电感耦合等离子体原子发射光谱法同时测定土壤中的铜、锌、镍、铬

建立电感耦合等离子体原子发射光谱法同时测定土壤中铜、锌、镍、铬的含量。在土壤样品中分步加入盐酸、硝酸、氢氟酸,电热板加热消解,将土壤标准物质GSS–17,GSS–22,GSS–8,GSS–27与样品按相同的方法处理绘制工作曲线。铜、锌、镍、铬的分析波长分别为327.39,206.20,231.60,267.72 nm。在一定的质量浓度范围内工作曲线表现出良好的线性关系,相关系数均大于0.999,4种元素的方法检出限分别为0.4,0.5,0.3,0.6 mg/kg。采用土壤标准物质GSS–26,GSS–20,GSS–16对方法准确度进行验证,测定值与标准值基本一致,样品加标回收率为82.3%～107.0%,测定结果的相对标准偏差为1.58%～4.68%(n=8)。该方法检出限、准确度和精密度均满足检测要求,可用于快速准确检测批量土壤样品中的重金属含量。     

化学蒸气发生-电感耦合等离子体原子发射光谱法测定地质样品中痕量金

地质样品经盐酸-硝酸(3+1)混合酸溶解,活性炭分离富集后,于90℃用12g.L-1硼氢化钠溶液(溶于0.5g.L-1氢氧化钠溶液中)作还原剂,用化学蒸气发生-电感耦合等离子体原子发射光谱法测定其中痕量的金。金的质量浓度在1 500μg.L-1以内与其发射强度呈线性关系,方法的检出限(3s)为0.59μg.L-1。方法用于测定2个标准物质(GBW 07289和GBW 07291)中金含量,测定值与认定值相符。     

泡沫塑料吸附-电感耦合等离子体发射光谱法测定地质样品中的金

建立了泡沫塑料吸附-电感耦合等离子体原子发射光谱法测定地质样品中的金的方法,采用王水溶解地质样品中痕量的金,经泡沫塑料吸附富集,结合电感耦合等离子体原子发射光谱法进行测定。实验表明,方法的加标回收率为94.4%~111.0%,对国家一级标准物质进行测定,结果与认定值一致,方法的相对标准偏差RSD为3.2%~12.8%。     

预混旋流雾化-氢化物发生电感耦合等离子体原子发射光谱法同时测定氢化物及非氢化物形成元素

在原旋流雾室气动雾化-氢化物发生装置上增加样品-硼氢钠溶液混合通道,使氢化物形成元素的检出限较原装置明显改善,非氢化物形成元素的检出限也有一定改善;汞可还原为原子蒸汽而提高进样效率,检出限较通常的气动雾化法改善20倍。方法应用于地质样品中氢化物及非氢化物形成元素的同时测定。     

电感耦合等离子体原子发射光谱法快速测定水泥中三氧化硫

水泥样品经硝酸-盐酸(2+6)混合溶液溶解后,采用电感耦合等离子体原子发射光谱法测定水泥中的三氧化硫的含量。在基体中不含有钙元素时,选择波长为180.7 nm谱线的作为测定三氧化硫的分析线;当基体中含有钙元素时,选择波长为182.0 nm的谱线作为分析线。方法的检出限(3s)为20μg·L~(-1)。该方法用于测定标准物质(GBW 03201a,GBW 03205)中三氧化硫的含量,相对标准偏差(n=10)在1.00%～0.56%之间,所得结果与标准值相一致。     

电感耦合等离子体原子发射光谱法在环境分析中的应用

对1996—2010年间电感耦合等离子体原子发射光谱法在环境分析中的应用进展作了评述,主要涉及在大气和飞灰、水、土壤、污泥和植物等方面中的应用(引用文献23篇)。     

电感耦合等离子体原子发射光谱法同时测定铜基低银焊料中的银、磷和锡

采用王水消解铜基低银焊料样品,选择Ag 328.0 nm、P 178.2 nm、Sn 189.9 nm作为分析线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)同时测定铜基低银焊料中银、磷和锡元素的分析方法.在选定的试验条件下,方法检出限为0.002 4%~0.004 8%(质量分数),各元素校准曲线线性相关系数均大于0.999 5.按照试验方法测定样品,加标回收率为95%~103%,测定结果的相对标准偏差(RSD,n=10)均小于5%.     

