微波消解-电感耦合等离子体质谱法检测土壤中16种稀土元素

建立了微波消解-电感耦合等离子体质谱法( ICP - MS)测定土壤样品中16种稀土元素的分析方法.样品经硝酸-过氧化氢-氢氟酸消解,试液直接用ICP - MS测定16种稀土元素.研究了ng·mL-1水平的Ba氧化物及轻稀土氧化物对重稀土元素的干扰程度,测定土壤标准物质GBW07446及GBW07451,结果与标准物质证书值一致.     

微波消解-电感耦合等离子体质谱法同时测定化妆品中五种微量元素

本文以Sc、Ge、In、Re内标校正体系,采用微波消解-电感耦合等离子体质谱法(ICP-MS)对化妆品中As、Pb、Hg、Cd和Cr五种微量元素进行同时测定,通过对三种化妆品的加标回收试验,建立了化妆品中As、Pb、Hg、Cd和Cr五种微量元素含量的ICP-MS分析方法,Hg所采用线性范围为0～10ng/ml,其它元素所采用线性范围为0～500ng/ml,各元素校正方程的线性相关系数均大于0.9996,各元素检出限均小于0.1ng/mL、测定五种元素的相对标准偏差均小于10%,各元素的加标回收率在84.1%～107.9%。实验表明:该法操作简单、快速,灵敏度高,重现性好,而且能够对五种微量元素进行同时测定,大大提高了检测效率。     

离子色谱-电感耦合等离子体质谱法快速测定食品中的硼酸

目的：建立了一种离子色谱-电感耦合等离子体质谱法快速测定食品中的硼酸含量的方法。方法：采用4%三氯乙酸溶液和超纯水溶液超声提取,离子色谱分离,电感耦合等离子体质谱测定,外标法定量。结果：在0.05-5.0μg/mL浓度范围内呈良好线性关系;相关系数大于0.999;方法检出限为：1.0mg/kg,低于国标方法检出限;加标回收率为89.6%-102%,相对标准偏差为0.95-3.72%。结论：该方法操作简便快捷、分离效果好、抗基体干扰性强、检测灵敏度高。所用试剂对环境污染、人体危害更小,可应用于快速测定食品中的硼酸含量。     

微波消解-电感耦合等离子体原子发射光谱法在铝合金多元素检测中的应用

本文建立了铝合金中多元素含量的微波消解-(ICP-AES)法来对铝合金中硅、锰、镁、铁、铜等9种元素含量进行检测。实验结果表明,本方法测定的各元素相对标准偏差(RSD)均小于2.0%,回收率在(96.08~102.50)%之间,方法灵敏度高,重现性好,能够满足实际样品检测要求。     

微波消解-电感耦合等离子体质谱法测定面制食品中铝的含量

本文以Li6为内标,采用微波消解-电感耦合等离子体质谱法(ICP—MS)对面制食品中铝的含量进行测定,通过对三种面制食品的加标回收试验,建立了面制食品中铝含量的ICP—MS分析方法,仪器检出限为在0.12ng/mL、测定的相对标准偏差均小于5.2%,加标回收率在90.4%97.6%。实验表明该法操作简单、快速,灵敏度高,重现性好,能够满足实际样品检测的要求。     

微波消解-电感耦合等离子体质谱法同时测定土壤样品中八种重金属元素

本文以Ge、In、Re内标校正体系,采用微波消解-电感耦合等离子体质谱（ICP—MS）对土壤样品中砷、铅、铜、锌、镉、铬、汞、镍八种重金属元素进行同时测定,通过加标回收试验,建立了土壤样品中砷、铅、铜、锌、镉、铬、汞、镍八种重金属元素ICP—MS分析方法,各元素检出限均小于1．0ng／mL,测定8种元素的相对标准偏差均小于10％,各元素的加标回收率在86．3％～101．0％。实验表明：该法操作简单、快速,灵敏度高,重现性好,而且能够对八种重金属元素进行同时测定,大大提高了检测效率。     

水中汞的电感耦合等离子体-质谱法测定

为解决水中汞不稳定以及易吸附而引起记忆效应的问题,建立分析水中汞的电感耦合等离子体质谱新方法,汞标准溶液中加金形成金汞齐,采用200μg/LAu2+-5%HNO3溶液作为清洗液,选取Rh103作为内标元素。结果标明:在79d内,汞溶液的标准曲线稳定,其相关系数在0.9993⁰.9998之间,仪器检出限在1.15×10-30.9998之间,仪器检出限在1.15×10-3³.11×10-2μg/L范围内。该方法分析水中痕量汞具有检出限低、数据准确性高、再现性好的特点,所用试剂种类少且毒性小。     

