电感耦合等离子体发射光谱法(ICP-OES)测定钴白合金中的锗

建立了一种电感耦合等离子体原子发射光谱法(ICP-OES)测定钴白合金中锗含量的分析方法,确定了溶样方法和分析谱线,进行了基体元素的干扰等实验,对方法精密度和准确度进行了考察,结果表明,方法的检出限为0.043 μg/mL,对钴白合金中锗的测定结果与其它标准分析方法分析结果基本一致,方法的相对标准偏差RSD在1.1%~1.9%(n=7),样品的加标回收率在98.5 %~102.1 %。所建立的方法准确、快速,适用于钴白合金中锗的测定。     

Problems,possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum,palladium and rhodium in samples with different matrix composition

The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g^− 1 were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts.     

Analytical Characterization of a Solution Cathode Glow Discharge with an Interference Filter Wheel for Spectral Discrimination

Solution cathode glow discharge–atomic emission spectrometry (SCGD–AES) has attracted increasing attention in recent years in water and environmental analysis. In this article, the traditional spectrometer was replaced by an interference filter wheel for spectral discrimination using SCGD–AES. The aforementioned interference filters selected the spectral lines of Na, K, Ca, Li, Sr, Rb, and Cs. These spectral signals were transferred to weak currents using a photomultiplier tube and amplified by a picoammeter. The solution flow rate, discharge current and slit width were optimized individually. The analytical performance of SCGD coupled with an interference filter wheel was studied for atomic emission (SCGD–IFW–AES). The results show that the limits of detection for Na, K, Ca, Li, Sr, Rb, and Cs were 0.16, 0.36, 107, 0.53, 330, 1.93, and 13.58?µg/L, respectively. The relative standard deviations of the spectral intensities for the seven elements were 0.58, 0.94, 0.69, 0.70, 0.63, 0.67, and 0.65%, which indicated that the system operated stably. Matrix effect experiments were performed to study the effect of different concentrations of Na on the spectral intensities of K and Ca. Based on these measurements, the concentration of K in physiological saline was determined to be 0.534?mg/L by SCGD–IFW–AES.     

Determination of phosphorus in waste-waters by inductively-coupled plasma atomic emission spectrometry

Inductively coupled plasma—atomic emission spectrometry offers a simple and rapid method for the determination of total phosphorus in waste-waters: the optimum operating conditions are described. The detection limits are 0.02, 0.04, and 0.11 μg ml^-1 at the 213.618, 214.914, and 253.565-nm lines, respectively. Interferences by other elements are negligible at the concentration levels of these elements in environmental and waste-waters, except for the spectral interference of copper on the lines at 213.618 and 214.914 nm. Differences in emission response for various inorganic and organic phosphorus compounds are small. Analytical results for phosphorus in municipal and industrial waste-waters agree well with those obtained by standard methods.     

电感耦合等离子体发射光谱法测定稀土发火合金中铁、镁、铜和锌

采用盐酸辅以加热的方式处理稀土发火合金样品,以电感耦合等离子体原子发射光谱法测定稀土发火合金中铁、镁、铜和锌含量。采用矩阵模拟实验优化分析谱线,利用多点定标校正曲线法计算测量结果。在最佳实验条件下,稀土发火合金中的基体元素对待测元素的测定结果无明显影响,各元素在检测范围内线性关系良好,相关系数均为0.999 9,方法检出限为0.001~0.010μg/m L。测定结果的相对标准偏差为1.10%~1.75%(n=11),样品加标回收率在96.00%~104.05%之间。该方法简便、快速且具有较高的灵敏度,适用于稀土发火合金中铁、镁、铜、锌等非稀土元素的测定。     

Direct determination of trace elements in tungsten products using an inductively coupled plasma optical emission charge coupled device detector spectrometer

An echelle inductively coupled plasma optical emission spectrometer equipped with a segmented array of charge coupled device detectors was used for the direct determination of trace impurities in tungsten products. No sample preparation was necessary. The multicomponent spectral fitting software provided by the instrument was used for the correction of spectral interference and background. The detection limits of the trace elements Al, As, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, P, Pb, Sb, Sn, Ti and V in tungsten matrix were obtained under optimized operating conditions. The accuracy of the proposed method was assessed using three National Reference Materials. As a result of their ultra-trace concentrations in the reference materials, As, Pb and Sn could not be determined satisfactorily. The concentrations found for the other elements agreed quite well with those of the certified values of the reference materials.     

