X射线荧光光谱法测定钒钛磁铁矿中的主次量元素

采用X射线荧光光谱法测定钒钛磁铁矿中铁、钛、硅、铝、锰、钒、钙、镁等8种主次量元素。样品以四硼酸锂、偏硼酸锂和氟化锂(质量比为4.5比1比0.4)为熔剂,脱模所得熔块用于X射线荧光光谱分析。以GBW 07224、GBW 07225、GBW 07227、YSBC 19701-76、GSB 03-2584-2010、YSBC 19722-2011等6种标准物质和光谱纯二氧化硅、氧化钙、氧化铝、五氧化二钒、二氧化钛为基础制作校准曲线。优化了各元素的基体校正数学模型。各元素的检出限在3.79~39.06mg·kg-1之间。对钒钛磁铁矿标准样品GBW 07225重复测定10次,测得其相对标准偏差(n=10)在0.83%~2.9%之间。方法用于钒钛磁铁矿标准样品GBW 07225,GBW 07227的分析,所得结果与认定值相符。     

ICP-AES法高精度测定钕铁硼合金中主量元素

电感耦合等离子体原子发射光谱(ICP-AES)法测定钕铁硼合金主量元素波动大,相对标准偏差通常高达0.5%以上,严重影响不同牌号钕铁硼磁体的成分配比与性能控制。为了解决这一难题,本文研究了电感耦合等离子体原子发射光谱法同时高精度测定钕铁硼合金中Nd,Fe,B三种主量元素,选择了合适的分析线并扣除了背景。通过采用基体匹配、优化仪器参数、保持稳定的ICP焰炬、校正谱峰漂移(采用软件的校正功能,对各元素进行漂移校正,校正完成后,对原测试数据进行再处理)等,实现了对钕铁硼主量元素的高精密度测试。结果表明:Nd,Fe,B三种元素的短期相对标准偏差分别为:0.09%,0.04%,0.31%,加标回收率为97%~103%;5天内的长期相对标准偏差为:0.17%,0.08%,0.52%;测试同一合成样品,ICP测定值与X射线荧光光谱法测定值相对偏差小于1%,与国外实验室ICP法的测定值相对偏差小于0.1%,测定值与X射线荧光光谱法和国外实验室ICP法的测定值对照结果满足生产、科研的测定要求。     

X射线荧光光谱法分析玻璃纤维中主、次量元素成分

采用粉末压片-波长色散X射线荧光光谱法分析了中碱及无碱玻璃纤维中硅、铝、钙、镁、铁、钛、钾、钠、砷、氟等10种主、次量元素成分含量。以6个标准样品并结合两个参考样品建立校准曲线,采用DeJongh模式方程有效校正玻璃基体中元素间的吸收增强效应和重叠效应。该方法测定10个元素的精密度和准确度均较好,其相对标准偏差在0．35％～2．86％之间,对实际样品的分析结果与化学法相吻合,可应用于玻璃纤维中多元素成分的快速分析。     

铝青铜合金样品的X射线荧光光谱分析

建立了X 射线光谱测定铝青铜系列铜合金中Al、Mn、Fe、Si、Ni、Zn、Sn和Pb 8种元素的方法,探讨电流、电压对荧光强度的影响,基体效应校正采用基本参数法.用该方法对实际样品进行分析,分析结果与化学法分析结果相吻合.各元素测定结果的相对标准偏差为0.10%-5.56%(n=10).     

X射线荧光光谱法测定石油焦中主量元素硫和痕量元素的含量

提出了粉末压片制样-X射线荧光光谱法测定石油焦样品中硫、钠、镁、铝、硅、磷、氯、钾、钙、钡、钛、钒、铬、锰、铁、镍、铜和锌等18种元素含量的方法。将粒径小于0.076mm的石油焦粉末经105℃烘干后置于模具中,以160MPa压力制成厚度小于4mm的样品。以经验系数法和康普顿散射线内标法校正基体效应和元素间的谱线重叠干扰。对石油焦样品连续11次测定,各元素测定值的相对标准偏差均小于8%。方法用于标准样品的分析,测定结果与认定值相符。     

X射线荧光光谱法测定石膏中11种元素的含量

采用X射线荧光光谱法测定石膏中钠、镁、铝、硅、硫、钾、钙、钛、锰、铁、锶等11种元素的含量。样品研磨30s后压片,样片用于X射线荧光光谱分析。以GBW 03109、GBW 03110、GBW 03111、GBW 03109a、GBW 03111a、GSB 08-1352-2001、GSB 08-1352-2006、GSB 08-1352-2009等8种标准物质为基础制作校准曲线,优化了各元素的基体校正数学模型。各元素的检出限在0.001 4%~0.27%之间。对同一石膏样品平行测定10次,其相对标准偏差(n=10)在0.51%~4.0%之间。方法用于3个石膏样品的分析,所得结果与国家标准方法测定结果相符。     

