A three-step metal fractionation scheme for fly ashes collected in an Argentine thermal power plant

A new three-step fractionation scheme was applied to study the distribution of Al, As, Cd, Cr, Cu, Fe, Mn, Mo, Ni, Pb, S, Sb, Ti, V and Zn in fly ashes collected in the electrostatic precipitator of a thermal power plant in the city of San Nicolás (Argentina). Seven samples were collected during one week of operation in 2005. For the fractionation, the scheme applied consisted of extracting the elements in three fractions: (i) soluble and exchangeable elements, (ii) carbonates, oxides and reducible elements and (iii) residual elements. Metals and metalloids at μg g⁻¹ level were determined in each fraction by plasma based techniques namely, inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). For validation, a certified reference materials NIST SRM 2711 (Montana soil) was subject to the same chemical sequential extraction procedure. X-ray diffraction powder (XRD) analysis and scanning electron microscopy (SEM) were used to characterize the major minerals present in the matrix. The predominant phases found in the total samples were mullite, quartz, iron oxides and lime. Total analyte concentration varied (in μg g⁻¹) from 1.54 for Cd to 30 600 for Al. The leachability of the 15 elements under study proved to be different. All the elements (except Cd and Pb) were detected in the soluble fraction in the order: Cu (0.10%) ∼ Mn (0.13%) < Ni (0.17%) ∼ Ti (0.19%) ∼ Fe (0.20%) ∼ As (0.21%) < Zn (0.86%) < Al (1.3%) < Cr (2.9%) < V (3.9%) < Sb (6.9%) < Mo (45.1%) < S (58.0%). Percentages higher than 20% of S (24.1%) < V (27.5%) < Mn (29.0%) were detected in the second fraction. Al, As, Cr, Cd, Cu, Fe, Ni, Pb, Sb and Zn were mostly associated to the residual fraction. Recoveries of the overall procedure varied between 106% (Mo) and 72% (Cr).     

应用ICP-MS同时测定矿泉水中22种微量金属

研究结果表明应用ICP-MS可以同时测定饮用天然矿泉水中的Li、Be、B、Al、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、Ge、As、Se、Sr、Mo、Ag、Cd、Sb、Ba、Pb、等微量金属元素.ICP-MS法具有快速、准确、处理简单、干扰少等优点.     

Content, mobility and transfer behavior of heavy metals in MSWI bottom ash in Zhejiang province, China

Municipal solid waste incinerator (MSWI) bottom ash samples were taken from six cities of Zhejiang province, where 1/4 incinerators of China were located. The samples were instrumentally analyzed to detect the content of heavy metals. Sequential extraction procedure (SEP) was adopted to characterize the mobility and environmental impact of heavy metals. And the transfer coefficients of heavy metals from the input MSW to the bottom ash during the incineration were also calculated. It showed that the average content of Zn, Mn, Cu, Pb and Cr in the bottom ash exceeded 300 mg/kg, which was much higher than that in the soils. SEP results showed that although the residue fraction was the primary fraction of the heavy metals in the bottom ash, there were still 1.84 mg of Cd, 86.21 mg of Cu, 83.46 mg of Pb and 939.46 mg of Zn in 1 kg bottom ash having the potential of leaching, which indicated a great threat to the surrounding environment. The result of coefficients calculation revealed that almost all the Cu, Cr, Mn and Ni in the input MSW were transferred to the bottom ash during the incineration. Bottom ash was also the main destination of Cd, Co, As, Mo, Pb and Zn though considerable amounts of those metals were transferred to the raw gas.     

Trace metal contents of acidic,basic and neutral components of a cyclohexanol extract of Kosova Basin lignite

A sample of Kosova Basin lignite was extracted with cyclohexanol. The yield of extract was 19.98 wt%. The extract was fractionated into acidic, basic and neutral components and benzene- and petroleum ether-insoluble fractions. After ashing with HClO₄ and HNO₃, eleven elements (K, Ca, Mg, Fe, Pb, Zn, Cu, Mn, Cr, Cd and Ni) were analysed by atomic absorption spectroscopy and seven elements (Al, Ba, Sr, Be, B, Ga and V) by inductively coupled plasma optical emission spectroscopy. A majority of the elements (Fe, B, Al, Zn, Pb, Cu, Ca, Mg, Sr, Ga and V) were found concentrated in the acidic and phenol fractions, while K, Ni, Ga and Cu predominated in the amine fraction. The metals thus analysed were associated with heteroatoms.     

