ICP-AES法测定高温合金中5种非金属元素

本文研究了快速测定高温合金中5种非金属元素(As、B、P、Se、Si)的分析方法,以满足高温合金行业对非金属元素检测的需求。利用王水和高氯酸对高温合金进行酸溶解,并系统研究了基体元素和共存元素对分析元素谱线的光谱干扰情况,同时进行了分析谱线的选择。5种非金属元素的检出限在5.5 ～ 11.9 ug/ml,5次数据的相对标准偏差(RSD,n=5)为0.9 % ～ 7 %,各元素的回收率在96 % ～ 102 %之间,该方法适用于高温合金中非金属元素的测定。     

盐酸-硝酸体系溶解―ICP-OES法测定镍-铬基高温合金GH4133B中铝铌钛铬铁

GH4133B是Ni-Cr基沉淀硬化型变形高温合金,近年来我国还没有适宜的国家标准,基于此对样品主要元素含量准确测定方法进行了研究和探讨。采用盐酸-硝酸体系对GH4133B镍基高温合金进行溶解,确定了盐酸和硝酸比列为8:3,混合酸用量为11mL;采用ICP-OES法快速准确的对GH4133B镍基高温合金中铝、铌、钛、铬、铁元素含量进行测定;确定了各元素分析谱线为Al396.152nm、Nb309.417nm、Ti334.941nm、Cr267.716nm、Fe238.204nm;建立了校准工作曲线,各元素线性相关系数均在0.999以上;优化仪器参数消除基体干扰,测定了方法检出限,各元素检出限均小于0.003%,各元素测定结果的RSD/%在0.26%～0.47%之间(n=7),加标回收率在103.0％~104.5％之间。有效解决了GH4133B镍基高温合金快有效速溶解及准确测定问题。     

电感耦合等离子体发射光谱(ICP-OES)法测定镍基/钴基高温合金中硼磷硅

采用一定比例的混合酸溶解样品,利用基体匹配配制一系列标准溶液消除基体的影响,以及轴向观测喷嘴吹扫技术来提高待测元素的灵敏度,使用电感耦合等离子体发射光谱(ICP-OES)法测定镍基/钴基高温合金中硼磷硅。各元素选的分析线依次为B 182.577 nm、P 178.222 nm、Si 185.005 nm。检测范围分别是:B 0.001%~3.0%,P 0.003%~0.20%,Si 0.005%~3.0%,检出限范围为0.00005%~0.0004%,线性相关系数>0.9995。加标回收率为90.0%~105%,精密度RSD<2.0%。方法操作简单快速,结果令人满意。     

电感耦合等离子体光谱法测定镍基高温合金中的硅、锰、磷

建立了电感耦合等离子体光谱测定镍基高温合金中硅、锰、磷元素的方法,优化了试样前处理方法,对前处理所用酸的酸度进行不同比例试验,确定了仪器测量条件及分析谱线.在一定浓度范围内,各元素的浓度与谱线强度呈线性关系,相关系数大于0.9999.加标回收率为93.3%～106.7%,测定结果的相对标准偏差小于3.0%(n=10)....     

ICP-AES法测定镍基高温合金中的铂

采用电感耦合等离子体原子发射光谱法测定镍基高温合金中铂元素。通过实验探讨了镍基高温合金中基体元素镍,主量元素如铬、钴、铝、钼、镍、钽等对铂元素测量的干扰情况,确定了适合的分析谱线。测定结果的相对标准偏差不大于6.55%(n=6),加标回收率为94%～105%。该法可用于镍基高温合金中铂元素的测定。     

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法测定高温合金中低含量钇

建立电感耦合等离子体原子发射光谱法测定高温合金中低含量钇的方法。采用盐酸、硝酸、氢氟酸溶解样品,在优化的仪器条件下,采用基体匹配法配制系列标准工作溶液,选择分析线为360.073 nm。钇的含量在0.0005%~0.050%范围内与光谱强度具有良好的线性关系,相关系数为0.99999,检出限为0.000003%。该方法测定结果的相对标准偏差不大于6.0%(n=8),加标回收率为90.0%~104.0%。该方法简便、快速、准确,可用于高温合金中低含量钇的测定。     

激光剥蚀-电感耦合等离子体质谱对高温合金中17种痕量元素的测定

建立了镍基高温合金中Sc、Cu、Zn、Ga、Ge、As、Ag、Cd、In、Sn、Sb、Te、Ce、Hf、Tl、Pb、Bi17种痕量元素的激光剥蚀-电感耦合等离子体质谱测定方法。对激光剥蚀进样及质谱分析条件进行了优化,通过激光对样品表面的层层剥蚀顺利完成了对低沸点杂质元素的测定。采用格栅扫描采样,严格控制样品的聚焦位置和散焦距离以保证采样的准确性,由高温合金系列标准物质建立了18种痕量元素的校正曲线,其中14种痕量元素的线性相关性较好(r2≥0.99),In、Sn、Sb、Ce、Tl、Pb、Bi等超痕量元素的检出限和气体空白分别低于或接近0.000 005%和0.000 001%。方法对镍基高温合金样品中Cu、Ga、Ag、Cd、In、Sn、Sb、Te、Hf、Tl、Pb和Bi等痕量元素的测定结果与参考值吻合较好,且大部分元素的RSD(n=4)小于或接近30%。     

