电感耦合等离子体发射光谱法测定植物油中的磷

用电感耦合等离子体发射光谱法(ICP-AES)测定了植物油中的磷.采用多谱线拟合技术(MSF)校正了铜对P213.617 nm和P214.914 nm光谱干扰.比较了活性炭炭化灰化法和微波消解法两种样品前处理方法对分析结果的影响.结果表明这两种前处理方法所得结果都能与国标磷钼蓝分光光度法的分析结果吻合,其中活性炭炭化灰化法的方法检出限(0.053 mg/kg)较微波消解法的方法检出限(0.42 mg/kg)更低,所以对低含量的磷的检测结果其相对误差及精密度更好.该法应用于植物油中磷的测定.     

用高分辨率电感耦合等离子体-原子发射光谱仪测定高纯铬中的杂质元素

本文报道了高分辨率、高灵敏度的顺序扫描型电感耦合等离子体原子发射光谱仪(ICPS-8100)在高纯物质分析中的应用。对元素分析线进行优化选择;采用轴向观测方式,对高纯铬中μg/g级的杂质元素As、Sn、Sb、Pb进行直接同时测定,分析结果令人满意。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定锌-铝-镉牺牲阳极中多种元素含量

利用稀王水溶解试样,建立了电感耦合等离子体原子发射光谱法测定锌-铝-镉牺牲阳极中铝、镉、铁、铅、铜和硅6种元素的分析方法。各元素的精密度均小于5%,检出限及回收率分别在0.0012%～0.016%和94.6%～105%。对实际样品进行分析,检测结果与其它实验室结果一致。     

电感耦合等离子体发射光谱法测定磷酸中的金属元素

建立了一种用电感耦合等离子体发射光谱仪(ICP-AES)测定磷酸中金属元素的分析方法。实验结果表明：选择合适的样品前处理方式和优化的仪器操作条件,方法的检出限可达到0.0012 ug/g~0.0552ug/g、加标回收率达到95%~105%,满足实际样品分析要求。     

Solid phase extraction of trace Hg(II) on silica gel modified with 2-(2-oxoethyl)hydrazine carbothioamide and determination by ICP-AES

In this work, a new 2-(2-oxoethyl)hydrazine carbothioamide modified silica gel (SG-OHC) sorbent was prepared and applied for preconcentration of trace mercury(II) prior to the measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimization of some analytical parameters affecting the adsorption of the analyte such as acidity, shaking time, sample flow rate and volume, eluent condition, and interfering substances were investigated. At pH 3, the maximum static adsorption capacity of Hg(II) onto the SG-OHC was 37.5 mg g⁻¹. The quantitative recovery (>95%) of Hg(II) could be obtained using 2 mL of 0.5 mol L⁻¹ HCl and 1% CS(NH₂)₂ solution as eluent. Common coexisting substances did not interfere with the separation of mercury(II) under optimal conditions. The detection limit of present method was 0.10 ng mL⁻¹, and the relative standard deviation (RSD) was lower than 4.0% (n = 8). The prepared sorbent was successfully applied for the preconcentration of trace Hg(II) in certified and water samples with satisfactory results.     

Application of sequential extraction and the ICP-AES method for study of the partitioning of metals in fly ashes

In this work, the original BCR extraction scheme was modified and applied to study the partitioning of metals in fly ashes. In the first step, the water-soluble fraction was investigated here. The next metal fractions were acid-soluble, reducible, and oxidisable. Two kinds of coal fly ash certified reference materials were analysed. Metal concentrations in the extracts were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). The efficiency of the extraction process for each step was examined. The partitioning of metals between the individual fractions was investigated and is discussed.     

Hair analysis and the early detection of imbalances in trace elements for members of expeditions in Antarctica

In the framework of the Human Biology and Medicine Project of the National Program for Research in Antarctica (Programma Nazionale di Ricerche in Antartide, PNRA) a study was undertaken to explore the suitability of trace element determination in human hair as a tool for the early detection of the impact of extreme environmental conditions on the health of members of the Italian and French expeditions. This study included three campaigns, namely, the 1995–1996 expedition to the Italian base of Terra Nova Bay, as well as the 1997–1998 and 1998–1999 expeditions to both the Italian base of Terra Nova Bay and the Italian–French base of Dome C. Sampling of hair of participants in the expeditions was carried out both prior to departure and at the end of the period spent at the bases. As regards storage, pre-treatment and analysis of hair samples they were performed in accordance with previously established procedures. Acid-assisted microwave digestion was adopted as the best approach for preparing solutions for subsequent analysis by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry. In the first part of this study, only the elements Ca, Cu, Fe, Mg and Zn were selected, while at a later stage it was decided to also include Co, Cr, Mn, Mo and Ni. Experimental results were subjected to basic statistical analysis to detect possible significant differences in element concentrations that occurred during the sojourn at the bases, with a view to identify possible remedial action to minimize adverse consequences.     

