均匀实验设计-电感耦合等离子体发射光谱(ICP-OES)法测定N36锆合金中微量钠元素含量

建立了电感耦合等离子体发射光谱(ICP-OES)法测定N36锆合金中微量钠元素含量的分析方法。对样品溶解方法、观测方式、谱线选择、基体效应干扰等对实验的影响进行了讨论。采用均匀试验设计法确定了最佳的等离子体发生器功率、等离子气流量、辅助气流量、雾化气流量。实验结果表明,锆基体对测定结果有较大影响。采用基体匹配消除干扰,在均匀实验设计优化的仪器测定参数下,实验证明,方法的相对标准偏差(RSD,n=11)5%,加标回收率在95%～105%。所建立的方法快捷、简便、准确,满足核用N36锆合金中微量钠元素的分析要求。     

电感耦合等离子体原子发射光谱法测定N36锆合金中微量钼和铅

建立了电感耦合等离子体原子发射光谱（ICP-AES）法测定N36锆合金中微量钼和铅的分析方法.讨论了样品溶解、基体效应干扰、谱线选择和观测方式等对测定结果的影响.采用均匀试验设计确定最适合的仪器测定参数,包括等离子气流量、辅助气流量、雾化气流量和等离子体发生器功率.结果表明,锆基体对测定结果有较大影响,在试验中采用基体匹配消除干扰,在试验设计优化的仪器测定参数下,使用N36锆合金样品对方法的精密度与准确度进行验证,相对标准偏差（RSD,n=11）低于5%,加标回收率为93%~104%.所建立的方法快捷、简便、准确,满足核用N36锆合金中微量钼和铅元素的分析要求.     

ICP–AES测定铌铪合金中的铪、钛、锆、钨、钽

采用氢氟酸–硝酸溶解铌铪合金样品,建立电感耦合等离子体原子发射光谱法(ICP–AES)测定铌铪合金中铪、钛、锆、钨、钽元素的分析方法。铪、钛、锆、钨、钽的分析谱线分别为232.247,368.519,339.197,224.876,248.870nm,通过基体匹配法消除基体铌的干扰。在优化条件下对铌铪合金样品进行测定,各元素的质量浓度在其线性范围内与其光谱强度呈良好的线性关系,线性相关系数大于0.998,定量限为0.003 6%~0.007 4%。测定结果的相对标准偏差(n=11)小于1%,回收率为96.8%~105.0%。该方法快速、准确,可以满足实际生产中铌铪合金样品的测定要求。     

微波消解–电感耦合等离子体质谱法测定铀合金中铌、钼、锆

建立微波消解–电感耦合等离子体质谱法测定铀合金中铌、钼、锆。铀铌钼锆合金样品经8 mL HNO_3 (1+1)和2 mL HF微波消解并稀释处理后,利用电感耦合等离子体质谱法测定合金样品中铌、钼、锆含量,研究了铀浓度在0～30 μg/L时对铌、钼、锆元素直接测定的影响。铌、钼、锆的质量浓度在各自的范围内与其质谱响应值线性关系良好,相关系数大于0.999。铌、钼、锆的加标回收率为96.10%～105.00%,测定结果的标准偏差为0.74%～2.71%(n=6)。该方法流程简单,无需分离基体元素,可实现铀合金中铌、钼、锆元素的快速测定。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定N18锆合金中Nb,Sn,Fe,Cr元素含量

建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定N18锆合金中Nb,Sn,Fe和Cr含量的分析方法。对溶样方法、基体影响、谱线选择等进行了讨论,结果表明,锆基体对测定结果有一定的影响,在实验中采用基体匹配法消除基体干扰,并对实验条件进行了优化。在优化的实验条件下,该方法用于样品中Nb、Sn、Fe、Cr的测定,测定结果与化学法测定结果基本一致,加标回收率为96.7%~101.0%,相对标准偏差(RSD,n=11)均小于3%。     

电感耦合等离子体发射光谱法测定二硼化锆中26种杂质

建立微波消解样品,电感耦合等离子体发射光谱法测定二硼化锆中26种杂质元素含量的方法。根据二硼化锆的化学组成对杂质检测的影响,确定了各元素最佳分析线;通过考察不同浓度的锆基体对待测元素的影响来确定最佳锆基体浓度;通过萃取法分离硼元素,消除硼对杂质检测的干扰;采用基体匹配法、多谱拟和技术消除了锆基体的干扰。在选定的仪器工作条件下,各待测元素的质量浓度与信号强度成良好的线性关系,线性相关系数均大于0.999。测定结果的相对标准偏差不大于6%(n=11),样品加标回收率为94%~101%。该方法操作简便,测定结果准确,可用于二硼化锆中26种杂质元素的测定。     

