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1.
ICP-AES determination of trace elements after preconcentrated with p-dimethylaminobenzaldehyde-modified nanometer SiO2 from sample solution 总被引:1,自引:0,他引:1
A new method that utilizes p-dimethylaminobenzaldehyde-modified nanometer SiO2 (SiO2-p-DMABD) as a solid phase extractant has been developed for simultaneous preconcentration of trace Cr(III), Cu(II), Fe(III) and Pb(II) prior to the measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). The preconcentration conditions of analytes were investigated, including the pH value, the shaking time, the mass of sorbent, the sample flow rate and volume, the elution condition and the interfering ions. The adsorption capacity of nanometer SiO2-p-DMABD was found to be (mg g− 1) Cr(III): 6.2, Cu(II): 18.6, Fe(III): 4.7 and Pb(II): 6.0 at pH 4. The adsorbed metals were quantitatively eluted with 4 mL of 1.0 mol L− 1 HCl. According to the definition of IUPAC, the detection limits (3σ) of this method for Cr(III), Cu(II), Fe(III) and Pb(II) were 0.79, 1.27, 0.40 and 1.79 ng mL− 1, respectively. The proposed method achieved satisfied results when it was applied to the determination of trace Cr(III), Cu(II), Fe(III) and Pb(II) in biological and water samples. 相似文献
2.
V. N. Dwivedi P. L. Mahanta A. Premadas 《Journal of Radioanalytical and Nuclear Chemistry》2003,258(3):575-581
A procedure for the complete chemical analysis of magnesium or sodium diuranate (yellow cake) sample is reported. Uranium is determined gravimetrically after peroxide precipitation. Optimum parameters, such as pH, quantity of hydrogen peroxide, volume of sample, temperature and complexing agent for quantitave precipitation of uranium, and effective separation of other elements were studied. Aluminum, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, and Zn were determined by flame atomic absorption spectrometer and B, Mo, SO4, REEs and Y by inductively coupled plasma atomic emission spectrometer in the filtrates of hydroxide and peroxide precipitation separation. The proposed method is accurate and the precision is characterized by an RSD of ~0.2% for U; 2 to 6% for Mg, Na, K, Ca, Fe, SiO2, Al, Cd, Co, Cr, Fe, Mn, Ni, Pb, and Zn and 3 to7% for REEs, Y, Mo and B 相似文献
3.
Petru Jitaru Marco Roman Giulio Cozzi Paola Fisicaro Paolo Cescon Carlo Barbante 《Mikrochimica acta》2009,165(3-4):319-327
Silica gel and nanometer SiO2 modified with 4-(2-aminoethylamino)-N-(2-(2-aminoethyl amino)ethyl)butanamide (SG-AAEB and nanometer SiO2-AAEB), which were prepared based on chemical immobilization, were used as sorbents for the solid phase extraction of Cu(II), Fe(III), and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry. Adsorption efficiencies of the two sorbents towards metal ions were investigated by batch and column procedures. For both sorbents the preconcentration conditions of analytes including effects of pH, shaking time, sample flow rate and adsorption capacity, were investigated and compared. The differences of silica gel and nanometer SiO2 in sizes and surface structures resulted in distinct chemical activity and selectivity toward metals. At pH 4, the adsorption capacity of SG-AAEB was found to be 12.2, 14.5 and 9.8 mg g?1 for Cu(II), Fe(III), and Pb(II), respectively. In comparison, nanometer SiO2-AAEB showed a high selectivity toward Pb(II) and has a much larger adsorption capacity (22.3 mg g?1). Furthermore, the application of SG-AAEB and nanometer SiO2-AAEB for simultaneous preconcentration of trace Cu(II), Fe(III), and Pb(II) from natural samples was performed with satisfactory results. 相似文献
4.