高分辨电感耦合等离子体质谱法测定镍基单晶高温合金中36种痕量元素

基于高分辨电感耦合等离子体质谱法(HR-ICP-MS)的质谱干扰消除技术,对镍基单晶高温合金中36种痕量元素检测的质谱条件、基体干扰、质谱干扰与同位素选择进行了研究。取样品0.100 0 g,用体积比为3∶1的盐酸-硝酸混合酸10 mL、氢氟酸1 mL溶解,用水定容至250 mL。通过复杂基体质谱干扰计算判定、共存元素干扰消除,确定了待测元素的同位素和分辨模式,将镍基单晶高温合金中痕量元素准确测定的元素种类确定为36种。采用标准加入法进行定量分析,36种痕量元素的检出限(3s)为0.004～6.000μg·L^-1。方法用于分析国际标准物质,得到的测定值与认定值基本一致。方法用于镍基单晶高温合金样品分析,36种痕量元素的检出量为0.000 001 0%～0.018%。     

Determination of toxic elements in coal by ICP-MS after digestion using microwave-induced combustion

A microwave-induced combustion (MIC) procedure was applied for coal digestion for subsequent determination of As, Cd and Pb by inductively coupled plasma mass spectrometry (ICP-MS) and Hg using cold vapor (CV) generation coupled to ICP-MS. Pellets of coal (500 mg) were combusted using 20 bar of oxygen and ammonium nitrate as aid for ignition. The use of nitric acid as absorbing solution (1.7, 3.5, 5.0, 7.0 and 14 mol L⁻¹) was evaluated. For coal samples with higher ash content, better results were found using 7.0 mol L⁻¹ HNO₃ and an additional reflux step of 5 min after combustion step. For coal samples with ash content lower than 8%, 5.0 mol L⁻¹ nitric acid was suitable to the absorption of all analytes. Accuracy was evaluated using certified reference material (CRM) of coal and spikes. Agreement with certified values and recoveries was better than 95 and 97%, respectively, for all the analytes. For comparison of results, a procedure recommended by the American Society of Testing and Materials (ASTM) was used. Additionally, a conventional microwave-assisted digestion (MAD) in pressurized vessels was also performed. Using ASTM procedure, analyte losses were observed and a relatively long time was necessary for digestion (>6 h). By comparison with MAD procedure, higher sample mass can be digested using MIC allowing better limits of detection. Additionally, the use of concentrated acids was not necessary that is an important aspect in order to obtain low blank levels and lower limits of detection, respectively. The residual carbon content in digests obtained by MAD and MIC was about 15% and <1%, respectively, showing the better digestion efficiency of MIC procedure. Using MIC it was possible to digest completely and simultaneously up to eight samples in only 25 min with relatively lower generation of laboratory effluents.     

Determination of trace elements in liquid aspartame sweeteners by ICP OES and ICP-MS following acid digestion

In order to determine inorganic constituents and contaminants in liquid aspartame sweeteners, different brands of this product were analyzed by ICP OES and ICP-MS. The samples were submitted to acid digestion and parameters such as internal standardization and wavelengths, in the case of ICP OES, and a recovery test were evaluated. The analytes studied were As, Ca, Cd, Co, Cu, K, Fe, Mg, Mn, Na, Ni, Pb, Se and Zn. Since there is not a certified reference material for sweeteners, the accuracy of the proposed method was evaluated by recovery tests and the values were in the range of 90–110% for the majority of the analytes. The detection limits for the elements determined by ICP OES were in the range 0.01 (Mn)– 2.0 (K) μg g⁻¹ while those determined by ICP-MS were 0.001 μg g⁻¹ for all the elements except Mn and As (0.002 μg g⁻¹). The relative standard deviations were below 12% for ICP OES and below 14% for ICP-MS determinations. The mean concentration of the elements detected by ICP OES (Ca, Fe, K, Mg, Na, and Zn) varied according to the brand. The other analytes, were determined by ICP-MS. For these elements, a significant variation in their concentrations was also found for different samples, except for Co and Ni. The use of both multielemental techniques allowed the evaluation of the inorganic composition and the rapid determination of several elements in aspartame sweeteners, with adequate accuracy.     