电感耦合等离子体原子发射光谱法测定钛合金中锆

建立电感耦合等离子体原子发射光谱法(ICP-AES)测定钛合金中锆元素的含量。采用盐酸-氢氟酸-硝酸溶解钛合金样品,选择357.247 nm为锆的分析谱线,通过基体匹配法消除基体钛的干扰,以电感耦合等离子体原子发射光谱法测定钛合金中锆的含量。锆的质量分数在0%~0.4%范围内与光谱强度呈良好的线性关系,相关系数大于0.999,定量下限为0.21%。测定结果的相对标准偏差小于2%(n=11),样品加标回收率为99.0%~102.7%。该方法快速、准确,能够满足实际生产中钛合金样品的测定要求。     

电感耦合等离子体原子发射光谱法测定N18锆合金中Nb、Sn、Fe、Cr含量

本文建立了电感耦合等离子体原子发射光谱法测定N18锆合金中Nb、Sn、Fe和Cr含量的分析方法。对溶样方法、基体影响、谱线选择等进行了讨论。结果表明,锆基体对测定结果有一定的影响,在实验中采用基体匹配法消除基体干扰,并对实验条件进行了优化。在优化的实验条件下,该方法用于样品中Nb、Sn、Fe、Cr的测定,测定结果与化学法测定结果基本一致,回收率为96.7％～101.0％,RSD(n=11)均小于3％。     

低温多酸溶样-电感耦合等离子体原子发射光谱法测定核用锆材中锗

采用低温多酸无锗损失的样品预处理后,利用电感耦合等离子体原子发射光谱(ICPAES)测定锆合金中锗。对仪器参数以及被测元素的谱线选择进行了讨论。在选定最佳条件下,铁和铬对锗的测定无影响,基体元素锆和合金元素锡对锗测定的影响可以分别采用基体匹配和与ICP-MS法的测定结果进行对比。在选定的仪器工作条件下,对锆合金试样中锗含量进行多次测定,考察了方法检出限、精密度及加标回收率等,方法相对标准偏差小于2%(n=11),回收率为97%~109%。该方法可成功应用于锆合金中锗以及其他主成分的快速检测。     

王水溶解-电感耦合等离子体发射光谱法测定铁矿石中的微量磷

样品经王水分解后,在电感耦合等离子体发射光谱仪上测定了样品溶液中磷的含量。通过实验确定了基体元素的干扰、酸度、样品提升量、雾化气流速、功率、观测高度、分析谱线等分析条件。通过铁的干扰实验结果表明,样品中的基体元素铁不影响磷含量的测定。在用Ｐ178.222 nm分析线测定时,方法的检出限为P 0.0006％（相对于0.1ｇ样品,定容至100 mL）,相对标准偏差在3.14%～6.04％（ｎ＝11）,样品加标回收率在92%～110%。方法测定样品中磷含量的结果同光度法测定结果对比数据相符。     

Determination of iron, copper and zinc in tinned mussels by inductively coupled plasma atomic emission spectrometry (ICP-AES)

Summary An optimisation of the ICP-AES determination of Fe, Cu and Zn in tinned mussels has been carried out. The optimum conditions for the radio frequency power, peristaltic pump flow, plasma gas flow, nebuliser gas pressure, auxiliary gas flow and observation height above load coil were determined manually for each element, since the Simplex method was less adequate. Scans were carried out with the aim of finding the most sensitive spectral lines, whose intensity did not always coincide with literature data. Limits of detection, linearity, precision, and accuracy were also investigated. The possible spectral interferences due to Na, K, Ca, Mg, P, I and nitric acid were studied from three different points of view and the results did not agree. The influence of the matrix on the determination of the above elements in tinned food from the Galician Rias (in the south coast of Galicia) was also studied. The results obtained were comparable to those obtained by AAS.     

Determination of tin in marine materials by using hydride generation-high resolution inductively coulped plasma mass spectrometry

A hydride generation system combined with high-resolution inductively coulped plasma mass spectrometry was used to determine tin in marine materials. The optimization conditions for determination of tin in this system are 0.015 M of sulfuric acid solution as medium, 0.2% (w/v) of sodium tetrahydroborate(III) in 0.015 M of sodium hydroxide solution as a reductant and argon as the carrier gas at a flow rate of 1.1 l min(-1). In order to remove the interferences from transition element ions, a strongly basic anion exchanger was used in this method. Tin was converted to its chlorostannate with 2 M hydrochloric acid followed by passing to an anion exchanger. The tin absorbed on the column was then eluted with 1 M nitric acid. Under the optimized conditions, the detection limit of the method was 12 ng l(-1) without using the anion column as preconcentration method. The results obtained using this method were in good agreement with the certified values of marine standard reference materials. The recoveries for the method when applied to determine trace tin in river water were 95-115%.     