A silica-based inorganic sorbent was synthesized by the thermal decomposition of ammonium heptamolybdate on silica and applied for the preconcentration and simultaneous determination of Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb in river water samples using a column system with flame atomic absorption spectrometry. Attenuated total reflection-Fourier transformation infrared spectroscopy, scanning electron microscopy, and electron dispersive spectroscopy were used for sorbent characterization. The effects of pH, sample volume, eluent type, eluent concentration, eluent volume, sample flow rate, and matrix ions (Al, Bi, Ca, Mg, and Zn) on the recovery of the metals in model solutions were investigated. The adsorption capacities (µmol g?1) of SiO2-MoO3 were 88.96 (Cd), 169.69 (Co), 153.85 (Cr), 188.88 (Cu), 179.05 (Fe), 163.81 (Mn), 136.31 (Ni), and 38.61 (Pb). The detection limits of the method were 9.09, 10.82, 10.77, 49.57, 31.64, 6.40, 8.86, 19.15?µg L?1 for Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb, respectively, with a preconcentration factor of 25. The developed method was used for the determination of the target metals in real samples and the recoveries for spiked samples were found to be from 91.2% to 102.9%. 相似文献
5.
P. Burba und K. H. Lieser 《Fresenius' Journal of Analytical Chemistry》1979,297(5):374-380
Zusammenfassung Spurenelemente in Mineralwässern werden auf kleinen Trennsäulen mit dem Celluloseaustauscher Hyphan abgetrennt, mit verdünnter Salzsäure eluiert, durch Schütteln an 100 mg Hyphan fixiert und durch energiedispersive Röntgenfluorescenzanalyse bestimmt. Folgende Schwermetalle werden quantitativ erfaßt, sofern sie in Konzentrationen 1 ppb im Wasser vorhanden sind: Mn, Fe, Co, Ni, Cu, Zn, Ta, Pb und U. Neben verschiedenen handelsüblichen Mineralwässern werden eine Natriumchloridsole und Meerwasser auf ihren Spurenelementgehalt untersucht. Die Ergebnisse der Röntgenfluorescenzanalyse und der Atomabsorption stimmen im Rahmen der Fehlergrenzen überein.
Energy-dispersive X-ray fluorescence analysis of traces of heavy metals (Mn, Fe, Co, Ni, Cu, Zn, Ta, Pb, U) in mineral waters after separation on the cellulose-exchanger hyphan
Summary Trace elements in mineral water are separated in small columns on the cellulose-exchanger Hyphan, eluted by diluted hydrochloric acid, bound on 100 mg of Hyphan by shaking and determined by energy-dispersive X-ray fluorescence. The following heavy metals can be analysed quantitatively if present in water in concentrations 1 ppb: Mn, Fe, Co, Ni, Cu, Zn, Ta, Pb and U. Several commercial mineral waters, a sodium chloride spring and seawater were analyzed for trace elements. The results obtained by X-ray fluorescence and by atomic absorption agree within the limits of error.相似文献
6.
X-ray fluorescence spectrometry (XRF) was applied to determine aluminium in AlCl3- and Al2O3-modified silica catalyst supports that were prepared by gas-solid reactions in an atomic layer epitaxy (ALE) process using
aluminium chloride or aluminium chloride and water as adsorbates and silica as support. INAA and AAS were used as reference
methods to determine the aluminium content of the supports. The calibration of XRF results was done by plotting the Al/Si
intensity ratios against the aluminium content as determined by atomic absorption spectrometry (AAS) and verified by instrumental
neutron activation analysis (INAA). Correlation factors for the calibration graphs were 0.984 for AlCl3/SiO2 and 0.995 for Al2O3/ SiO2 samples in the aluminium content range 0–2.6 g Al per 100 g of sample.
Received: 19 October 1998 / Accepted: 14 December 1998 相似文献
7.
X-ray fluorescence spectrometry (XRF) was applied to determine aluminium in AlCl3- and Al2O3-modified silica catalyst supports that were prepared by gas-solid reactions in an atomic layer epitaxy (ALE) process using
aluminium chloride or aluminium chloride and water as adsorbates and silica as support. INAA and AAS were used as reference
methods to determine the aluminium content of the supports. The calibration of XRF results was done by plotting the Al/Si
intensity ratios against the aluminium content as determined by atomic absorption spectrometry (AAS) and verified by instrumental
neutron activation analysis (INAA). Correlation factors for the calibration graphs were 0.984 for AlCl3/SiO2 and 0.995 for Al2O3/ SiO2 samples in the aluminium content range 0–2.6 g Al per 100 g of sample.
