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1.
A flow injection online displacement solid-phase extraction (DSPE) via magnetic immobilization of mercapto-functionalized magnetite microspheres onto the inner walls of a knotted reactor (KR) coupled with inductively coupled plasma mass spectrometry was developed for selective preconcentration and determination of trace noble metals (Ru, Rh, Pd, Pt, Ir and Au) in complex matrices. Online DSPE of 2.7 mL aqueous solution gave the enhancement factors of 32-46 for the six noble metals in comparison with direct nebulization of aqueous sample solution, and the detection limits (3 s) of 2.1 ng L(-1) for Ru, 1.9 ng L(-1) for Rh, 2.5 ng L(-1) for Pd, 1.8 ng L(-1) for Ir, 1.9 ng L(-1) for Pt and 1.7 ng L(-1) for Au. The sample throughput of the developed method was about 20 samples h(-1), and the relative standard deviation for eleven replicate determinations of the noble metals at the 30 ng L(-1) level ranged from 1.2% to 2.1%. The recoveries of Ru, Rh, Pd, Pt, Ir and Au still maintained 90% even after successive 140 cycles of DSPE. The developed method was successfully applied to selective determination of trace Ru, Rh, Pd, Pt, Ir and Au in complex matrices. 相似文献
2.
Determination of Pd,Rh, Pt,Au in road dust by electrothermal vaporization inductively coupled plasma mass spectrometry with slurry sampling 总被引:1,自引:0,他引:1
Inductively coupled plasma mass spectrometry coupled with ultrasonic slurry sampling electrothermal vaporization (USS-ETV-ICP-MS) has been applied to determine Pd, Rh, Pt and Au in 0.5% m/v slurries of several road dust samples. 2% m/v ammonium pyrrolidine dithiocarbamate (APDC) was used as the modifier to enhance the ion count. The influence of instrument operating conditions, slurry preparation and interferences on the ion count was reported. This method has been applied to the determination of Pd, Rh, Pt and Au in BCR 723 Road Dust and NIST SRM 2709 San Joaquin Soil reference materials and two road dust samples collected locally. The analysis results of the standard reference materials agreed with the certified values. Precision between sample replicates was better than 10% for all the determinations. The method detection limits estimated from standard addition curves were 0.9, 0.4, 0.6 and 0.4 ng g−1 for Pd, Rh, Pt and Au, respectively, in original dust samples. 相似文献
3.
N.N. Fedyunina I.F. Seregina K. Ossipov A.S. Dubenskiy G.I. Tsysin M.A. Bolshov 《Analytica chimica acta》2013
The reversible sorption preconcentration of noble metals (NMs) using different schemes “sorbent–reagent–eluent” was investigated. The extraction of Au, Pd, Pt, Ir, Rh and Ru chlorocomplexes from hydrochloric acid solutions on hyper-crosslinked polysterene MN-200 in the form of ion associates with tributylamine (TBA) and 4-(n-octyl)diethylenetriamine (ODETA) was investigated. It was found that Pd, Pt and Au were quantitatively and reversibly extracted using TBA on hyper-crosslinked polysterene; the appropriate eluent for desorption was 1 M solution of HCl in ethanol. Ir, Rh and Ru under these conditions were not sorbed quantitatively. It was found that sorbent hydrophobicity is not the main characteristic that defines the efficiency of sorption of a particular NM ion associate. Different efficiencies of hyper-crosslinked polysterene MN-200 for sorption of square-planar chlorcomplexes of Pt, Pd and Au and octahedral complexes of Ir, Rh and Ru were found. For the first time, the sorbents with their own N-atoms – StrataX and StrataX-AW – were used for the sorption of Ir, Rh and Ru. Using these sorbents, the sorption of Ir was increased up to 95%, and the sorption of Ru and Rh was increased to about 40%. We can explain these results by nonspecific interaction of chlorcomplexes of Ir, Rh and Ru with ethylenediamine groups of the sorbent. Weak bases with large anions may be applied for desorption of Ir, Rh and Ru. Two schemes of dynamic sorption preconcentration of NMs from hydrochloric acid solutions were proposed – hyper-crosslinked polysterene MN-200 for the determination of Au, Pd, Pt, and StrataX-AW for Ir, Rh and Ru. 相似文献
4.
《Spectrochimica Acta Part B: Atomic Spectroscopy》1996,51(5):543-548
Trace determination of Au, Rh, Ir, Pd and Pt in pure water solution has been performed by electrothermal atomization-laser induced fluorescence (ETA-LIF). Limits of detection obtained are in the ng/l−1 range, improving previously published absolute limits of detection by one or two orders of magnitude. The day to day reproducibility for iridium is around 8%. Thus, the ETA-LIF technique can be used routinely for the determination of precious metals at ultratrace concentrations. 相似文献
5.