电感耦合等离子体原子发射光谱法高纯三甲基镓中的痕量杂质

对电感耦合等离子体原子发射光谱（ＩＣＰ－ＡＥＳ）法测定高纯三甲基镓（９９．９９９９Ｔ,相对于金属镓的含量）中Ｃu、Ｆe、Ｓi、Ｚn等３１种痕量杂质元素的含量进行了研究,考察了基体元素镓对杂质元素的光谱和非光谱干扰以及基体浓度对杂质元素谱线信噪比和检出限的影响在优化的实验条件下,获得了满意的结果。     

Determination of Manganese in Sludge,Alloy, and Soil by Tungsten Coil Atomic Emission Spectrometry

A tungsten coil atomic emission spectrometer (WCAES) was developed and evaluated for the determination of manganese in industrial sludge, alloy, and soil. The system employed a coil extracted from a 150 watts/15 volts commercial slide projector light bulb and a simple power supply that provided a constant current to the coil. The analytical signals were resolved and detected using a Czerny-Turner spectrometer and a charge coupled device. Three manganese emission lines were detected simultaneously. Using different emission lines, limits of detection for manganese varied from 0.54 to 0.65 milligram per liter, and relative standard deviations for manganese at 5 milligrams per liter varied from 5.9 to 8.5 percent (n = 10). Summation of the Mn signals improved the detection limit to 0.17 milligram per liter and decreased the relative standard deviation to 1.7 percent. Spectral interferences were observed in the presence of Al, Ca, K, and Na. The accuracy was determined using two certified reference materials, and the results obtained by WCAES were in agreement with those obtained by inductively coupled plasma-optical emission spectrometry at the 95 percent confidence level.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定硫化物矿石中的铜铅锌

建立了电感耦合等离子体原子发射光谱(ICP-AES)法同时测定硫化物矿石中Cu、Pb、Zn三种元素的方法,取代了传统的四酸(HCl+HNO3+HClO4+HF)溶样法,采用简单的盐酸和硝酸溶解矿石,大大缩短了分析时间。选择干扰少且灵敏度高的谱线作为待测元素的分析谱线,采用左右两点扣背景的方法校正光谱干扰和基体匹配方法消除物理干扰,用GBW07162和GBW07163等不同种类的国家一级标准物质进行精密度和准确度实验,测定结果的相对标准偏差都在10%以内,测定结果都在标准值的误差范围内,符合地质矿产开发的要求。     

电感耦合等离子体原子发射光谱法同时测定高强度玻璃纤维粉体中9种金属元素

建立电感耦合等离子体原子发射光谱法测定高强度玻璃纤维粉体中铝、镁、钙、铁、钛、锂、铈、钠、钾9种金属元素含量的方法。采用氢氟酸、高氯酸和盐酸分两段溶解样品,分别在选定的各元素分析谱线下,采用电感耦合等离子体原子发射光谱仪测定各元素含量。9种金属元素在各自的质量浓度范围内与光谱强度成良好的线性关系,相关系数均大于0.999,检出限为8.0~17.4 μg/g。测定结果的相对标准偏差小于1.8%(n=6),加标回收率为97.6%~103.7%。该方法准确,简便,快速,适用于高强度玻璃纤维中多金属元素的同时测定。     

微波消解-ICP-AES法测定钴基合金中的硼

采用微波消解-ICP-AES法测定钴基合金中硼元素。通过试验探讨了钴基高温合金中基体元素,主量元素如铬、钨、钼等对硼元素分析谱线的光谱干扰情况,采用基体匹配法对基体干扰进行校正,确定了合适的分析谱线。方法的线性范围为0～8 mg/L,检出限为0.0003%。测定结果的相对标准偏差为1.88%～6.04%(n=6),回收率为92.0%～104.2%。     

Simultaneous determination of Cr,Ga, In and V in soil and water samples by tungsten coil atomic emission spectrometry