Received: 19 October 1998 / Accepted: 14 December 1998 相似文献
8.
M. Förster und K. H. Lieser 《Fresenius' Journal of Analytical Chemistry》1981,309(5):355-358
Zusammenfassung Die Spurengehalte an Pb, Cu, Zn, Fe und Ni in den Salzen NaCl, CaCl2, Al(NO3)3, ZnCl2, Mn(NO3)2 und Cr(NO3)3 des Reinheitsgrades p.A. wurden aus 10%igen Lösungen dieser Salze in einer mit dem Celluloseaustauscher 4-[Pyridil-(2)-azo]-resorcin (PAR) gefüllten Trennsäule quantitativ abgetrennt, mit Ausnahme von Eisen aus Al(NO3)3 und Cr(NO3)3 sowie von Nickel aus Mn(NO3)2. In der gleichen Weise wurden die genannten Schwermetalle aus den organischen Lösungsmitteln Methanol und Ethanol abgetrennt. Nach Elution der angereicherten Schwermetalle mit Salzsäure wurden sie an 0,1 g des Celluloseaustauschers fixiert und durch energiedispersive Röntgenfluorescenzanalyse oder direkt im Eluat durch flammenlose Atomabsorptionsspektroskopie bestimmt.
Determination of traces of heavy metals in inorganic salts and organic solvents by energy-dispersive X-Ray fluorescence analysis or flameless atomic absorption spectrometry after enrichment on a cellulose exchanger
Summary The trace element contents of Pb, Cu, Zn, Fe and Ni in the p.a. grade salts NaCl, CaCl2, Al(NO3)3, ZnCl2, Mn(NO3)2 and Cr(NO3)3 were quantitatively separated from 10% solutions of these salts in a column filled with the cellulose exchanger 4-[pyridil-(2)-azo]-resorcinol (PAR), with the exception of Fe from Al(NO3)3 and Cr(NO3)3 and of Ni from Mn(NO3)2. In the same way the heavy metals were separated from the organic solvents methanol and ethanol. After elution of the heavy metals from the column by HCl they were either fixed on 0.1 g of the cellulose exchanger and measured by energy-dispersive X-ray fluorescence analysis or they were determined directly in the eluate by flameless atomic absorption spectroscopy.
Dem Bundesministerium für Forschung und Technologie danken wir für finanzielle Unterstützung. 相似文献
9.
Trace elements (Mn, Fe, Co, Zn, Ni, Cu and Cr) were preconcentrated from sea water by retention on Chelex-100 resin, APDC/8-quinolinol complexation followed by extraction with 4-methyl-2-pentanon or Freon-113, or coprecipitation with Mg(OH)2 or Fe(OH)2. After consideratin of analytical blanks, extraction efficiency, precision preconcentration factor, and suitability for operation on board ship, the best results were obtained by preconcentrating Mn, Fe, Co, Zn, Ni and Cu on Chelex-100 resin and coprecipitation of chromium(III) and (VI) with Fe(OH)2. Graphite-furnace atomic absorption spectrometry and inductively-coupled plasma atomic emission spectrometry were used for the final measurements. The accuracy of the method was tested by using the reference sea water sample NASS-1. 相似文献
10.
《Analytical letters》2012,45(10):855-868
Abstract Background correction in atomic absorption spectrophotometry using a high temperature furnace has a close relation to the chemical treatment and the detection limit. Conventionally used for this correction is the D2 lamp method, but spectral interference is inevitable in this method because the spectral bandwidth of the light from the D2 lamp after passing through a monochromator is as wide as 0.1 to 5 nm. In the analysis of Sb in lead alloy or in steel, there is spectral interference due to high concentration of elements such as Pb, Cu or Fe, in the matrix, so accurate measurement is impossible unless these elements are removed at the pretreatment stage. In polarized analyte Zeeman atomic absorption spectrophotometry developed by the authors, the wavelength of the measuring beam is the same as that of the reference and they are identical in spectral line profile as well as in geometrical shape. They differ only in the direction of polarization. For these reasons, we found that there is no spectral interference like that recognized in the D2 lamp correction technique. As a result, a direct analysis was done simply by dissolving gunmetal or steel in acid without removing the matrix elements Pb, Cu or Fe. 相似文献
11.