X射线荧光光谱法测定白云石中12种元素的含量

采用X射线荧光光谱法测定白云石中钠、镁、铝、硅、磷、硫、钾、钙、锰、铁、钛、锌等12种元素的含量。样品以四硼酸锂和偏硼酸锂为熔剂和溴化锂为脱模剂于1 050℃熔融,样片用于X射线荧光光谱分析。以GBW 07114、GBW 07216A、GBW 07217A、YSBC 11703-1995、YSBC28722-1993、YSBC 28723-1993等标准物质为基础制作工作曲线。优化了各元素的基体校正数学模型。对白云石样品重复测定11次,测得其相对标准偏差(n=11)在0.2%~7.3%之间。方法用于白云石标准样品的分析,所得结果与认定值相符。     

自动元素分析仪测定碳纤维中氮、碳、氢

利用Vario ELⅢ型元素分析仪测定了碳纤维中氮、碳和氢的含量。优化的试验条件为:称样量2.1～2.4 mg,加氧时间120 s,燃烧管温度980℃。选用乙酰苯胺计算当天校正因子,方法用于碳纤维和石墨样品分析,含碳量在88.05%～99.46%之间,而在绝大多数样品中氮和氢的质量分数都小于0.30%。     

电感耦合等离子体质谱法测定海洋沉积物中34种痕量元素

用电感耦合等离子体质谱法测定海洋沉积物中34种痕量元素,样品于聚四氟乙烯封闭坩埚中用氢氟酸和硝酸溶解,运用干扰方程校正光谱干扰,用内标校正消除基体影响。方法检出限(3s/k)在0.046～160 ng.g-1之间。通过分析4个海洋沉积物标准物质对所提出方法的准确度和精密度做了考核,所得测定结果与标准物质的认定值相吻合,各元素测定结果的相对标准偏差均小于10%。     

混酸消解-电感耦合等离子体质谱法（ICP-MS） 同时测定土壤样品中10种重金属元素

建立了盐酸、硝酸、氢氟酸、高氯酸四酸消解-电感耦合等离子体质谱体系,对土壤环境样品中的铜、铅、锌、镍、镉、铬、钴、铊、锰、锑等重金属的测定进行了研究与讨论。优化了样品前处理条件和电感耦合等离子体质谱仪的相关参数,并利用内标元素45Sc、103Rh、209Bi校正土壤基体效应干扰。实验结果表明,各元素标准曲线的相关系数R均在0.9996之上,方法检出限（3σ）在0.007-0.325ug/g之间,加标回收率为92.5%-108.2%,相对标准偏差为0.2%-4.2%。研究过程中选用国家一级土壤成分分析标准物质进行质量控制,其测定值与标准值基本相符,从而为土壤中重金属元素提供了真实有效的检测依据,可用于大批量土壤中重金属元素的测定。     

电感耦合等离子体原子发射光谱法测定四氯化钛液体中杂质元素

提出了电感耦合等离子体原子发射光谱法测定四氯化钛液体中硅、铝、钒、铬、铜、铁等微量元素含量的方法。对方法的测定条件及相关参数进行了优化;用在样品本身中加入上述各元素的混合或单独标准溶液的方法,标准加入法消除基体效应的影响,选择适宜待测元素的分析谱线以消除光谱干扰。方法的检出限(3s)在0.001~0.015 mg.L-1之间。     

电感耦合等离子体原子发射光谱法测定镍基单晶高温合金中Mo、W、Ta、Re、Ru时元素之间相互干扰的消除与校正的研究

称取镍基单晶高温合金0.100 0g于聚四氟乙烯烧杯中,先令其与盐酸9mL和硝酸1mL加热反应,待反应缓慢时滴加氢氟酸2mL并继续加热使样品完全溶解。加入500g·L^-1酒石酸溶液2mL,冷却至室温,在塑料容量瓶中加水定容至100.0mL。按仪器工作条件采用电感耦合等离子体原子发射光谱法测定其中5种合金元素(Mo、W、Ta、Re、Ru)的含量,选择分析谱线依次为204.598,207.911,240.063,197.312,240.272nm。结果发现:除了Re外,其余4种元素的测定中均受共存元素的光谱干扰,严重影响了测定结果的准确性。为克服其干扰,除了采用基体匹配法消除镍的基体干扰外,试验采用混合校正系数矩阵法对测定结果进行校准。通过一系列试验计算得到混合校准系数矩阵K,并应用于模拟样品的分析。结果表明:经过矩阵K的校准,所测定的5种元素的准确度显著提高,达到了消除共存元素之间光谱干扰的目的。通过精密度试验,测得上述5种元素测定值的相对标准偏差(n=11)均在1.5%以下,并通过标准加入法进行回收试验,测得5种元素的回收率为97.0%~105%。     

电感耦合等离子体原子发射光谱分析中易电离元素的基体干扰及其抑制的研究

选取铝、铜、镁、钙、铁、锰和锌等7种元素的9条谱线,研究电感耦合等离子体原子发射光谱法对其测定时易电离元素钾、钠的基体干扰。结果表明:易电离元素对待测元素具有较明显的干扰作用,而增大射频发射功率及降低雾化器压力可有效地抑制易电离元素对待测元素的干扰。     