Determination of Y,Sm, Eu,Gd, Dy,Ho, Er in high purity terbium oxide by ICP-AES

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was employed to determine Y, Sm, Eu, Gd, Dy, Ho and Er in high purity terbium oxide. Terbium oxide was dissolved in 0.5 mol/l HNO₃ and nebulized into the plasma generated by a 56 MHz RF generator at 1.5 kW output power. Using a Jobin-Yvon 1-m Czenry-Turner high resolution, high dispersion scanning monochromator, lines mutually interference-free as well as free of interference from the matrix Tb were chosen for the seven analytes. A set of standards containing the analytes in the concentration range 0.01–1.0 gmg/ml with 1 mg/ml Tb was used for calibration. It was necessary to apply background correction to the gross analyte line intensities in order to obtain linear calibration plots for the analytes.     

ICP-AES 法测定硅铁中痕量元素

采用电感耦合等离子原子发射光谱法测定硅铁中的痕量元素,研究了 Fe 基体对被测元素的影响,并选择了最佳工作条件.被测元素的检测限为 0 .60～76.2 ng/mL,样品加标回收率为 92%～108%,RSD(n=8)<3%.     

电感耦合等离子体原子发射光谱(ICP-AES)法与EDTA滴定法联用测定含白云岩矿石中氟化钙

氟化钙的测定目前较多采用的是GB/T5195.1-2017和DZG93-05两种方法,前者测定范围≥60%,后者测定范围>3%。两种方法各有优缺点,然而却都无法满足矿石中含有白云岩时的测定。近年来,青海省地勘局大力探寻萤石矿,各矿区矿石组成、矿床类型各不相同,且氟化钙品位高低不一,尤其是青海省海西州喀雅克登矿区中常见萤石矿与白云岩共存,直接采用国家标准方法,测定结果偏高,行业标准方法的精密度和准确度也很难达到要求。本文对方法进行优化,准确称量样品0.2000g至50mL的锥形瓶中,加入10mL含钙冰乙酸(1+9),瓶口放置φ40mm的短颈漏斗,在控温电热板上100℃加热40min,取下过滤,残渣放回原锥形瓶,加入20mL混合酸,瓶口放置漏斗,于控温电热板上150℃微沸30min,将溶液转移至100mL比色管中,摇匀,澄清。在Ca 317.933 nm处,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定氟化钙。根据ICP-AES的测定结果,将氟化钙质量分数大于15%的样品用EDTA滴定法再次测定。按照实验方法测定喀雅克登矿区实际样品,两种方法测定结果的相对标准偏差(RSD,n=11)分别为1.86%和0.77%,加标回收率为97.9%～102.2%,可满足含白云岩矿石中氟化钙的准确测定。     

Determination of Titanium in Nano-Titanium(IV) Oxide Composite Food Packaging by Microwave Digestion and Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry

Titanium was determined in nano-titanium(IV) oxide food packaging by microwave digestion with inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Microwave digestion was optimized using different acid combinations. Both spectrometry techniques showed good reproducibility, repeatability, and recovery. For ICP-AES, the limit of detection was 5.0 mg kg^?1, the linear dynamic range was 100–5000 µ g L^?1, the average recoveries for blank samples spiked with titanium were between 94.7% and 100.1%, and the relative standard deviations were from 2.1% to 7.1%. By ICP-MS, the limit of detection was 0.3 mg kg^?1, the linear dynamic range was 0.5–200 µ g L^?1, the recoveries were 88.4%–96.3%, and the relative standard deviations were 6.3%–7.4%. These results indicated that methods were effective for the determination of titanium in food packaging.     

微波消解-全谱直读等离子体发射光谱法测定面包改良剂中总溴的研究

采用微波消解样品、全谱直读等离子体发射光谱法(ICP—AES)测定面包改良剂中的溴含量。通过试验,优化了微波消解的条件和仪器的最佳工作参数：154．065nm波长处溴的检出限为0．015mg／L(3δ),线性范围为0．05～100mg／L,样品分析结果的相对标准偏差小于5％(n=7),加标回收率在93％～105％之间,样品分析结果与分光光度法相一致．该法简便、快速、灵敏、准确、线性范围宽。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定四种奶片中的钙和镁

采用HNO3-HClO4混酸体系溶解奶片,电感耦合等离子体原子发射光谱法测定试样中的钙和镁含量,结果表明非糖果型奶片中钙和镁的含量较高。通过加标回收实验,钙和镁的加标回收率为96.72%~101.40%,相对标准偏差均小于3%,该方法准确、快捷,为研究奶片在儿童成长发育中的作用提供了相关的依据。     

Indirect determination of fluoride in aqueous samples by inductively coupled plasma atomic emission spectrometry following precipitation of CeF3