Tikhomirova TI Fadeeva VI Kudryavtsev GV Nesterenko PN Ivanov VM Savitchev AT Smirnova NS 《Talanta》1991,38(3):267-274
A study has been made of the sorption of Ir(IV), Rh(III), Pt(IV), Ru(IV), Os(VIII), Pd(II) and Au(III) from aqueous solutions by silica chemically modified with nitrogen-containing organic ligands, as a function of hydrochloric acid concentration, time of contact, concentration of the element and the ionic strength. Sorption of noble-metal ions at pH > 1 on a sorbent containing monoamine groups seems to be due to a complexation mechanism, and to an anion-exchange mechanism at pH < 1. With aminopropyl-silica 1000-fold concentration of Ir(IV) and Rh(III) from their 10(-8)-10(-7)M solutions was achieved and these metals were subsequently determined on the sorbent surface by X-ray fluorescence. Detection limits were 10-20 ng/ml. There was no interference from 1000-fold quantities of non-ferrous metal ions and Fe(III). With the sorbent containing bonded diethylenetriamine groups, 1000-fold concentration of Au(III) was achieved, and it was then determined on the sorbent surface by an atomic-emission method. Conditions for desorption of Au(III) with pyridine and potassium thiocyanate were developed. 相似文献
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The ion chromatography of chloro complexes of Au(III), Ir(IV), Ir(III), Os(IV), Pd(II), Pt(IV), Rh(III) and Ru(III) was investigated using anion-exchange and ion-interaction techniques involving silica-based phases. Chloride was either absent or at a very low level and the pH was high enough to enable steel-fabricated liquid chromatography equipment to be used. With anion exchange, Ir(IV), Ir(III), Os(IV) and Pt(IV) gave good stable chromatography and all produced linear calibration plots, except Ir(IV) owing to instability of the sample solution. The detection limits were Ir(III) 5, Os(IV) 10 and Pt(IV) 2 ng ml?1. The ion-interaction technique was not so successful, only Au(III) and Pd(II) giving stable chromatography. The calibration plots were slightly curved, although acceptable, and the detection limits were 10 and 30 ng ml?1 for Au (III) and Pd(II), respectively. 相似文献
8.
Vasilyeva AA Yudelevich IG Gindin LM Lanbina TV Shulman RS Kotlarevsky IL Andrievsky VN 《Talanta》1975,22(9):745-749
The extraction of Pt, Pd, Ir, Rh, Ru, Ag, Au, Co, Cu, Ni and Fe with n-octylaniline has been investigated. Noble metals are extracted 10(3)-10(4) times better than Cu, Ni, Co and Fe. A method of determination of Pt, Pd, Ir, Rh and Ru is proposed. They are first separated from Cu, Ni, Co and Fe by means of extraction (and then determined, in either the aqueous or organic phase, by atomic-absorption spectrophotometry. The atomic absorption of platinum metals (with the exception of Pd) is affected by other elements of the platinum group and by non-noble metals. La(NO(3))(3) and Nd(NO(3))(3) lower the limit of detection for Pt, Rh, Ir and Ru and inhibit the effect of Co, Cu, Ni, Fe, Bi, Zn, Na, etc. on their determination. Lanthanum and neodymium chlorides and sulphates produce a similar effect but only on the determination of Pt and Rh. The coefficient of variation of the determination, in both phases, is within 2-6.8%. 相似文献
9.
Nguyen Van Suc 《Journal of Radioanalytical and Nuclear Chemistry》1994,187(1):67-71
A procedure for separation of Au, Ag, Pt, and Pd in geological samples has been developed. After irradiation, samples were fused with Na2O2 and silver was separated by filtering through a PbCl2 filter in 4M nitric acid solution. Au, Pt and Pd were concentrated with rhodium and thiourea as rhodium sulfide and the separation process of these elements was carried out by a chromatographic method. Au, Pt and Pd were retained on a Dowex-1×8 anion column in 1M HCl. Pd was eluted from the column by using a mixture of 75% HCl acid-25% acetone. Au was eluted by using a mixture of 10% HCl-90% acetone. In the gold fraction, Pt was also determined through the photopeak of199Au radionuclide (158 keV). The method was simple and rapid. 相似文献
10.
