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1.
A new po1y(acrylphenylamidrazone phenylhydrazide) chelating fiber is synthesized from polyacrylonitrile fiber and used for preconcentration and separation of trace Ga(III), In(III), Bi(III), V(V) and Ti(IV) from solution (5–50 ng ml−1 Ti(IV) or V(V) and 50–500 ng ml−1 Ga(III), In (III) or Bi(III) in 1000–100 ml of solution can be enriched quantitatively by 0.15 g of fiber at a 4 ml min−1 flow rate in the pH range 5–7 with recoveries >95%). These ions can be desorbed quantitatively with 20 ml of 4 M hydrochloric acid at 2 ml min−1 from the fiber column. When the fiber which had been treated with concentrated hydrochloric acid and washed with distilled water until neutral was reused eight times, the recoveries of the above ions by enrichment were still >95%. Two-hundred-fold to 10 000-fold excesses of Cu(II), Zn(II), Ca(II), Mn(II), Cr(III), Fe(III), Ba(II) and Al(III) caused little interference in the determination of these ions by inductively coupled plasma-atomic emission spectrometers (ICP-AES). The relative standard deviations for enrichment and determination of 50 ng ml−1 Ga, In or Bi and 10 ng ml−1 V or Ti are in the range 1.2–2.7%. The contents of these ions in real solution samples determined by this method were in agreement with the certified values of the samples with average errors <3.7%.  相似文献   

2.
Gong B  Li X  Wang F  Chang X 《Talanta》2000,52(2):217-223
A novel spherical macroporous epoxy-dicyandiamide chelating resin is synthesized simply and rapidly from epoxy resin and use for the preconcentration and separation of trace Ga(III), In(III), Bi(III), Sn(IV), Pb(II), V(V) and Ti(IV) ions from solution samples. The analyzed ions can be quantitatively concentrated by the resin at flow rate of 3.0 ml min(-1) at pH 3, and can also be desorbed with 10 ml of 4 M HCl+0.2 g thiourea from the resin column with recoveries of 97-100%. The chelating resin is reused for eight times, the recoveries of these ions are still over 92%, and a 100-1000 times of excess of Fe(III), Al(III),Ca(II), Mg(III), Ni(II), Mn(II), Co(II), Cu(II), Zn(II), and Cd(II) cause no interference in the determination of these ions by inductively-coupled plasma atomic emission spectrometry. The capacities of the resin for the analytes are in the range of 0.66-4.20 mmol g(-1). The results show the relative standard deviation for the determination of 50.0 ng ml(-1) Ga(III), In(III), Bi(III), Sn(IV) and Pb(II), 5.0 ng ml(-1) V(V) and Ti(IV) are in the range of 1.2-4.0%. The recoveries of a standard added in real solution samples are between 96 and 100%, and the concentration of each ion in mineral sample detected by the method is in good agreement with the certified value.  相似文献   

3.
《Analytical letters》2012,45(14):2611-2623
Abstract

A new epoxy-urea chelating resin was synthesized from epoxy resin and used for the preconcentration and separation of trace Bi(III), In(III), Sn(IV), Zr(IV), V(V) and Ti(IV) ions from solution samples. The analyzed ions can be enriched at pH 5 at a flow rate of 1–4 ml/min, and can be also desorbed with 10 mL of 2 M HCl +0.1g NH4F solution from the resin column, with recoveries over 97%. The chelating resin reused 6 times can still adsorb quantitatively the Bi, In, Sn, Zr, V and Ti ions, and eighty to thousand-fold excesses of Ca(II), Mg(II), Cu(II), Zn(II), Al(III), Sb(III), Ni(II), Mn(II) and Fe(III) cause little interference with the enrichment and determination of these ions. The RSDs of the proposed method for the determination of 500–50 ng/ml Bi, In and Sn, 50–5.0 ng/ml Zr, V and Ti were in the range of 0.4 ~ 4.0%, the enrichment factor of the resin for the ions is in the range of 10–100. The recoveries of added standard in waste water are between 96% and 100%, and the concentration of each ion in alloy steel sample determined by the method is in good agreement with the reference value analyzed by a steel plant with average error <2.8%.  相似文献   

