电感耦合等离子体发射光谱法测定石灰石中二氧化硅的研究

本文旨在建立电感耦合等离子体发射光谱法测定石灰石中二氧化硅含量的方法.样品通过碱熔融,热水提取再经强酸酸化形成清亮待测液,针对Si的5条分析谱线进行测试研究.通过对GBW07214、GBW(E)070155、GBW07215、GBW07120四件具有代表性的国家标准物质进行试验结果的精密度、准确度、加标回收统计分析.结...     

电感耦合等离子体发射光谱法测定球化剂中氧化镁

本文用电感耦合等离子体发射光谱法测定球化剂中氧化镁含量。试样用重铬酸钾浸取、分离,在稀盐酸介质中测定氧化镁含量,考察了浸取时间、放置时间和仪器工作条件的影响,并进行了干扰试验以及精密度试验。选取4个球化剂样品进行了测定,与标准方法原子吸收方法测定结果基本一致。方法简便快速准确,结果满意。     

电感耦合等离子体发射光谱法测定面制品中铝含量

建立ICP-AES等离子体发射光谱法测定面制品中铝含量的方法,该方法检测线性好与检出限低5.6mg/kg,精密度RSD为0.1~0.6%,回收率高方法的回收率为97.4%~104.5%。ICP-AES法测定面制品中铝方法检测速度快,操作简单,结果准确可靠,适合于面制品中铝的日常监督检验。     

电感耦合等离子体发射光谱法测定重晶石矿石中Cu、Pb、Zn

采用电感耦合等离子体发射光谱法对重晶石标准物质定值,同时测定重晶石矿石中cu、Pb、Zn.研究了基体效应对元素测定的影响及消除,测定值与确定值(标准值)符合,Cu、Pb、Zn相对标准偏差(RSD%,n=12)为0.62%、2.89%、1.82%.本方法简便、快速,准确.     

应用电感耦合等离子体发射光谱法测定岩矿中的金

用电感耦合等离子体发射光谱法测定锑金精矿中金量解决了样品在烧样除炭过程中因锑的熔解而结块、在溶解实验过程中因大量锑的水解包裹使金的溶解变得较为困难的问题。采用电感耦合等离子体发射光谱法测定金,克服了原子吸收法测定的线性范围小,而稀释倍率大,造成分析误差偏大的不足。方法的检出限为0．1μg／g。金加标回收率96％～104％,精密度（RSD,n=6）〈3．0％。适宜于锑金精矿中金的测定。     

刍议电感耦合等离子体原子发射光谱法测定矿石中的钨钼含量

本文立足于矿石钨、钼测定的现实状况,通过形象、生动地实验重点探析矿石钨、钼两种金属元素的测量流程。通过实验论述原子发射光谱的方法在测定金属钨、钼含量的具体方法与策略。     

电感耦合等离子体原子发射光谱法测定铬铁中的铬磷硅

用电感耦合等离子体原子发射光谱法(ICP-AES)测定铬铁中铬磷硅存在的问题是一些高碳铬铁、氮化铬铁等试样难以用酸溶解,在碱熔基体中,大量的易电离元素钠的存在使得测定困难,铬铁中高含量铬和微量的磷、硅等同时测定尤为困难。ICP-AES法同时测定铬铁中铬磷硅是一种新颖的方法。通过试验研究,确定了利用氢氧化钠-过氧化钠混合熔剂熔样的样品处理方法。在用ICP进行测试时,不同谱线所受到的干扰不同。推荐选择Cr 267.716 nm、Cr 206.158 nm、P 213.617 nm、Si 251.611 nm、Si 288.158 nm为分析线;对于干扰,采用基体匹配和两点校正法消除,方法的线性相关系数在0.995以上,磷的测试精密度在5.0%,铬、硅在1.0%以下;铬、硅检出限在0.006%以下,磷为0.002%。准确度试验表明,分析结果与推荐值和手工分析结果间的分析误差在试验允许的误差范围内。     

电感耦合等离子体原子发射光谱法测定纯钛中加入的合金元素

采用电感耦合等离子体原子发射光谱法测定纯钛中加入的合金元素,确定了样品中元素的分析谱线以及优化了仪器工作条件。测试方法的加标回收率在98.0%～112.0%之间,RSD2.90%,与标准样品测试结果一致,测试方法高效可行。     

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。     

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...     