An indirect fluoride determination method has been developed based on the ICP-AES determination of excess cerium(III) ion after precipitation. From four cations—Y(III), Sr(II), Ce(III), La(III)-cerium(III) proved to be the best precipitate forming cation in the 0-20 mg L⁻¹ fluoride concentration range with the limit of detection of 1.4 mg L⁻¹. The precision (RSD) of the proposed method is 0.71% at 8 mg L⁻¹ fluoride. The role of sulphate ions in the formation of the fluoride precipitate was studied as well. The applicability of the technique for the study of solid hazardous wastes as well as for groundwater monitoring of a fluoride contaminated area is demonstrated.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定四种奶片中的钙和镁

采用HNO3-HClO4混酸体系溶解奶片,电感耦合等离子体原子发射光谱法测定试样中的钙和镁含量,结果表明非糖果型奶片中钙和镁的含量较高。通过加标回收实验,钙和镁的加标回收率为96.7%～101%,相对标准偏差均小于3%,方法准确、快捷,为研究奶片在儿童成长发育中的作用提供了相关的依据。     

萃取-非水介质氢化物发生-ICP-AES中的干扰及Ni-Fe基合金的分析

本文结合溶剂萃取研究了非水介质中氢化物发生-ICP-AES的分析条件、干扰等因素的影响。利用KI~+H_2SO_4/MIBK萃取体系将As,Sb,Bi萃取到MIBK中而与基体元素分离,然后将该有机相与甲酸按等体积混合后,即可直接进行氢化物发生-ICP-AES分析。还对影响萃取和氢化物发生的一些因素及共存元素的干扰进行了讨论。该方法应用于Ni-Fe基合金中As和Sb的分析,取得了较满意的结果。     

电感耦合等离子体原子发射光谱法（ICP-AES）测定RoHS指令聚合物中的铅和镉

本文引入微波技术消解聚合物塑料样品,使用电感耦合等离子体原子发射光谱仪（ICP-AES）测定聚合物中的铅（Pb）和镉（Cd）含量,并建立了优化的样品消解程序和测定方法,得到满意的测定结果。[摘要应包括目的、方法、结果、结论,请修改,同时修改英文]该方法具有效率高、污染小的优点。检测结果具有良好的精密度。     

ICP-AES中乙醇作用机理的定量研究Ⅰ.乙醇干扰函数和各种干扰因素的相对贡献

本文应用Einstein-Boltzmann-Saha方程和Raoult-Clausius-Clapeyron方程,定量地考察了乙醇对电感耦合等离子体(ICP)中各种干扰因素的影响及各干扰因素对乙醇干扰效应(用干扰因子表示)的相对贡献。实验结果表明,Boltzman因子项和活度系数项的变化是乙醇增敏效应的主要来源。由实验结果分别提出了提升量、校正提升量变化后的干扰因子和活度系数项与乙醇浓度的关系方程。     

Comparison of different sampling heads applied for investigation of welding fume

Welding fume samples were collected in two Hungarian welding plants, where different types of steels were welded with metal active gas (MAG) welding. Welding fumes were sampled with “fixed point” and personal sampling techniques applying different sampling heads: Institute of Occupational Medicine (IOM) sampler and conical inhalable sampler (CIS) for the inhalable aerosol fraction and the Higgins-Dewell (HD) cyclone for the respirable fraction. When sampled, the welding fume samples were digested with the mixture of nitric acid and hydrogen peroxide in a closed vessel microwave digestion system. The Cr, Mn, Ni and Co contents of the solutions were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Iron was analysed only by the ICP-AES method. Metal concentrations of the workplace air were calculated for the three samplers, and the results were compared to each other. The differences of the metal concentrations determined by the different inhalable sampling heads, which were paired during the sampling, proved not to be significant. Therefore, the IOM and CIS heads can be equally used for the sampling of welding fume. Finally, the distributions of metals were determined between the inhalable and respirable fractions. Metal concentrations in the respirable aerosol fraction were 57-98% of the concentrations in the inhalable fraction. These high rates of metals in the respirable aerosol call the attention to the increased health risk of the welding fume.     

Slurry nebulization ICP-AES spectrometry method for the determination of tin in organotin(IV) complexes

This paper proposes a quick, novel method for tin determination in organotin chemicals by slurry nebulization inductively coupled plasma atomic emission (ICP-AES) spectrometry. The method was tested by the measurement of five organotin carboxylate complexes of known composition for obtaining simple stoichiometric data. The slurries were prepared by first dissolving the organotins in an adequate solvent (methanol, pyridine or acetone) well miscible with water and then adding this solution drop-by-drop to a 0.005% TX-100 tenzide solution while maintaining intensive mixing. Dynamic laser light scattering experiments showed that the average equivalent particle size in the resulting slurry was ≈0.3 μm for all samples and solvents. Under suitable ICP-AES measuring conditions, the signal recoveries were found to be between 101.8 and 106.6%, which allowed direct nebulization and calibration against aqueous solutions. Typically, 70 μg l⁻¹ detection limit and 1–5% relative S.D. on five replicates can be achieved by the described method.