T.M. Tuella A.H. Ullman B.D. Pollard A. Massoumi J.D. Bradshaw J.N. Bower J.D. Winefordner 《Analytica chimica acta》1979
The feasibility of using acid-treated metal powder standards for the determination of trace wear metals in spent jet engine oils is evaluated. The addition of 2:3:3 (v/v/v) HF—HCl—HNO3 mixture to used lubricating oils did not cause any statistically reliable differences from results obtained with organometallic standards. Two sets of six correlation samples, one set being acid-treated, were analyzed for Cu, Cr, Mg, Fe, Mo and V by flame atomic absorption and flame atomic fluorescence spectrometry against each set of standards. 相似文献
12.
Procedures based on flameless atomic absorption spectrometry are described for the determination of Cd, Co, Cr, Cu, Ni and Pb in mineral waters. Because of matrix effects and the inadequate detection limits for direct determinations, the metals are separated from the macrocomponents by precipitation of their tetramethylenedithiocarbamates with iron(III) as collector, or by co-precipitation on Fe(OH)3. The detection limits are 0.005, 0.3, 0.08. 0.10, 2 and 0.10 μg l- for Cd, Co, Cr, Cu, Ni and Pb, respectively, and are satisfactory for the determination of these elements in mineral waters. The precision is 2–7%. 相似文献
13.
14.
Xiaojun Zou Yuemei Cui Xiangbing Zhu Zheng Hu Xijun Chang 《Journal of Sol-Gel Science and Technology》2009,50(1):35-43
Morin was successful as a chemical modifier to improve the reactivity of the nanometer SiO2 surface in terms of selective binding and extraction of heavy metal ions. This new functionalized nanometer SiO2 (nanometer SiO2-morin) was used as an effective sorbent for the solid-phase extraction (SPE) of Cd(II), Cu(II), Ni(II), Pb(II), Zn(II) in
solutions prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions
for effective adsorption of trace levels of metal ions were optimized with respect to different experimental parameters using
static and dynamic procedures in detail. The pH 4.0 was chosen as the optimum pH value for the separation of metal ions on
the newly sorbent. Complete elution of the adsorbed metal ions from the nanometer SiO2-morin was carried out using 2.0 mL of 0.5 mol L−1 of HCl. Common coexisting ions did not interfere with the separation and determination at pH 4.0. The maximum static adsorption
capacity of the sorbent at optimum conditions was found to be 22.36, 36.8, 40.37, 33.21 and 25.99 mg metal/g SiO2-morin for Cd(II), Cu(II), Ni(II), Pb(II) and Zn(II), respectively. The time for 95% sorption for Cu(II) and Ni(II) and 70%
sorption for Cd(II), Pb(II) and Zn(II) was less than 2 min. The relative standard deviation (RSD) of the method under optimum
conditions was lower than 5.0% (n = 11). The procedure was validated by analyzing the certified reference river sediment material (GBW 08301, China), the results
obtained were in good agreement with standard values. The nanometer SiO2-morin was successfully employed in the separation and preconcentration of trace Cd(II), Cu(II), Ni(II), Pb(II) and Zn(II)
from the biological and natural water samples yielding 75-folds concentration factor. 相似文献
15.
E. Vassileva S. Arpadjan R. Stefanova V. Vassileva 《Fresenius' Journal of Analytical Chemistry》1990,336(7):582-585
Summary Different extraction sytems including long chain quaternary alkylammonium salts and APDC were investigated in order to determine the optimal conditions for extraction separation and preconcentration of traces of Ag, Bi, Cd, Cu, Fe, Mo, Pb, Sb and Zn from high purity NiSO4·6H2O, NiCl2·6H2O, Ni(OOCCH3)2·4H2O and Ni(NO)3)2·6 H2O. Best results for multielement preconcentration were found with the extraction system HCl-trioctylmethylammonium chloride-0,002 mol/l APDC/MIBK. The proposed method permits the flame atomic absorption determination of 5·10–6%, Ag, Cd, Cu and Zn, 1·10–5% Bi, Fe, Pb and 5·10–5% Mo and Sb with good accuracy and precision. 相似文献
16.