4.
Chang X  Su Q  Liang D  Wei X  Wang B 《Talanta》2002,57(2):253-261
Poly(acryldinitrophenylamidrazone-dinitroacrylphenylhydrazine) chelating fiber was synthesized from polyacrylonitrile fiber and used for enrichment and separation for traces of Au(III), Ru(III), In(III), Bi(III), Zr(IV), V(V), Ga(III) and Ti(IV) ions from solution samples. The acidity, rate, re-use, capacity and interference on the adsorption of ions on the chelating fiber as well as the conditions of desorption of these ions from the chelating fiber were investigated by means of inductively coupled plasma optical emission spectrometry. The results show that 10-100 ngml(-1) of Au(III), Ru(III), In(III), Bi(III), Zr(IV), V(V), Ga(III) and Ti(IV) ions can be quantitatively enriched by the chelating fiber at a 2 mlmin(-1) of flow rate in the range pH 4-5, and desorbed quantitatively with 20 ml of 5 M HCl for In(III), Bi(III), Zr(IV), V(V), Ga(III), Ti(IV) and 20 ml of 4 M HCl+2% CS(NH(2))(2) solution for Au(III), Ru(III) (with recovery>95%). 50- to 500- fold excesses of Fe(III), Al(III), Mg(II), Mn(II), Ca(II), Cu(II), Ni(II) ions cause little interference in the concentration and determination of analyzed ions. When the fiber was reused for 8 times, the recoveries of the above ions enriched by the fiber were still over 87%. The relative standard deviations (RSDs) for the enrichment and determination of 10 ngml(-1) Au, Ru, In, Bi, Ga and 1 ngml(-1) Zr, V, Ti were lower than 3.0%. The results obtained for these ions in real solution samples by this method were basically in agreement with the given values with average errors of less than 6.3%. FT-IR spectra show that existence of NNCNHNH, OCNHNH and NO(2) functional groups are verified in chelating fiber, and Au(III) or Ru(III) is mainly combined with nitrogen (or oxygen) of the groups to form a chelate complex.  相似文献   

5.
A new poly(acrylamidrazone-hydrazide) chelating fiber has been synthesized using polyacrylonitrile fiber as a starting material. An ICP-OES method for applying the fiber to preconcentrate and separate trace Au(III) and Pd(IV) ions in solution has been established. The experiments show that 8 ng/ml Au(III) and 6 ng/ml Pd(IV) in 1000 ml of solution can be enriched quantitatively by the fiber column at a flow rate of 12 ml/min at pH 2. These ions can be desorbed quantitatively with 10 ml of 2.5% CS(NH2)2 + 6% H2SO4 containing 0.2% Fe(II) from the column at an elution rate of 6 ml/min. A fiber treated with 12M HCl or 15M HNO3 can be re-used 10 times with above 95% recoveries of Au(III) and Pd(IV), and 120–800-fold excesses of Cu(II), Mn(II), Fe(III), Al(III), Ni(II), Mg(II) and Ca(II) ions cause little interference. The RSDs are 2.0% for 8 ng/ml Au and 3.5% for 6 ng/ml Pd. The recovery of added standard in a solution sample from a metal smelter is 96.2% for Au and 100% for Pd, and the content of each ion in the sample determined by the method is in agreement with the analysed value from the smelter laboratory.  相似文献   

6.
Chang X  Su Z  Luo X  Zhan G 《Talanta》1993,40(4):527-532
A poly(acrylamidrazone-hydrazide) chelating fiber has been synthesized from polyacrylonitrile fiber and used for enrichment-separation of traces of In(III), Sn(IV), Cr(III), VO(I) and Ti(IV) from solution samples with satisfactory results. These ions (5-250 ng/ml) can be quantitatively enriched (recovery > 95%) by the fiber at a 10 ml/min flow rate in the pH range 4-7, and desorbed quantitatively (recovery > 95%) with 10 ml of 2-5M hydrochloric acid from a fiber column at 6 ml/min flow rate. When the fiber, which had been stored in a glass bottle for about two years and then treated with strong acids (concentrated hydrochloric or nitric acid), was reused 10 times, the recoveries of the above ions by enrichment were still over 94%, and hundred-fold to thousand-fold excesses of Cu(II), Zn(II), Co(II), Ca(II), Mg(II), Fe(III) and Al(III) caused little interference in the determination of these ions by ICP-AES. The lowest concentrations for the proposed method were 50 ng/ml and In and Sn and 5 ng/ml for Cr, V and Ti. The RSD was 1.2-4.0%. The contents of these ions in real solution samples determined by this method were basically in agreement with the certified values of the samples, with average errors below 3.3%. The IR spectra of the fiber adsorbed with Cr(III) or VO(I) showed that Cr(III) or VO(I) combined mainly with nitrogen atoms in the fiber to form a coordination complex.  相似文献   