Optimization of an open-focused microwave oven digestion procedure for determination of metals in diesel oil by inductively coupled plasma optical emission spectrometry

This work reports the optimization of a focused microwave assisted procedure for the wet acid dissolution of diesel oil in order to allow the determination of metals in the samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The dissolution process was monitored by measuring residual carbon content (RCC), also by ICP-OES, in the final solutions obtained after application of digestion program. All experimental work was performed using a commercial sample of diesel oil containing 85.74+/-0.13% of carbon. The initial dissolution program comprised three steps: (i) carbonization with H(2)SO(4); (ii) oxidation with HNO(3) and (iii) final oxidation with H(2)O(2). During work it was verified that the first step played an important role on the dissolution process of this kind of sample. It is therefore, necessary to give a detailed optimization of such step. Employing the optimized conditions it was possible to digest 2.5 g of diesel oil with a 40 min-heating program. At these conditions, residual carbon content was always lower than 5%. Optimized methodology was applied in the determination of metals in three diesel oil samples by ICP-OES. Recovery tests were also performed by adding 10 microg of metals, as organic standards, to the samples before digestion. Recovery percentages always higher than 90% were obtained for the metals of interest (Al, Cu, Fe and Ni), except for Zn, which presented recoveries between 70 and 78%.     

电感耦合等离子体原子发射光谱法测定电解钴中杂质元素

金属钴试样经酸消解后,未经基体分离直接以全谱直读电感耦合等离子发射光谱仪测定其中杂质元素。确定了仪器的最佳工作条件,选择了合适的分析谱线,采用钇作为内标物质,补偿基体效应。方法测定各元素的检出限在0.0001～0.02mg.L-1范围内。方法用于样品的测定,相对标准偏差为1.5%～7.5%,回收率为94.0～104.0%,各元素的测定值与国家标准方法的测定值相符合。     

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。     

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%。     

Time evolution of electronegativity in a pulsed inductively coupled oxygen plasma

The electronegativity in a continuous wave (CW) and pulsed mode plasmas was calculated using the measured results of both the single Langmuir probe and the retarding field analyzer. For the pulsed mode measurement, both of the measurements were performed in a time-resolved method using a boxcar sampling technique. For the conversion of the retarding field analyzer measurement results into absolute positive ion densities, argon plasma was used as a reference. The pulsed oxygen plasma was generated using the inductively coupled antenna and modulated at a repetition rate of 5 kHz and the duty ratio of 50%. The gas pressure was changed from 5 to 30 mTorr. The time evolution of the electronegativity shows that there is a pressure regime where the electron attachment reaction during the RF on-time is very active, indicating that the negative ion density reaches its maximum value during the RF on-time. Compared to the CW oxygen plasma, the electronegativity of the pulsed oxygen plasma varies within a wider range of values.     

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。     

微波辅助萃取-电感耦合等离子体质谱法检测食品中的硼砂

建立了一种应用微波辅助萃取-电感耦合等离子体质谱法检测食品中的硼砂的方法。以0.1 mol/L氨水来消除硼的记忆效应。硼含量在0～2.0μg/mL范围内线性关系良好,R=1.0000。硼砂检测限为2.0 ng/mL(σ=3),RSD小于5%,方法回收率为95.2%～103.4%。该法与GB/T21918-2008中的三种检测方法相比,具有操作简单、快速、试剂污染少的特点。可作为食品中硼砂含量的检测方法之一。     

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%.