Ivanka St. Markova 《Fresenius' Journal of Analytical Chemistry》1988,332(1):11-16
Summary Spectral interferences associated with the determination of trace contents of Au, Ag, Pt and Pd in samples with complex matrices (hydrometallurgical solutions, metallurgical products and ore processing products) were investigated. It was found that it is necessary to separate Au, Pt and Pd from the matrix elements. The results obtained with various methods for separation and pre-concentration of these elements showed that in the case of hydrometallurgical solutions adsorption on activated carbon satisfies the requirements of analytical control. For the determination of these elements in ore processing products it is necessary to use additional extraction for their preconcentration. The most suitable organic solution found for the extraction of Au, Pt and Pd and their determination with ICP is isoamyl alcohol. 相似文献
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A method for determining Au, Pt, Pd, Ir and Rh in ores and silicates and Fe-formation rocks is described. Sample decomposition was carried out with aqua regia and HF, followed by fusion of any insoluble residue with Na22O2 in a glassycarbon crucible. The precious metals were separated, in 1.2 mol dm−3 HCl media, from the matrix elements by ion-exchange, using a mini-column with tetraethylenepentamine (metalfix-chelamine) resin. The resin was destroyed with HNO3 and H2O2 in a high-pressure vessel assisted by microwave heating, and the precious elements were determined by flow-injection inductively coupled plasma mass spectrometry. The sample treatment, optimization of analytical variables and measurable concentration levels are discussed. The limits of quantification (10 sdn − 1) calculated from a procedural blank sample solution were 4.0, 2.0, 1.5, 0.8 and 0.5 ng g−1 for Au, Pt, Pd, Ir and Rh, respectively. The accuracy of the proposed method was tested by determining these elements in SARM 7 platinum-ore reference material. For all the analytes, the relative standard deviation of the combined dissolution, separation and determination methods was below 3.5% (n = 6). 相似文献
13.
The anionic chlorocomplexes of Au(III), Pt(IV), Pd(II), Ir(IV), Ir(III) and Rh(III) can be floated from aqueous solutions with cationic surfactants of the type RNR'3Br. The flotation behavior of each metal is reported with respect to variations of hydrochloric acid and sodium chloride concentrations, the R and R' chain lengths, initial surfactant concentrations and initial metal ion concentrations. The flotation behavior of the metals is compared to the anion-exchange selectivity coefficients and a flotation selectivity sequence of Au(III) > Pt(IV), Ir(IV), Pd(II) > Ir(III) > Rh(III) is generally observed. Nearly 100% of Au(III), Pt(IV), Ir(IV) and Pd(II) can be recovered from dilute solutions using the ion flotation procedures. 相似文献
14.
A number of aliphatic mono- and triamines have been investigated as potential reagents for solid phase extraction of Rh, Pd and Pt. Platinum group metals are recovered from hydrochloric acid solutions as ionic associates of their chloride complexes with protonated amines. The recovery of metals depends both on hydrophobic properties of amine and sorbent and on sorption behaviour of amine itself. For on-line solid phase extraction of platinum group metals 4-(n-octyl)diethylenetriamine and hyper cross-linked polystyrene sorbent SSPS have been applied. Quantitative recovery of rhodium and platinum in the form of their hexachloride complexes was achieved under non-equilibrium conditions of on-line dilution. Metals recovered are quantitatively eluted with 1 M hydrochloric acid solution in ethanol. A new FIA-FAAS method for the determination of Rh, Pd and Pt in solutions based on the decomposition of ores and alloys has been proposed. The RSD values are 0.03-0.08 at 50-ppb concentration level. The detection limits are 3-8 ppb for 1 min of preconcentration. The accuracy of the procedure was verified by the analysis of standard reference materials of sulfide ores and alloys. 相似文献
15.
利用密度泛函理论系统研究了贵金属原子(Au、Pd、Pt和Rh)在CeO2(111)表面的吸附行为。结果表明,Au吸附在氧顶位最稳定,Pd、Pt倾向吸附于氧桥位,而Rh在洞位最稳定。当金属原子吸附在氧顶位时,吸附强度依次为Pt > Rh > Pd > Au。Pd、Pt与Rh吸附后在Ce 4f、O 2p电子峰间出现掺杂峰;Au未出现掺杂电子峰,其d电子峰与表面O 2p峰在-4~-1 eV重叠。态密度分析表明,Au吸附在氧顶位、Pd与Pt吸附在桥位、Rh吸附在洞位时,金属与CeO2(111)表面氧原子作用较强,这与Bader电荷分析结果相一致。 相似文献
16.