Determination of platinum and rhodium in dust and plant samples using microwave-assisted sample digestion and ICP-MS

The platinum group elements (PGEs), particularly platinum, palladium and rhodium, are nowadays increasingly emitted into the environment from automotive catalytic converters. Thus, a method for the determination of PGEs (especially platinum and rhodium) in dust and plant samples was developed. The developed method was based on microwave-assisted sample digestion and inductively coupled plasma mass spectrometric (ICP-MS) determination. Spectral interferences in ICP-MS determination were corrected using mathematical correction equations based on signal ratio measurement. In addition, platinum and rhodium concentrations in the digested dust samples were also determined after Te coprecipitation without correction of the interferences. The results for platinum and rhodium in reference materials (NIST SRM 2557, recycled monolith autocatalyst and BCR-723, road dust) were in good agreement with the certified values. Preliminary results for the anthropogenic platinum and rhodium emissions in Oulu, northern Finland, based on dust and plant samples, indicated a common traffic-related source of these metals.     

Determination of trace elements in residual oil by high-resolution inductively coupled plasma mass spectrometry

An analytical method using high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 20 elements, including Na, Mg, Al, Ca, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Mo, Cd, Sn, Sb, Ba, and Pb elements, in residual oil was described. The sample was dissolved in HNO₃ by microwave digestion, and then the above 20 elements in the solution were analyzed directly by HR-ICP-MS. Most of the spectral interferences could be avoided by measuring in the high-resolution mode. The matrix effect caused by the sample-digesting solution and corrected by Sc, Rh, and Bi as the internal standard elements was studied in detail. The optimum condition of the determination was also tested and discussed. The result showed that the detection limits of the method were in the range of 0.014 to 11.6 μg L⁻¹; the relative standard deviation was less than 3.8% and recoveries in the samples were in the range of 88.4% to 108.0%. This method can be used to determine the trace elements in residual oil with the features of accurate, rapid, and convenient determination.     

Uncertainty propagation through correction methodology for the determination of rare earth elements by quadrupole based inductively coupled plasma mass spectrometry

Determination of rare earth elements by quadrupole based inductively coupled plasma mass spectrometry (ICP-QMS) shows several spectroscopic overlaps from M⁺, MO⁺ and MOH⁺ ions. Especially, the spectroscopic interferences are observed from the atomic and molecular species of lighter rare earth elements including Ba during the determination of Eu, Gd and Tb. Mathematical correction methods, knowing the at.% abundances of different interfering isotopes, and the extent of formation of molecular species determined experimentally, have been used to account for various spectroscopic interferences. However, the uncertainty propagated through the mathematical correction limits its applicability. The uncertainty propagation increases with the increase in contribution from interfering species. However, for the same extent of total contribution, the overall error decreases when the interfering species are more than one. In this work, chondrite as well as a few geological reference materials containing different proportions of various rare earth elements have been used to study the contributions of different interfering species and the corresponding uncertainty in determining the concentrations of rare earth elements. A number of high abundant isotopes are proposed for determining the concentrations of various rare earth elements. The proposed isotopes are tested experimentally for determining the concentrations of different rare earth elements in two USGS reference materials AGV-1 and G-2. The interferences over those isotopes are corrected mathematically and the uncertainties propagated due to correction methodology are determined for those isotopes. The uncertainties in the determined concentrations of rare earth elements due to interference correction using the proposed isotopes are found to be comparable with those obtained by the commonly used isotopes for various rare earth elements.     

Non-linear spectral interferences in an inductively coupled plasma optimized for simultaneous multi-element analysis of plant and soil samples by atomic emission spectrometry

Summary The spectral interferences by Al, Ca, Fe, K, Mg and Na in the direct simultaneous determination of As, Cd, Co, Cu, Hg, Pb and Se in plant and soil samples by ICP-AES are investigated, and a non-linear relationship between the apparent analyte concentration for As, Cd, Co, Hg and Se is observed. A correction method for non-linear spectral interferences is discussed and non-linear spectral correction coefficients are calculated.     

电感耦合等离子体质谱法测定稀土元素的状况与展望

本文综述了电感耦合等离子体质谱法测定稀土元素的技术状况，包括谱干扰、非谱干扰及其克服方法，激光烧蚀、电热蒸发、超声雾化等进样方法和联测技术、发展趋势、引用参考文献７７篇。     

Instrumental neutron activation analysis in geochemistry: Emphasis on spectral and uranium fission product interferences

Summary The accuracy of the analytical results may suffer from unsolved interferences both spectral or due to U fission products despite progress performed in electronics and informatics in instrumental neutron activation analysis. This contribution deals with the correction of spectral and U fission product interferences using a multicomponent method based on the resolution of simultaneous equation method and using the Erdtmann isotope-related k_I-factors for the determination of the correction factors of interferences due to U fission products, respectively. These resolution methods were tested on typical phosphate and uraniferous ore samples.