewed inductively coupled plasma (ICP) is presented. New findings are presented with respect to the nature of the noise in the analytical signals from the axial ICP. It is observed that a high degree of correlation exists in the line signals from the axial ICP. Using the yttrium ion line at 371.030 nm as the internal standard, the analytical precision after the application of real-time internal standardization is maintained between 0.1 and 0.2% relative standard deviation (RSD) for ion lines. Precision improvement factors of 3 to 4 are obtained by comparison with the uncorrected results. With atomic lines, real-time internal standardization using the yttrium ion line is less effective, yielding precision values between 0.2 and 0.7% RSD. The precision improvement factors for atomic lines are between 1.5 and 3. Thus, real-time internal standardization provides significant improvements in the RSDs of the line signals. The limits of these improvements are explored and an equation is presented which yields the fundamental shot noise limit for precision. Shot noise limited precision is demonstrated. However, this is not possible for all elements using a single internal standard signal. The effectiveness of real-time internal standardization is shown to be dependent on the nature of the specific spectral line. With the axially-viewed ICP, the dominant phenomenon preventing the full benefit of internal standardization from being obtained is the amplitude of the noise in the line signals and not the degree of correlation between analyte and internal standard signals. A trend is observed for atomic transitions in which lower excitation energy is correlated with higher relative noise amplitudes. This finding is in contrast with previously published work on the radially-viewed ICP. An explanation of this result is proposed which takes into account the influence of vaporizing sample droplets in the observation volume.  相似文献   

14.
电感耦合等离子体质谱法测定农产品土壤中痕量稀土元素   总被引:1,自引:1,他引:0  
建立了电感耦合等离子体质谱法(ICP-MS)测定农产品土壤中15个稀土元素的分析方法.研究了溶样体系用量、标准溶液配制、质谱干扰、内标元素的选择.采用HNO3-HF—H2O2体系电热板溶解样品,稀土元素的溶出率较高.用ICP—MS同时测定土壤中的钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥.以Rh、Re双内标在线校正,有效地降低了信号漂移对分析结果的影响.方法检出限为0.0012—0.0071ng/mL.对实际样品进行连续7次测定,方法精密度为0.2%~4.7%,回收率为97%-114%.经国家标准物质验证,结果与标准值相符.方法弥补了微波消解法的不足,且快速、准确,适合于大批量土壤样品分析.  相似文献   

15.
Cohen NE  Reeves RD  Brooks RR 《Talanta》1968,15(12):1449-1456
Studies were carried out on the optimum conditions for the successful use of a large quartz spectrograph for the determination of thorium, yttrium and the rare earths in silicate rocks. The best line-to-background ratios were achieved by arcing samples in a matrix of 4 % sodium chloride in carbon powder. An atmosphere of 20 % argon and 80% oxygen was used to reduce background and eliminate cyanogen band interference. An anion-exchange procedure was used to separate the rare earths from other elements. The resultant enrichment allowed use to be made of less sensitive rare earth lines in the ultraviolet end of the spectrum where the spectrographic dispersion is greater. Line interferences were studied and necessary corrections for these interferences were calculated. The technique was tested by analysing the standard rocks, G-1, W-1 and CAAS syenite. Good agreement with recommended values was obtained.  相似文献   

16.
为研究并解决测试生物质样品中碱金属和碱土金属含量的干扰,采用微波消解-电感耦合等离子体发射光谱(ICP-OES)法对生物质中的碱金属和碱土金属钾、钙、钠、镁元素进行测定,考察了样品消解后不同的酸体系,共存元素干扰对钾、钠、钙、镁含量测定的干扰研究。经过研究表明,接近分析标准曲线酸浓度的样品干扰小,铅、铟、钛、锰元素对钠元素测定造成干扰,砷、铜、镉对钙元素测定干扰,铝对钾元素测定有干扰,镁测定不受共存元素干扰影响,运用干扰系数法可以减少共存元素对测定元素的误差。各待测元素标准曲线相关系数大于0.9996,检出限为0.0014~0.023 mg/L,玉米芯各元素的相对标准偏差为0.98%~1.9%,加标回收率为80.2%~106%;西瓜皮的各元素相对标准偏差为0.91%~2.3%,加标回收率为85.3%~106%。方法用于测定国家标准物质GBW07603,各元素结果均在标准值参考范围内。方法用于测定生物质中碱金属和碱土金属的结果,用t检验法与离子色谱测定值进行比对,结果无显著性差异。  相似文献   

17.
The matrix effects for single-matrix component (Na or Ca) and mixed-matrix component (Na plus Ca) systems were investigated for an inductively coupled plasma with radial viewing and employing ultrasonic nebulization. Correction for matrix effects was carried out using the internal standard ratio method and a method named proportional correction, both with scandium and yttrium as internal standard elements. The best correction was observed using proportional correction both for the single-matrix component systems and for the mixed-matrix component system.  相似文献   

18.
The effects of a magnetic field on spectral intensities in plasma-jet spectrometry were examined, and detection limits for rare-earth elements were calculated. Plasma-jet emission spectrometry was applied to the determination of lanthanum, yttrium and gadolinium in a monazite sample from which thorium had been separated. A standard addition method was used in order to improve accuracy, and the internal standard and background compensation method was applied to measurements of spectral line intensities to achieve good precision. The coefficient of variation was 1.51% for 50 μg La ml?1.  相似文献   

19.
Before preconcentration the yttrium matrix is separated from the lanthanides by means of cation- and/or anion-exchange. The rare earth elements are then concentrated by coprecipitation with 5.0 mg of iron as Fe(OH) in quartz centrifuge tubes. The dehydrated Fe-REE mixture is then irradiated and counted, without any further major manipulations, by means of Ge(Li) gamma-spectrometry, the59Fe activity acting as a f' x monitor and as an internal standard.  相似文献   

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