电感耦合等离子体原子发射光谱法同时测定高强度玻璃纤维粉体中9种金属元素

建立电感耦合等离子体原子发射光谱法测定高强度玻璃纤维粉体中铝、镁、钙、铁、钛、锂、铈、钠、钾9种金属元素含量的方法。采用氢氟酸、高氯酸和盐酸分两段溶解样品,分别在选定的各元素分析谱线下,采用电感耦合等离子体原子发射光谱仪测定各元素含量。9种金属元素在各自的质量浓度范围内与光谱强度成良好的线性关系,相关系数均大于0.999,检出限为8.0~17.4 μg/g。测定结果的相对标准偏差小于1.8%(n=6),加标回收率为97.6%~103.7%。该方法准确,简便,快速,适用于高强度玻璃纤维中多金属元素的同时测定。     

电感耦合等离子体原子发射光谱法同时测定植物样品中多种元素

本文为环境样品分析建立了准确、灵敏、快速的分析方法,探讨了酸类及酸度对谱线强度的影响,同时对基体元素的谱线干扰进行了校正和背景扣除,测定了环境背景值样品树干和树叶中15种元素,经标样测定结果满意。     

电感耦合等离子体原子发射光谱法测定生物样品中13种元素

用电感耦合等离子体原子发射光谱法测定了生物样品中13种元素(铝、钡、钾、钠、钙镁、锰、铁、锶、钛、磷、硫、硼),并建立了等离子体的稳健状态(高频功率1 150 W,载气压力1.92×105Pa),生物样品用浓硝酸与浓盐酸(3+1)的混合酸加压消解.为使样品溶解完全(特别对铝、钡及钛从样品中完全溶出)加入氢氟酸1～2滴(约0.1 mL).经试验,样品溶液中硝酸-盐酸混合酸以10份溶液中占1份(体积比)为宜,例如用硝酸-盐酸混合酸2.5 mL溶解0.5 g试样后,将溶液用水定容为25 mL,提出选用一种生物标准物质(GBW 07602)与样品同时操作后制作校正曲线为验证所提出方法的可行性,按方法分析了几种生物样品的标准物质(GBW 10014,GBW 10015GBW 10046,GBW 07604等),所测得各元素的含量与证书值一致.     

Simultaneous determination of the constituents in Al-Ge-Si alloys by inductively coupled plasma atomic emission spectrometry

An accurate method for determination of the constituents Ge, Si, In and Mg in Al–Ge–Si based compact alloys and foil materials by ICP atomic emission spectrometry is developed. The material samples were dissolved in nitric acid–hydrofluoric acid. Optimum parameters for the simultaneous measurement of the constituent elements are worked out. To compensate the time determined sensitivity fluctuations the analytical signal was corrected by a special procedure of external standardization.     

Simultaneous determination of the constituents in Al-Ge-Si alloys by inductively coupled plasma atomic emission spectrometry

An accurate method for determination of the constituents Ge, Si, In and Mg in Al-Ge-Si based compact alloys and foil materials by ICP atomic emission spectrometry is developed. The material samples were dissolved in nitric acid-hydrofluoric acid. Optimum parameters for the simultaneous measurement of the constituent elements are worked out. To compensate the time determined sensitivity fluctuations the analytical signal was corrected by a special procedure of external standardization.     

电感耦合等离子体质谱法同时测定地质样品中镉、锗、钴

建立电感耦合等离子体质谱法同时测定地质样品中镉、锗、钴含量的分析方法。样品用氢氟酸-硝酸混合溶液加热溶解,然后加热浓缩驱酸,再用硝酸溶液(1+1)复溶提取,在选定的仪器工作条件下进行测定。镉、锗、钴的含量分别在0.00~0.10,0.00~5.00,0.00~50.00 μg/g范围内与质谱峰强度呈良好的线性关系,相关系数均大于0.999,方法检出限分别为0.01,0.02,0.02 μg/g。用该方法对国家一级标准物质进行测定,测定值的相对误差均小于10%,测定结果的相对标准偏差为0.79%~8.45%(n=12)。该方法样品处理过程简便,检测效率高,适用于批量地质样品中镉、锗、钴的测定。     

Accurate determination of trace amounts of phosphorus in geological samples by inductively coupled plasma atomic emission spectrometry with ion-exchange separation

In order to determine trace amounts of phosphorus in geological and cosmochemical rock samples, simple as well as reliable analytical schemes using an ICP-AES instrument were investigated. A (conventional) ICP-AES procedure could determine phosphorus contents at the level of several 100 μg g⁻¹ with a reasonable reproducibility (<10% for 200 μg g⁻¹; 1σ). An ICP-AES procedure coupled with matrix-separation using cation and anion exchange resins could lower the quantification level down to 1 μg g⁻¹ or even lower under the present experimental conditions. The matrix-separation ICP-AES procedure developed in this study was applied to twenty-one geological reference samples issued by Geological Survey of Japan. Obtained values vary from 1250 μg g⁻¹ for JB-3 (basalt) to 2.07 μg g⁻¹ for JCt-1 (carbonate). Matrix-separation ICP-AES yielded reasonable reproducibility (less than 8.3%; 1σ) of three replicate analyses for all the samples analyzed. In comparison of our data with certificate values as well as literature or reported values, there appear to be an apparent (and large) discrepancy between our values and certificate/reported values regardless of phosphorus contents. Based on the reproducibility of our data and the analytical capability of the matrix-separation ICP-AES procedure developed in this study (in terms of quantification limit, recovery, selectivity of an analyte through pre-concentration process, etc.), it is concluded that certified values for several reference standard rocks should be reevaluated and revised accordingly. It may be further pointed that some phosphorus data reported in literatures should be critically evaluated when they are to be referred in later publications.     