ICP-AES法快速测定青菜中14种元素的含量

研究了微波消解样品,电感耦合等离子体原子发射光谱(ICP-AES),快速测定青菜中K、Na、Ca、Mg、Fe、Mn、Cu、Zn、Pb、Cd、Cr、Ba、As、Ni等14种常量元素和微量元素。方法操作简便,分析速度快,结果令人满意,该方法也可用于农副产品中上述元素的同时测定。     

ICP-MS法测定注射用双黄连(冻干)无机阳离子的含量

注射用双黄连(冻干)样品经微波消解后,利用电感耦合等离子体质谱(ICP-MS)测定其中B、Al、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Cd、Ba、Hg等15种微量元素的含量。结果表明,方法回收率为81.6%～96.3%,检出限为0.001～1.53 ng/g,方法快捷、准确、灵敏度高,可以用于注射用双黄连(冻干)的微量元素的测定,同时也进一步完善了注射用双黄连(冻干)无机元素分析,为其质量控制提供了参考依据。     

原油电脱盐废水中多种金属元素的快速测定

采用微波消解/电感耦合等离子体质谱(ICP-MS)法分析了炼油厂原油电脱盐废水中Be、V、Cr、Mn、Co、Ni、Cu、Zn、As、Se、Mo、Ag、Cd、Ba、T1、Pb、Hg共17种金属元素的含量,样品采用硝酸和过氧化氢消解,上述17种金属元素的仪器检出限(IDL)为0.4～ 215 ng/L,标准样品分析的相对标...     

微波消解-ICP-OES法测定黑芝麻中的18种矿质元素

采用HNO3/H2O2湿法微波消解制样,利用全谱直读电感耦合等离子原子发射光谱法(ICP-OES),全面详细地分析测定了黑芝麻中的矿质元素,共检出Ca、P、S、Mg、K、Al、Si、Fe、Na、Zn、Se、Sr、Cu、Mn、Ba、B、Ti、Cr等18种矿质元素,RSD值在1.21%～10.1%,其中13种元素在5%以内。黑芝麻中所含人体常量元素Ca、P、S、Mg、K、Na等的质量分数分别为1.79%,1.08%,0.59%,0.43%,0.41%和0.009 1%;微量元素Fe、Zn、Se、Cu、Mn、B、Cr、Sr、Si、Al等的含量分别为18.6,4.55,3.87,1.74,1.62,0.91,3.21,78.8,125.8 mg/100 g,未检出Pb、Hg、Cd、As以及Ni、Co、Mo等元素。     

中低温煤焦油蒸馏过程中金属元素的迁移规律

以中低温煤焦油轻油和重油为实验原料,采用常压蒸馏获得170~200℃、200~240℃、240~270℃、270~300℃、300~320℃、320~340℃、340~360℃和360~390℃煤焦油馏分油;利用配有油品加氧制冷进样系统的ICP-OES测定了21种微量元素在馏分油中的含量,考察了不同馏分油中元素的分布情况。研究表明：在原煤焦油中,未发现Ag、Mg、Mo、Na、Ni、Fe、Mn、Cr及Ti元素,含量较高的元素有Sn、P、Al、Pb、Si,其中Sn元素在轻油和重油中的含量分别为11.78μg/g和14.04μg/g;在所有馏分油中,未发现Al、Mo、Fe、Mn、Cr及Ti元素,含量比较高的元素有Si、Sn、Na、Zn、Pb,特别是Si、Na、Sn、Zn、Ni、Pb及B元素可以有效富集于馏分油中。可能的原因是Ca、Fe、Mg、Al等金属以不同的盐类形态存在,在煤焦油脱水及<170℃蒸馏过程中,这些金属盐类会被部分带出,导致其在馏分油中的含量未富集或未检出;通过关联金属元素在馏分油中的分布与其组成的关系,馏分油中元素的分布可能与酚类化合物、杂环化合物和蒸馏温度等相关。酚类化合物及杂环化合物可能与Ag、B、Cu、Mo、Sn、Na、Zn、Ca、Pb等金属形成络合物或卟啉配合物,蒸馏温度一方面可以破坏Sn、Cd、Pb、Zn、Cu、Ca、Pb等元素在馏分油中的结合力,另一方面也可以促进这些元素与馏分油中的含氧、含氮等化合物更好地发生化合反应,进而影响金属元素在馏分油中的含量分布。     

The development of a digestion procedure for the determination of metals in gum obtained from deposits in internal combustion engines by ICP-OES