水中汞的电感耦合等离子体-质谱法测定

为解决水中汞不稳定以及易吸附而引起记忆效应的问题,建立分析水中汞的电感耦合等离子体质谱新方法,汞标准溶液中加金形成金汞齐,采用200μg/LAu2＋-5%HNO3溶液作为清洗液,选取Rh103作为内标元素。结果标明：在79d内,汞溶液的标准曲线稳定,其相关系数在0.9993~0.9998之间,仪器检出限在1.15×10-3~3.11×10-2μg/L范围内。该方法分析水中痕量汞具有检出限低、数据准确性高、再现性好的特点,所用试剂种类少且毒性小。     

微波消解-电感耦合等离子体发射光谱法测定松茸中9种金属元素

建立松茸中钾、钠、铝、锰、锌、铜、铁、钙、镁的微波消解-电感耦合等离子体发射光谱法测定方法。样品采用3 mL硝酸和2 mL过氧化氢作为消化液,微波消解后,用电感耦合等离子体发射光谱法进行测定。结果表明:各元素线性范围为钠0～2.00μg/mL,钾0～100.00μg/mL,铝、锰、锌、铜、铁、钙、镁均为0～5.00μg/mL,平均回收率在94.14%～102.30%之间,相对标准偏差(RSD)为0.23%～3.21%范围,检出限为0.33～5.25 mg/kg,定量限为1.10～17.50 mg/kg。测得四川省6个主产区松茸中钾、钠、铝、锰、锌、铜、铁、钙、镁的含量范围分别为21～35 g/kg、42.1～117mg/kg, 183～1210mg/kg, 10.2～91.8mg/kg, 23.1～69.5mg/kg, 21.6～37.2mg/kg, 159～1174mg/kg, 51.2～349 mg/kg,441～740 mg/kg。该方法简便、快速、准确,适用于松茸中上述9种元素的同时测定。     

电感耦合等离子体质谱法测定饮用水中微量元素

采用电感耦合等离子体质谱法快速测定饮用水中的微量元素 ,样品处理简便 ,检出限低 ,重现性好 ,分析速度快。方法检出限为 (0 0 0 7～ 0 911) μg L ,精密度达到 0 73%～ 4 87%。     

Solid-phase extraction of Cu, Co and Pb on oxidized single-walled carbon nanotubes and their determination by inductively coupled plasma mass spectrometry

A novel method using a microcolumn packed with single-walled carbon nanotubes (SWNTs) as a new adsorption material was developed for the preconcentration of trace Cu, Co and Pb in biological and environmental samples prior to their determination by inductively coupled plasma mass spectrometry (ICP-MS). SWNTs oxidized with concentrated nitric acid have been proved to possess an exceptional adsorption capability for the analytes due to their surface functionalization. The adsorption behaviors of the analytes on SWNTs under dynamic conditions were studied systematically. The main factors influencing the preconcentration and determination of the analytes (pH, sample flow rate and volume, eluent concentration and interfering ions) have been examined in detail. Under the optimum conditions, the detection limits for Cu, Co and Pb were 39, 1.2 and 5.4 pg mL⁻¹, respectively; the relative standard deviations (RSDs) were found to be less than 6.0% (n = 9, c = 1.0 ng mL⁻¹). This method was validated using a certified reference material of mussel, and has been successfully applied for the determination of trace Cu, Co and Pb in real water sample with the recoveries of 96.0–109%.     

A complete inorganic survey study to reveal and study sensitometric deviations in photographic AgX emulsions by inductively coupled plasma mass spectrometry

Abstract

Inductively coupled plasma mass spectrometry (ICP-MS) offers excellent possibilities for multi-element trace analysis of photographic silver halide emulsions. In the present study, an analytical method was developed for the simultaneous determination of essential elements, such as ruthenium, rhodium, iridium and gold, in small emulsion samples, both overall as well as on the crystal surface. Sample preparation was performed by dissolving the silver halide emulsion into a self-made acid fixer. In-house standard reference emulsion material was prepared to verify the accuracy and precision of the quantitative method. The final result is a quantitative method for the selected elements with a precision of typically 1 per cent or better with relative standard deviations of 0.1–2.0 per cent. Detection limits were in the range 0.01–0.03 μg/kg. Using the scanning mode option of the instrument, the complete mass spectrum can be generated. Overlays can be made of two mass spectra and used as ‘fingerprints’ to reveal sensitometric deviations. Hence elemental trends can be traced or anomalies pinpointed in large batches of samples.     