7.
 An ICP-OES method using a new poly (acrylphenylamidrazone-phenylhydrazide-acylphenylhydrazine) chelating fiber to preconcentrate and separate trace In(III), Zr(IV), Tl(I), V(V), Ga(III) and Ti(IV) ions from solution samples has been established. The new chelating fiber was synthesized using polyacrylonitrile fiber as a starting material and the structure of the chelating fiber was determined by FT infrared spectrometry. The acidity, adsorption rate, re-use, capacity and interference on the adsorption of ions on the chelating fiber as well as the conditions of desorption of these ions from the chelating fiber were investigated by means of inductively coupled plasma optical emission spectrometry (ICP-OES). The results show that the relative standard deviations for the determination of 10 ng/ml In, Tl, Ga and 1 ng/ml Zr, V, Ti were lower than 2.5%. The results obtained for these ions in real solution samples by this method were basically in agreement with the given values with average errors of less than 4%. Received November 29, 2000. Revision May 22, 2001.  相似文献   

8.
A new poly(acrylamidrazone-hydrazide lacmoid) chelating fibre has been synthesized from polyacrylonitrile fibre and used for the preconcentration and separation of traces of Cr(III), Ga(III), In(III) and Ti(IV) from solutions with satisfactory results. These ions can quantitatively be enriched by the chelating fibre at a flowrate of 6 ml/min at pH 6, and quantitatively desorbed with 10 ml of eluent at a rate of 4 ml/min. The chelating fibre reused ten times can still quantitatively concentrate traces of the above ions; twenty to two hundred-fold excesses of coexistent ions caused only little interference. With concentrations of 10 ng/ml Cr(III) and Ti(IV), and 50 ng/ml Ga(III) and In(III), the RSD was in the range of 1.4–4.6%. The contents determined in real samples were generally in agreement with the results obtained by HG-AAS; the recoveries of added standards were >96%.  相似文献   

9.
Poly(acrylp-aminobenzenesulfonamideamidine-p-aminobenzenesulfonylamide) chelating fiber containing "S", "N", and "O" elements was synthesized from polyacrylonitrile fiber and p-aminobenzene sulfonamide and used to enrich and separate trace Bi(III), Hg(III), Au(III), and Pd(IV) ions from wastewater and ore sample solution. The enrichment acidity, flow rate, elution conditions, reuse, interference ions, saturated adsorption capacity, constant of adsorption rate, analytical accuracy, and actual samples on chelating fiber were investigated by means of inductively coupled plasma optical emission spectrometry (ICP-OES) with satisfactory results. Solutions of 100 ng mL–1 of Bi(III), Hg(III), Au(III), and Pd(IV) ions can be enriched quantitatively by this chelating fiber at a rate of 1.0 mL min–1 at pH 4 and desorbed quantitatively with 20 mL of 0.25 M HCl and 2% CS(NH2)2 solution at 50 °C (with recovery 97%). When the chelating fiber was reused for 20 times, the recoveries of the analyzed ions enriched by the fiber were still over 95% (except for Hg(III)). One thousand-fold excesses of Mn2+, Ca2+, Zn2+, Mg2+, Fe3+, Cu2+, Ni2+, Al3+, and Ba2+ ions and thousands-fold excesses of Na+ and K+ cause little interference in the pre-concentration and determination of the analyzed ions. The saturated adsorption capacity of Bi(III), Hg(III), Au(III), and Pd(IV) was 4.850×10–4, 3.235×10–4, 2.807×10–4, and 3.386×10–4 mol g–1, respectively. The constants of adsorption rate were 0.409 min–1 for Bi, 0.122 min–1 for Hg, 0.039 min–1 for Au, and 0.080 min–1 for Pd. The relative standard deviations (RSDs) for the enrichment and determination of 10 ng mL–1 Bi(III), Hg(III), Au(III), and Pd(IV) were lower than 2.3%. The results obtained for these ions in actual samples by this method were basically in agreement with the given values with average errors of less than 1.0%. FT-IR spectra shows that the existence of –SO2–Ar, –H2N–Ar, O=C–NH–, HN=C–NH–, and –HN–SO2 functional groups are verified in the chelating fiber. From the FT-IR spectroscopy, we can see that Hg(III), Au(III), and Pd(IV) are mainly combined with nitrogen and sulfur (or oxygen), and Bi(III) is mainly combined with nitrogen (or oxygen) of the groups to form a chelating complex.  相似文献   