The accurate determination of metals in gum (deposits found in internal combustion engines) is strongly influenced by a selection of the right sample digestion method. The difficult and heterogeneous nature of this kind of sample, and its unpredictable reaction behavior are the major obstacles in getting correct analytical results. The studies were implemented with one sample called “reference sample”. Two digestion procedures were tested in this work. The dry ashing procedure was followed by another dissolution procedure with HF and heating, in order to complete the dissolution of the ash in the samples. The process was performed in 36 h. The second digestion procedure was implemented in closed system (pressurized) with 2 mL of HNO₃ and 2 mL of H₂SO₄. This last one presented a reduction of 80.5% time-consuming in relation to the first one (dry ashing). Al, Ca, Cd, Cr, Cu, Fe, K, Mg, Na, Ni, Pb, Si, and Zn were determined in 14 samples of gum by ICP-OES. The wet closed system digestion procedure showed efficiency in the Cr, Cu, Fe, K, Ni, Pb, Si, and Zn determination. The correlation matrix results contribute to the characterization studies of the gum formation process, as well as the corrosion of the motor parts and fuel quality control.     

Trace metal distribution in fractions of solvent-refined coal by ICP-OES and implications regarding metal speciation

Separations of Amax solvent-refined coal according to its acid/base/neutral components and by selective elution from a silica column (SESC) to yield nine fractions have been carried-out. After ashing with H₂O₂-H₂SO₄, twenty metals (Mg, Al, P, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Mo, Cd, Sr, Zr, W, Hg and Ba) were analysed by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). A majority of elements (Zn, Cd, Hg, Cr, Mo, W, and Fe) were found concentrated in the acid fraction while Co, Ni and Cu preferred the neutral and base fraction. In the step gradient SESC fractions, the greatest concentration of metal was found in fractions that had been characterized as enriched with phenols.     

ICP-OES测定玩具新指令第三类物质17种可迁移元素

本实验通过试验,对ICP-OES仪器工作条件进行了选择和优化,建立了ICP-OES测定欧盟玩具安全新指令限制第三类物质的17种可迁移元素（铝、锑、砷、钡、硼、镉、铬、钴、铜、铅、锰、汞、镍、硒、锶、锡、锌）的方法。本方法的检出限低,选取的第三类物质：涂层、聚合物、纸张、纺织品、金属、木材等多种材料的平均回收率均在94%~109%。结果显示方法有良好的准确度。     

Concentration of trace elements in arable soil after long-term application of organic and inorganic fertilizers

The Ruzyně Fertilizer Experiment (RFE, the Czech Republic) was established on a permanent arable field (illimerized Luvisol) in 1955. The effects of long-term application of several organic fertilizers (dung water, farmyard manure, poultry litter) and mineral N, P and K fertilizers on plant-available (extracted by CaCl₂), easily mobilizable (extracted by EDTA), potentially mobilizable (extracted by HNO₃) and total concentrations of trace elements were investigated in 2008. Concentrations of all analyzed trace elements in the applied fertilizers did not exceed the limits permitted by Czech national legislation. Concentrations of As, Cd and Cr were highest in single superphosphate, those of Cu, Mn and Ni were highest in poultry litter and those of Pb and Zn were highest in dung water. Poultry litter had the second highest concentration of As and Zn. Poultry litter supplied the soils with considerable amounts of Cu, Mn and Zn and increased their concentrations in the soil. There was also a significant increase in plant availability of Mn, Ni and Zn and a decrease in soil pH. Although all fertilizers were applied for five decades, total concentrations of As, Cr, Cu, Ni, Pb and Zn in soil remained far below Czech legislation limits. For Cu and Zn this was probably due to the relatively low mean annual application rates of poultry litter. Total Cd concentrations in soil exceeded the legislative limit even in the control (without any fertilizer inputs) and the effect of treatment was not significant. This indicates that fertilizers were not the main source of Cd in the experimental area. Therefore, common cropping practices do not induce soil contamination by trace elements even if they have been applied for more than 50 years.     

电感耦合等离子体质谱法( ICP-MS)测定地下水中痕量元素

用电感耦合等离子体质谱法(ICP-MS)测定了地下水中痕量元素(Cd、Co、Cr、Cu、Mn、Mo、Ni、Pb、As、Se、Zn、Ba、Fe),应用在线加入内标校正干扰效应,元素检出限为0.002-0.179 μg,/L,加标回收率为96.50 ％～103.10％,相对标准偏差(RSD)＜2.31％.试验结果表明该法测...     