Preconcentration of Zr, Hf, Nb, Ta and W in seawater using solid-phase extraction on TSK-8-hydroxyquinoline resin and determination by inductively coupled plasma-mass spectrometry

Here, we present the first simultaneous preconcentration and determination of ultratrace (pmol kg⁻¹ level) Zr, Hf, Nb, Ta and W in seawater, both in the form of dissolved and acid-dissolvable species. 8-Hydroxyquinoline (8HQ) bonded covalently to a vinyl polymer resin, TSK-8HQ, was used in a chelating adsorbent column to concentrate the metals. The greatest advantage of this resin is its endurance to 5 M HF, since this is an effective eluent for all five metals. The analytes were successfully concentrated from 250 mL seawater with a 50-fold concentration factor through the column extraction and evaporation. The detection limit was 0.009-0.15 pmol kg⁻¹. The procedure blank determined using ultra pure water as a sample was 0.005-0.37 pmol kg⁻¹. The five metals were quantitatively recovered from seawater with good precision (2-4%). The effect of sample pH, sample flow rate, eluent composition and sample pretreatment were carefully studied. This method was applied to seawater.     

Simultaneous determination of trace metals in sewage and sewage effluents by inductively coupled argon plasma atomic emission spectrometry

Inductively coupled plasma excitation sources are adapted for the simultaneous determination of multiple elements in sewage and sewage effluents by atomic emission detection. Digestion with aqua regia in test tubes is recommended for sample preparation. A typical comparison of lead in sewage by atomic emission (x) and atomic absorption (y) gave a least-squares fit of x = 0.98 y + 0.03 with a standard error of 0.5 mg l^-1 and a correlation coefficient of 0.996. More complete comparison data by the atomic emission and absorption techniques are presented for other elements.     

Simultaneous determination of major to ultratrace elements in geological samples by fusion-dissolution and inductively coupled plasma mass spectrometry techniques

A method has been developed for the simultaneous quantification of major to ultratrace elements in geological samples using quadrupole ICP-MS techniques. The sample preparation involves fusion with LiBO₂ and dilution in HNO₃-HF which allows complete decomposition of refractory minerals and quantification of the elements of interest. The effects of high Total Dissolved Solids (TDS) and Li in the solution are minimized using a matrix-tolerant interface and conditioning the instrument with LiBO₂ solution. The signal drift is moreover controlled using conventional internal standards and specific Drift Correction Standards (DCS). A key issue of the technique is the external calibration using selected Certified Reference Materials (CRM). Depending on the sample type and analytes of interest three optimized programmable modes are used sequentially: Standard, Collision Cell (CCT) and Kinetic Energy Discrimination (KED) mode. The method allows to quantify more than 40 elements in concentrations from tens-of-percent to <0.1 ppm levels during a single experiment. The method has been validated through the analysis of different CRMs with recovery factors of ca. 100% and typical 2σ errors of <10%.     

Optimization of selenium determination in plant samples by hydride generation and axial view inductively coupled plasma atomic emission spectrometry

The use of hydride generation coupled with axial view inductively couple plasma atomic emission spectrometry was presented for the determination of selenium in plant samples. The chemical factors affecting potentially the hydride generation efficiency (hydrochloric acid, sodium borohydride and sodium hydroxide concentrations) were assessed through investigation of chemical interference, accuracy and repeatability. The accuracy of measurements was not affected by elements present in high concentration in the plant matrix (K, Ca, Mg, and P). No interference was also observed with transition metals. Using a real sample (maize) with standard additions, decreases of recoveries were sometimes observed for 0.1% (m/v) NaOH, and attained 13.8% in the most unfavourable case. The final accuracy of the method was verified by using two certified reference materials: CRM 402 (white clover) and CRM 279 (sea lettuce). No statistically significant differences were obtained between the measured concentrations and the certified values. The optimized method was found sensitive (detection limit 0.15 μg l⁻¹), reliable and repeatable (R.S.D. between 1.3% and 4.0%).     

ICP-AES法测定方铅矿中多元素的方法研究

采用电感耦合等离子体原子发射光谱法(ICP-AES)进行方铅矿中多元素同时测定.通过对方铅矿样品化学处理试验建立了HCl-NH4Cl-HNO3的溶矿体系.本体系采用基体匹配、背景系数和元素干扰系数校正及元素内标法确定了最佳综合实验测试条件.本实验建立的ICP-AES法同时测定方铅矿中镉、钴、铜、铁、铟、铅、锌7种元素的方法,本方法测量相对误差RE (n=8)为1.50%～7.50%,相对标准偏差RSD (n=8)为1.7%～5.7%.经国家一级标准物质GBW 07269分析验证可以满足方铅矿单矿物样品的分析要求.