Petr Buryan 《Journal of Thermal Analysis and Calorimetry》2018,133(2):981-989
Blast furnace slag was leached using HCl to prepare lithium-based sorbents for CO2 capture, and chemical composition and phase of the acid leaching slag were determined by X-ray fluorescence analysis. The microstructure and morphology of both sorbents were characterized by scanning electron microscope and X-ray diffraction. The absorption capacity of both sorbents was observed non-isothermally and isothermally using thermogravimetric analysis, and 12 carbonation and calcination cycles were conducted to observe cycling stability. Controlling step of absorption process was determined by fitting the isothermal graphs using a double exponential model. The results show that 98.33% amorphous SiO2 can be obtained when the blast furnace slag was treated at 373 K for 10 h. Purified lithium-based sorbent by acid leaching slag (LBS-ALS) shows dense polyhedral particles with particle size between 25 and 120 μm. LBS-ALS shows similar absorption capacity with pure Li4SiO4 (P-Li4SiO4), but narrower absorption temperature range at non-isothermal absorption condition. The double exponential model fits well with the isothermal graphs for LBS-ALS and P-Li4SiO4, and diffusion of CO2 is the controlling step of the absorption process at lower temperature. LBS-ALS shows different controlling mechanism for desorption process compared with P-Li4SiO4. LBS-ALS maintains higher absorption capacity after 12 cycles in 100% CO2 flow. 相似文献
17.
以不同结构的SiO_2为载体,采用传统浸渍法,合成3种负载型的Cu/SiO_2.使用X射线衍射(XRD)、 N_2的等温吸-脱附、紫外漫反射光谱(DR UV-vis)、 X射线电子能谱(XPS)、等离子原子发射光谱(ICP)和H_2的程序升温还原(H_2-TPR)方法对样品进行表征.考察了以H_2O_2为氧化剂,样品对苯酚直接羟基化合成苯二酚的催化性能.结果表明:具有介孔和MFI结构的二氧化硅(MS-1),稳定性强,有利于引入Cu物种在其孔内扩散及分布,形成更多的高分散CuO.一定反应条件下, Cu/MS-1催化活性最高,苯二酚的收率和选择性分别高达38.91%和81.5%. Cu/MS-1催化剂重复使用10次后,苯二酚的收率为37.64%,而Cu含量仅从2.5%变为2.1%,具有较强稳定性;高分散CuO是目标反应的主要活性物种. 相似文献
18.
M. Schmeling F. Alt R. Klockenkämper D. Klockow 《Analytical and bioanalytical chemistry》1997,357(8):1042-1044
Total reflection X-ray fluorescence spectrometry was applied for the certification of IAEA lichen-336. The elements Ca, Mn,
Fe, Cu, Zn, Rb, Sr and Pb were determined simultaneously. The concentrations range from 1.8 mg/kg for Rb to 2360 mg/kg for
Ca. The results were compared with those of other methods and laboratories having participated in this certification for the
International Atomic Energy Agency (IAEA): emission spectrometry, mass spectrometry, atomic absorption spectrometry, X-ray
spectrometry, neutron activation analysis and voltammetry. The results determined by TXRF are in good agreement with the overall
means of accepted values and differ from the means by 1 to 10%.
Received: 1 September 1996/Revised: 15 October 1996/Accepted: 22 October 1996 相似文献
19.
The determination of five elements in filter papers loaded with air particulate matter has been investigated. After a wet destruction of about 10 cm2 of filter material by a standard procedure, analysis was carried out with a flame atomic absorption method for zinc and a flameless procedure for Cd, Cu, Fe and Pb. Furnace program parameters for each of the elements in different acid solutions are reported. The interferences of some common anions and the most abundant cations in aerosol material are described. For some urban and industrial samples, the results are compared with those obtained by energy-dispersive x-ray fluorescence. Accuracy was checked against standard samples. 相似文献