Determination of trace bismuth in human serum by cloud point extraction coupled flow injection inductively coupled plasma optical emission spectrometry

A cloud point extraction method for the preconcentration of ultra-trace bismuth in human serum prior to its determination by inductively coupled plasma optical emission spectrometry had been developed in this paper. The cloud point extraction method was based on the complex of Bi(III) with 8-hydroxyquinoline and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time were investigated in detail. An enrichment factor of 81 was obtained for the preconcentration of Bi(III) with 25 mL solution. Under the optimal conditions, the detection limit of Bi(III) is 0.12 μg L⁻¹. The relative standard deviation (n = 7) of determination was 2.3%, values of recovery of bismuth were from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination trace bismuth in human serum.     

氢化物发生电感耦合等离子体发射光谱法测定钢中微量砷

该文研究氢化物发生-电感耦合等离子体发射光谱法测定非合金钢(碳素钢)和低合金钢中微量砷的分析方法,考察高频功率、雾化压力、辅助气流量、泵速等仪器工作条件与消解用酸及用量、硼氢化钠浓度对光谱强度的影响,并讨论王水、铁基体、共存离子对测定结果的背景干扰与消除方法.确定的最佳工作条件为:高频功率为1350 W,雾化压力为22...     

采用电感耦合等离子体质谱测定化肥中微量Cr、Cd、As、Pb、Hg元素

采用电感耦合等离子体质谱法测定化肥中微量Cr、Cd、As、Pb、Hg元素。仪器经条件优化，以In为内标，样品的基体效应和仪器漂移能得到很好的补偿。微波消解和敞开酸溶两种样品处理方法比较可知，微波法具有更高的精密度和准确度。方法的标准加入回收率在85-120％，RSD％〈15％，误差完全符合GB18877-2002的规定，方法简便快速。     

Impedance transition and series resonance between bulk plasma and sheath in biased inductively coupled plasma

The impedance transition and electron series resonance at an RF bias substrate were observed in 13.56 MHz inductively coupled plasma (ICP). As ICP coil power increased, the impedance of the RF bias transitioned from a capacitive to an inductive load. When bias voltages and discharge impedances reached minimums, bias voltages and currents were in-phase during the transition. The transition can be understood as a series LC resonance between the sheaths (capacitor) and plasma bulks (inductance due to electron inertia). This corresponds to the electron series resonance (ESR) observed in very high-frequency capacitive discharges, and a new ESR frequency which considers sheath resistances is presented.     

微波消解ICP-AES测定海绵铁中杂质元素含量的研究

运用微波消解处理海绵铁试样,结合ICP—AES测定钙、镁、硅、铝、磷、钾、钠等7种杂质元素。加标回收率在92．4％-101．8％,精密度为0．55％-3．85％,方法准确,分析速度快,效率高,在日常快速分析检测中有重要意义。     

电感耦合等离子体发射光谱法测定矿石中银的研究

目前,实验室测定矿石中银的方法主要有银的光度法、火焰原子吸收光谱法、石墨炉原子吸收光谱法等等,为了更好的简化测量过程、提高工作效率,本文旨在建立更适宜的、能满足于高中低含量银的测试方法,采用电感耦合等离子体光谱法测定金属矿中银的含量.样品采用氢氟酸、硝酸、硫酸(体积比10∶5∶1)溶解,赶净氟和破坏有机物后,经(1+1...     

Effect of swirl flow on an atmospheric inductively coupled plasma supersonic jet

Recently supersonic jets extracted from atmospheric inductively coupled plasmas (ICP) have attracted a lot of attention. Usually atmospheric ICP generators have employed swirl flow injection in order to stabilize the plasma. However the effect of the swirl flow injection on the performance of atmospheric ICP generators has not been understood enough. This work found that the injection of the swirl flow deteriorates the performance. First we conducted the total enthalpy measurement based on the sonic flow method and evaluated the averaged specific enthalpy. Then laser absorption spectroscopy was employed in order to measure the temperature and the velocity of the extracted supersonic jet. The both measurements observed that the specific enthalpy of the jets decreased with the increase in the swirl flow fraction. This would be because the swirl flow affected the shape and the position of the plasma significantly.