等离子体发射光谱法测定大白鼠脑组织中的铝

铝元素在脑中累积会损伤脑功能[1-2],据不少文献报道,阿尔茨海默氏病(A lzheimer′s d isease,简称AD)即人们统称的老年性痴呆病患者脑中的铝含量显著高于正常人[3-4]。铝在脑中含量很低,目前测定低含量铝使用较多的方法是石墨炉原子吸收法,由于铝在高温时容易与石墨管发生反应     

电感耦合等离子体—光发射光谱中抑制易电离元素干扰研究的进展

从等离子体的强化状态、影响强化状态的分析参数及易电离元素对进样系统的影响三方面综述了电感耦合等离子体-光发射光谱分析中抑制易电离元素干扰的研究进展,引用文献46篇。     

ICP-OES,AAS和AFS测定肝癌高发区红豆中23种矿质元素含量

收集了6种产自肝癌高发区——江苏省启东市的红豆和6种产自国内其他地区的红豆,经过微波消解或干灰化法处理后,采用电感耦合等离子体发射光谱法(ICP-OES)、原子吸收光谱法(AAS)和原子荧光光谱法(AFS)测定了其中A l、B、Ba、Ca、Cd、Co、Cr、Cu、Fe、Hg、K、Mg、Mn、Mo、Na、N i、P、Pb、Rb、S、Se、Sr和Zn共23种矿质元素的含量,并用生物标准参考物质黄豆评价了分析方法的准确度。结果表明,红豆中人体必需宏量、微量元素含量极为丰富,而传统意义上的有害元素Pb、Cd、Hg含量均较低;与国内其他产地的红豆相比,江苏省启东市产红豆中B、Mg含量显著偏高(P0.05),而大多数矿质元素含量两相比较并不存在显著性差异。产自江苏省启东市的部分红豆样品和产自江苏省海门市的红豆样品中Cd含量极低,预示着自然生态环境中有效态Cd缺乏可能与肝癌的高发病率和高死亡率存在一定程度的相关性。     

ICP-AES内标法测定钢铁及其合金样品中的化学成分

建立了内标法测定钢铁样品中化学成分的ICP-OES分析方法。利用铟元素作为内标物质,消除了铁基体元素对被测元素的干扰,减少了废气、废液的产生。钢铁样品中16种被测元素的检测范围在0．001％-20．00％之间,检出限为0．001-0．030μg／mL,回收率为97％-110％。该方法减少了高纯物质的使用。     

Determination of inorganic contaminants in glue by inductively coupled argon plasma optical emission spectrometry

A closed vessel method using a microwave oven was developed for the determination of As, B, Ba, Bi, Cd, Cr, Cu, Fe, Hg, Ni, Pb, Se, Sn and Sb by Inductively Coupled Argon Plasma Optical Emission Spectrometry (ICP OES). The method was applied to samples of polyvinyl acetate-based glue in water emulsions. Parameters such as wavelength, nebulization pressure and RF power were optimized and the residual acidity after the digestion process was determined. The addition of internal standards was evaluated and the accuracy of the proposed method was verified with addition and recovery experiments and also with certified reference materials, achieving good results. Using a nebulization flow rate of 0.73 L min⁻¹and a RF power of 1200 W it was possible to obtain adequate values for limit of detection and limit of quantification as well as recovery values in the range of 80-106%, for all the analytes. The analysis of coloured glue samples (white, black, blue, yellow, red and green), widely used by children, showed no contamination by the elements studied.     

Determination of lead in seawater by inductively coupled plasma optical emission spectrometry after separation and pre-concentration with cocrystallized naphthalene alizarin

An analytical method for separation and pre-concentration of lead in seawater for determination by inductively coupled plasma optical emission spectrometry has been investigated. Lead was retained in the solid phase (0.5 g) composed of co-precipitated naphthalene and alizarin red. The solid phase quantitatively sorbs Pb(II) at pH 8–9, and the metal was eluted using 5.0 ml of 2 mol l⁻¹ nitric acid. The effect of NaCl, KCl, BaCl₂, CaCl₂, Na₂SO₄, MgCl₂ and Na₃PO₄ on the sorption of Pb(II) in the solid phase was studied. A set of solutions containing varying amounts of electrolytes (0.5; 1.0; 3.0 and 5.0% m/v) with Pb (50 μg) was prepared and the recommended procedure applied. The Na₃PO₄ was found to interfere; the other electrolytes did not interfere up to 5% m/v. A pre-concentration factor of 40 was obtained in this analytical procedure. The limit of detection and limit of quantification for Pb(II) were 53 and 176 μg l⁻¹, respectively. Lead was determined in seawater samples collected in Salvador city, Bahia, Brazil. The precision, expressed as R.S.D., was 1.8–4.6%, and the recovery of lead added to seawater samples was 95–97%.     

The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.     

Quantification of Inorganic Constituents in Brazilian Human Milk by ICP OES

A fast procedure to determine essential and toxic metals in Brazilian human milk by ICP OES is proposed. Mature and colostrum human milk samples were mineralized using closed-pressurized and high-performance microwave digestion oven. Aqueous calibration was performed for all analytes investigated. A reference material, Infant Formula, was analyzed to test the accuracy of the proposed methodology. Recovery rates ranged between 83 and 117%. The precision of the method was better than 3.3% (R.S.D.) for all analytes investigated. Higher concentrations, on average, of the metals studied in the colostrum human milk could be found in relation to the mature human milk.