Tungsten coil atomic emission spectrometry is employed for the simultaneous determination of Cr, Ga, In, and V. Both V and In are detected by this technique for the first time. The atomizer is a simple, inexpensive tungsten filament extracted from a mass-produced, commercially-available 150 W, 15 V microscope bulb. A 25 µl sample aliquot is placed directly on the coil and a small constant-current power source is used to carefully dry, ash and atomize the sample. Analytical signals are detected with a Czerny-Turner spectrograph and a charge coupled device detector. Multiple emission lines from all 4 elements are monitored simultaneously in a 54 nm spectral window. Concentration limits of detection are in the µg l^− 1 range for all elements, and the absolute limits of detection are 0.2, 2, 0.5, and 10 ng for Cr, Ga, In, and V, respectively. Even lower values may be obtained by combining the signals for the multiple emission lines of a single element. The method precision is typically better than 5.0% relative standard deviation, and sometimes as good as 0.95% (Ga). Standard reference materials of soil and water are used to check the method accuracy. After a simple acid extraction, the values determined by the method presented no significant difference from the reported values at the 95% confidence level.     

电感耦合等离子体原子发射光谱法(ICP-AES)测定粗铅中的Cu，As，Sb，Bi 4种元素

建立了电感耦合等离子体原子发射光谱法（ICP-AES）测定粗铅中Cu,As,Sb,Bi 4种元素的定量分析方法。通过实验选择327.395,193.696,187.052,223.061nm分别作为Cu,As,Sb,Bi的分析谱线,方法的检出限均小于0.010μg/mL。方法的回收率在96%~104%,精密度实验结果表明,相对标准偏差（RSD,n=6）均小于3%,能满足日常分析对粗铅中杂质元素的快速检测要求。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定5XXX系铝合金中的高镁含量

采用电感耦合等离子体原子发射光谱法测定5XXX系铝合金中的高镁含量,选择20mL稀王水溶液溶解试样,以消除合金中的基体元素及其它共存元素的干扰为目标,选择测定镁含量的分析谱线为280.270nm。分别称取与分析试样基体近似的三种铝合金标准物质0.100 0g,按试样相同的溶解方法处理并定容至100mL,选择仪器工作条件,制作分析曲线,进行曲线校准,按照同样的方法对4个样品各测定6次,测定值的相对标准偏差均不大于0.59%,用标准加入法测得加标回收率在94.0%~104.0%,测定值和环己二胺四乙酸分离络合滴定法测定的5XXX系铝合金中的镁量结果一致。     

ICP-AES法测定稀土磁性材料中微量铬、镍和钛

研究了采用电感耦合等离子体原子发射光谱(ICP-AES)测定稀土磁性材料中微量铬、镍和钛的分析方法。确定了样品的溶解方法和待测元素的分析线,对基体元素和共存元素的干扰影响进行了考察,采用基体匹配法克服了基体效应。该方法测定结果与火焰原子吸收光谱法测定结果相一致。铬、镍、钛的检出限分别为0.001 4、0.002 8、0.000 5μg/mL,测定结果的相对标准偏差小于7.0%(n=8),方法的加标回收率为97.0%~104.7%。     

电感耦合等离子体原子发射光谱法测定钛合金中钨、铌、钽

采用电感耦合等离子体原子发射光谱法（ICP-AES）法测定钛合金中W,Nb,Ta元素的含量。样品采用盐酸、氢氟酸和硝酸溶解,并对仪器工作参数和试验条件进行了优化试验,确定了仪器最佳工作条件,考察了钛合金基体和共存元素对待测元素的影响,确定了各待测元素谱线为W207．911nm,Nb309．418nm,Ta240．063nm。选定的待测元素分析线不受合金基体和共存元素的干扰,通过基体匹配消除基体的影响。加标回收率在98％104％之间,测定结果的相对标准偏差为0．3％～2．4％（n=8）,方法的检出限为0．003-0．013μg／mL。进行了标准物质对照试验,试验结果与标准值相符。     

Developing electrodeposition techniques for preconcentration of ultra-traces of Ni, Cr and Pb prior to arc-atomic emission spectrometry determination