REACTION BETWEEN METALS AND MOLTEN GLASS *

A series of melts of soda-lime-silica glass cullet in contact with various chemical elements was made to determine by observation the extent of the reaction between metal and glass. The heat treatment consisted of a period of two hours at about 1250°C. An atmosphere of hydrogen gas was used to protect the element from oxidation during the the test period. Various colors were produced by Cu, Ag, Au, Se, C, S, and Zr. Black fogs resulted from melts containing Ba, Cr, or V; gray or black fogs with reddish zones resulted from Mg, Ca, Ti, Mn, Si, and Al. A faint blue with large reddish zones was produced by Co. Only slight attack was shown by Fe, Ni, Zn, Cd, Bi, Sn, Pb, Mo, and W.     

Development of a microwave-assisted digestion method using ICP-OES to measure metals in gum deposits of internal combustion engines

The heterogeneous nature of gum samples obtained from the deposits of internal combustion engines is the main difficulty in accurate determination of their metal content. A microwave-assisted digestion method was implemented using factorial experimental design. The optimization of this procedure was carried out by first evaluating the effects of variables on the response (i.e., the residual carbon content or RCC). The variables of maximum heating power, heating time and nitric acid volume were studied. The RCC response was measured by inductively coupled plasma optical emission spectrometry (ICP-OES). The time of maximum heating power was essential to obtain a desired RCC. The surface response was constructed with optimal conditions presented at 6 min and heating power of 700 W. Amounts of aluminum (Al), calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), nickel (Ni), lead (Pb) and zinc (Zn) were determined in 26 gum samples by ICP-OES. Ca, Fe, Mg and Zn were found at mg g⁻¹ levels in the samples, while Al, Cu, Mn, Ni and Pb were found at mg kg⁻¹ levels. Principal component analysis (PCA) was used to establish a correlation between the gum samples and the different metal contents. Three distinct groups were separated according to the characteristics of the collected samples.     

X射线荧光光谱法测定土壤样品中C和N等30个主次痕量元素

采用PVC环的粉末样品压片制样,用RIGAKU ZSX Primus Ⅱ型X射线荧光光谱仪对土壤样品中的C、N、Na2O、MgO、Al2O3、SiO2、P、S、Cl、K2O、CaO、Ti、V、Cr、Mn、TFe2O3、Co、Ni、Cu、Zn、Ga、Nb、Zr、Y、Sr、Rb、Pb、Th、Ba和Br等30个组分进行测定.重点研究了C、N、Cl、S等元素的测定条件、痕量元素的背景选择和谱线重叠校正问题.使用经验系数法和康普顿散射线、背景散射线作内标校正基体效应.经国家一级标准物质校验,方法的检出限、精密度和准确度,满足多目标地球化学调查样品的分析要求.     

合肥市南淝河表层沉积物重金属污染评价

对合肥市南淝河表层沉积物中重金属污染状况进行采样调查,选取了8个采样点,测定了沉积物中Cr、Cd、Pb、Ni、Zn、Cu 6种重金属的含量,并采用地质累积指数法和Hakanson潜在生态风险指数法对其污染程度进行分析评价。地质累积指数评价结果表明:南淝河6种重金属的生态风险等级由强至弱依次为Cd、Zn、Cu、Ni、Pb、Cr;生态风险指数评价结果显示:在南淝河沉积物重金属中,Cd存在一定的潜在生态风险,Cr、Pb、Ni、Zn、Cu均处于轻微等级,重金属生态风险等级由强至弱依次为Cd、Cu、Ni、Pb、Zn、Cr,多数采样点的沉积物重金属综合潜在生态风险等级处于轻微级,个别采样点达到了中等甚至强生态风险等级。     

Solvent-free liquid phase oxidation of benzyl alcohol to benzaldehyde by molecular oxygen using non-noble transition metal containing hydrotalcite-like solid catalysts

Performance of Co–Al, Ni–Al, Cu–Al, Zn–Cu–Al, Mg–Fe, Co–Fe, Ni–Fe, Mn–Cr, Co–Cr, Ni–Cr, Zn–Cr and Cu–Cr hydrotalcite-like solid catalysts has been evaluated for the liquid phase oxidation of benzyl alcohol to benzaldehyde using molecular oxygen as an oxidizing agent in the absence of any solvent. The Mn and Cu containing hydrotalcite-like solids show good catalytic activity in the oxidation and hence these are promising catalysts for the solvent-free oxidation reaction.     

ICP-AES测定土壤中的重金属

样品经加热酸消解,以ICP-AES测定其中的铜、锌、镍、铅、镉、铬。采用该方法测定土壤样品中的铜、锌、镍、铅、镉、铬,前处理操作过程简便,设备简单,成本低廉。实验结果表明,采用该法测定土壤中的重金属时,测定结果准确可靠,重复性好。