The sensitivities for the determination of 19 elements from Z = 44 to Z = 82, by means of 10-MeV proton activation, have been calculated from experimentally measured yields for 51 radioisotopes obtained mainly via (p,n) reactions. For an irradiation of 1 h at a beam current of 1 μA, the sensitivities established experimentally are about 0.02–2 p.p.m. for Ru, Pd, Ag, Cd, Sn, Sb, Te and I, 0.5–100 p.p.m. for In, W, Re, Ir, Pt, Au, Hg, Tl and Pb, and 15–900 p.p m- for Rh and Ba. Experimental results for the non-destructive analysis of these 19 elements in Al, Ag, Au, Co, Dy, Ho, Ir, Nb, Pr, Rh, Si, Ta and Tb, are presented. 相似文献
17.
Binary mixtures of Pt and Rh, Pt and Ir, Pd and Rh. and Pd and Ir were resolved by a countercurrent extraction technique. The metals were partitioned between an acidic aqueous phase containing potassium thiocyanate and an organic phase, n-tributylphosphate. Distribution coefficients were determined for each metal for a thiocyanate: metal mole ratio of 10 : 1 and 200 : 1 at pH values of 1, 2, 3, and 3.8. Optimum conditions for separations were determined to be a thiocyanate; metal mole ratio of 10 : 1 and a pH of 1. Under these conditions the Kd values tor Pd, Pt, Rh and Ir were 139, 62.3, 0.19 and 0.09 resp. Effective separations were achieved with each binary mixture on a Craig extraction apparatus utilizing less than 10 equilibrium stages. There was a 95% average recovery of each of the metals. 相似文献
18.
B. Hołyńska S. Kalita M. Lankosz A. Markowicz M. Wasilewska 《Journal of Radioanalytical and Nuclear Chemistry》1977,35(2):361-371
Radiometric methods of determination of platium and palladium (0.1 to 5% of Pt and 0.1 to 2% of Pd), gold and indium (0.01 to 1% of Au and 1 to 4 g In/l) and of platinum and rhodium (0.1 to 9% of Pt and 0.05 to 1% of Rh) in aqueous solution has been worked out. A suitable measuring device has been designed and constructed. The methods are based on the measurement of characteristic radiation of the Lα line for gold and platinum and of the K-series for indium, palladium and rhodium, as well as on the measurement of scattered radiation from a238Pu source. The r.m.s. error of the determination varies from 0.01 to 0.10% of Pt, 0.002 to 0.01% of Au and 0.01 to 0.15% of Pd depending on the concentration. In the case of Rh and In the errors are 0.008% and 0.04 g In/l, respectively. 相似文献
19.
Zhifeng Tu Shenci Lu Xijun Chang Zhenhua Li Zheng Hu Lijun Zhang Hua Tian 《Mikrochimica acta》2011,173(1-2):231-239
Activated carbon was chemically modified with ethyl-3-(2-aminoethylamino)-2-chlorobut-2-enoate to obtain a material for selective solid-phase extraction of trace Au(III), Pd(II) and Pt(IV) prior to their determination by inductively coupled plasma atomic emission spectrometry. Experimental conditions such as effects of pH, shaking time, sample flow rate and volume, elution and interfering ions were studied. The ions Au(III), Pd(II) and Pt(IV) can be quantitatively adsorbed on the new sorbent from solution of pH 1. The adsorbed ions were then eluted with 0.1 mol L?1 hydrochloric acid and containing 4% thiourea. Many common ions do not interfere. The adsorption capacity of the material is 305, 92, and 126 mg g?1 for Au(III), Pd(II) and Pt(IV), respectively, and the detection limits are 5, 11 and 9 ng mL?1. The relative standard deviation is less than 3.0% (n?=?8) under optimum conditions. The method was validated by analyzing two certified reference materials and successfully applied to the preconcentration and determination of these ions in actual samples with satisfactory results. Figure
Activated carbon was chemically modified with ethyl-3-(2-aminoethylamino)-2-chlorobut-2-enoate to obtain a material for selective solid-phase extraction of trace Au(III), Pd(II) and Pt(IV) prior to their determination by inductively coupled plasma atomic emission spectrometry. Parameters affecting solid-phase extraction were systematically studied. This new adsorbent exhibited good characteristics for separation and preconcentration of Au(III), Pd(II) and Pt(IV) in aqueous solution, such as excellent selectivity, fast adsorption equilibrium, high tolerance limits of potentially interfering ions, high enrichment factor and low costs. It also shows relatively high adsorption capacity when compared to several other adsorbents. In addition, the synthetic method of the adsorbent was very simple. 相似文献