In-situ vaporization and matrix removal for the determination of rare earth impurities in zirconium dioxide by electrothermal vaporization inductively coupled plasma atomic emission spectrometry

A novel method for the determination of trace rare earth impurities in ZrO₂ powder has been developed based on electrothermal vaporization inductively coupled plasma atomic emission spectrometry. A polytetrafluoroethylene slurry was used as a fluorinating reagent to convert both the matrix (Zr) and the analytes (rare earth elements) into fluorides with different volatilities at a high temperature in a graphite furnace. The more volatile ZrF₄ was removed in-situ by selective vaporization prior to the determination of the analytes, removing matrix spectral interferences. Under optimum operating conditions, the absolute detection limits of the analytes varied from 0.04 ng (Yb) to 0.50 ng (Pr) with relative standard deviations less than 5%. The recommended approach has been successfully applied to the determination of trace rare earth impurities (La, Pr, Eu, Gd, Ho and Yb) in ZrO₂ powder and the results were in good agreement with those obtained by pneumatic nebulization inductively coupled plasma atomic emission spectrometry after the separation of the matrix using a solvent extraction procedure.     

Polarographic determination of traces of zirconium in ores by use of complex-forming compounds adsorbable at the dropping mercury electrode

A polarographic method is proposed for the determination of trace zirconium down to the 5 x 10(-9)M level, based on the adsorption of the complex of zirconium with oxalic acid + cupferron + diphenylguanidine at the dropping mercury electrode in sodium acetate-acetic acid solution (pH 5.7). Under optimum conditions the wave-height is proportional to the concentration of zirconium in the range from 0 to 0.4 mug ml . The serious interference from titanium(IV) can be effectively eliminated by solvent extraction with 3% tri-n-octylamine from lN sulphuric acid and stripping with 0.1 M perchloric acid-lM hydrochloric acid-2M nitric acid mixture. The mechanism giving rise to the wave for the zirconium complex has been investigated. The method has been applied to the determination of trace zirconium in ores and ceramics.     

Determination of Sulfaguanidine in Food and Veterinary Pharmaceuticals by Flow Injection Analysis with Spectrophotometric Detection

This work proposes a flow injection analysis system for sulfaguanidine determination in pharmaceutical and food samples. The method was based on the reaction of sulfaguanidine with nitronium ion to produce a colored complex whose absorbance was measured at 545?nm. The flow injection analysis system’s significant parameters were checked by a fractional factorial design 2^7–2 and optimization by a Doehlert matrix. The flow injection analysis system shows optimum values at 0.28, 2.00, and 0.11% (w/v) for N-naphtil ethylenediamine, ammonium sulfamate, and sodium nitrite concentrations, respectively. The possible interferents present in pharmaceutical and food samples were assessed by a multivariate technique and depicted on probability charts, indicating no significant interferences at the 95% level of confidence interval. The method showed detection and quantification limits of 0.012 and 0.039?mg?L^?1, an analytical frequency of 30 readings h^?1 and precision always lower than 5.0% expressed as the relative standard deviation. The obtained results were in accordance with those obtained by high-performance liquid chromatography.     

Determination of trace amounts of sodium and lithium in zirconium dioxide (ZrO2) using liquid electrode plasma optical emission spectrometry

This paper describes a quantitative measurement of trace elements (Na, Li) in high purity zirconium dioxide powder using liquid electrode plasma optical emission spectrometry (LEP-OES). Conventionally, for such type of measurements, inductively coupled plasma optical emission spectrometry (ICP-OES) is frequently employed. The detection limits of elements in zirconium by ICP-OES are degraded due to the spectra interference between the trace elements and zirconium of the matrix, because zirconium is a line rich element in spectra obtained by ICP-OES. LEP-OES is an elemental analysis method developed by the authors. The measurement principle is simple, as follows. Sample solution is put into a narrow channel on a small cuvette and voltage pulse is applied from both ends of the channel. At the center of the channel which is made narrower, the voltage and current are concentrated there, and plasma is generated. From the emission of the plasma, the quantitative analysis of the elements in the solution is achieved. The LEP-OES has the property that the emission of zirconium is relatively weak, so that highly sensitive measurement of trace elements in zirconium matrix can be conducted without interference. Sample solution is prepared by dissolving high purity zirconium dioxide powder and trace amounts of Na or Li with sulfuric acid. The voltage dependence and the pulse width dependence of optical emission spectra are also investigated. With increase of the voltage or the pulse width, the ratio of emission intensities of Na to those of hydrogen increases. This suggests that the ratio of sensitivity of two elements is variable, that means the element selectivity is controllable to some extent by the measurement conditions in LEP-OES. In the case of Na and H, the ratio can be controlled from 7.4 to 21.6%. Finally, the detection limits (3S.D.) of the trace elements, Na and Li, in 4000 μg g⁻¹ zirconium dioxide aqueous solution are found to be 0.02 and 0.133 μg g⁻¹, respectively. These values correspond to 5 μg g⁻¹ for Na, 33.25 μg g⁻¹ for Li in original high purity zirconium dioxide powder. The correlation coefficient of calibration curve was 0.995 for Na, 0.985 for Li. Those are comparable to the literature values of detection limits using ICP-OES.