Electrodeposition is known to be proper for separation and preconcentration of extremely low concentrations of analytes from the bulk sample which is instrumentally very simple. In the present research, a combination of electrodeposition with arc atomic emission spectrometry (ED-AAES) method has been developed in order to improve the analytical performance of this spectrometry technique. The results show that sensitivity and detection limits by using ED-AAES were improved 1000–2000 folds over those of normal arc atomic emission spectrometry in determination of the selected elements. The detection limits for measurement of Ni, Cr and Pb were 2.56, 3.05 and 2.11 µg L^{− 1} for monodeposition and 3.31, 3.72 and 3.25 µg L^{− 1} for simultaneously deposition, respectively. The precision of determination was in the range of 2–4% RSD. Typical calibration graphs for these elements were linear up to 100 µg L^{− 1}, depending on the element and matrix.Application of this technique was also tested on determination of the studied elements in an electroplating plant's waste water. The accuracy of technique was verified by comparing the results of the waste water analysis with those of electrothermal atomic absorption spectroscopy as a reference standard method.The obtained results show that the combined technique (ED-AAES) has been progressed substantially toward the ultimate goal of direct interference-free determination of trace analysis in complex samples by AAES.     

Spectral interferences in the determination of traces of scandium, yttrium and rare earth elements in “pure” rare earth matrices by inductively coupled plasma atomic emission spectrometry: Part VII — Terbium, Dysprosium, Holmium and Thulium

This article is the seventh part of a series of papers discussing the spectral interferences of rare earth elements (REEs) in ICP-AES. Radial viewing 27.12 MHz inductively coupled plasma atomic emission spectrometry (ICP-AES) was used in the determination of scandium, yttrium and rare earth elements in Tb₂O₃, Dy₂O₃, Ho₂O₃ and Tm₂O₃ as “pure” rare earth matrices. The quantification of the interferences in terms of Q-values for line interference Q_I(_a) and wing background interference Q_W(Δλ_a) were used in accordance with Boumans and Vrakking [Spectrochim. Acta Part B 43 (1988) 69]. The “best” analysis lines from point of view of spectral interferences were selected. The true detection limits by using the “best” analysis lines were calculated.     

ICP–AES法测定锑铍芯块中铅、铁、锰和镁

建立电感耦合等离子体原子发射光谱(ICP–AES)测定锑铍芯块中铅、铁、锰和镁杂质元素的方法。对溶液酸度的选择、光谱和基体干扰等进行了试验和讨论,在优化仪器工作参数的条件下,通过基体匹配,有效消除了基体干扰的影响。铅、铁、锰、镁的质量浓度在0.05~10.0μg/mL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0.999。铅、铁、锰、镁的检出限在0.5~5.3μg/L之间,测定结果的相对标准偏差为0.9%~2.9%(n=7),加标回收率为92%~106%。电感耦合等离子体原子发射光谱法与原子吸收光谱法对照,测定结果相符合。该方法准确可靠,可用于锑铍芯块中铅、铁、锰和镁杂质元素的测定。     

Evaluation of tungsten coil electrothermal vaporization-Ar/H2 flame atomic fluorescence spectrometry for determination of eight traditional hydride-forming elements and cadmium without chemical vapor generation

A tungsten coil electrothermal vaporizer (W-coil ETV) was coupled to an Ar/H(2) flame atomic fluorescence spectrometer for the determination of eight traditional hydride-forming elements (i.e., As, Bi, Ge, Pb, Sb, Se, Sn, and Te) as well as cadmium without chemical vapor generation. A small sample volume, typically 20muL, was manually pipetted onto the W-coil and followed by a fixed electric heating program. During the vaporization step, analyte was vaporized off the coil surface and swept into the quartz tube atomizer of AFS for further atomization and excitation of atomic fluorescence by a flow of Ar/H(2) gas, which was ignited to produce the Ar/H(2) flame. The tungsten coil electrothermal vaporizer and Ar/H(2) flame formed a tandem atomizer to produce reliable atomic fluorescence signals. Under the optimal instrumental conditions, limits of detection (LODs) were found to be better than those by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma optical emission spectrometry (ICP-OES) for all the nine elements investigated. The absolute LODs are better or equivalent to those by hydride generation atomic fluorescence spectrometry (HG-AFS). Possible scattering interferences were studied and preliminary application of the proposed method was also reported.