10.
Gong B 《Talanta》2002,57(1):89-95
A novel polyacrylaminoimidazole chelating fiber is synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber) and used for the preconcentration and separation of trace Au(III), Hg(II) and Pd(IV) ions from solution samples. The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 15.0 mlmin(-1) at pH 3 and can also be desorbed with 15 ml of 4 M HCl+3% thiourea from the fiber column, with recoveries of 96.5-100%. The chelating fiber is reused ten times; the recoveries of these ions are still over 92%, and 100-1000 times of excess of Fe(III), Al(III), Ca(II), Mg(II), Ni(II), Mn(II), Cu(II), Zn(II) and Cd(II) causes no interference in the determination of these ions by inductively coupled plasma atomic emission spectrometry. The capacities of the fiber for the analytes are in the range of 1.56-2.92 mmolg(-1). The results show that the relative standard deviations for the determination of 50.0 ngml(-1) each of Au(III), Hg(IV) and Pd(IV) are in the range of 0.7-2.1%. The recoveries of a standard added in real solution samples are between 97 and 99%, and the concentration of each ion in powder sample detected by the method is in good agreement with the certified value.  相似文献   

11.
A new spherical macroporous epoxy-melamine chelating resin was synthesized simply and rapidly and used for the preconcentrating and separation of trace of Ga(III), In(III),Bi(III), Sn(IV)and Ti(IV) ions from sample solutions. The ions analyzed can be quantitatively enriched by the resin at a flow-rate of 2ml/min at pH4,and quantitatively desorbed with 10ml of 2mol/L HCl+0.2gCS(NH2)2 at a flow-rate of 1ml/min with recoveries of over 97%,The chelating resin can be reused 7times without obvious loss of efficiency.  相似文献   

12.
Chang X  Li Y  Zhan G  Luo X  Gao W 《Talanta》1996,43(3):407-413
A new kind of poly(N-aminoethyl)acrylamide chelating fiber was synthesized from nitrilon (an acrylonitrile-based synthetic fiber) and used for the concentration and separation of traces of noble metal ions from solution. The results showed that 16-80 ng ml (1) of Au(III), Pt(IV), Pd(IV), Ir(IV), Ru(III) and Rh(III) can be quantitatively concentrated by the fiber up to a flow rate of 20 ml min (-1) at pH 3, and can be desorbed quantitatively with an eluting agent from the fiber column with recoveries of 96-100%. For a fiber reused 10 times, the recoveries of these ions were still over 94%, and a 100-1000 times excess of Fe(III), Al(III), Ca(II), Mg(II), Ni(II), Co(II), Cu(II) and Zn(II) caused no interference in the determination of these ions by inductively-coupled plasma atomic emission spectrometry. The capacities of the fiber for the analytes were in the range 0.80-2.62 mol g(-1), The relative standard deviation of the method was between 0.02% and 2.6%. Recoveries of a standard added to a real sample were 96.8-99.2%. The average error for the analysis by this method for a powder sample was 3.5%. The IR spectra of the analyte-bearing fiber showed that these ions coordinated to nitrogen sites in the fiber.  相似文献   

13.
A new poly(epoxy-melamine) chelating resin is synthesized from epoxy resin and used for the preconcentration and separation of traces of Ru(III), Au(III), V(V) and Ti(IV) ions from sample solutions. The ions analyzed can be quantitatively enriched by the resin at a flow-rate of 2 mL/min at pH 4, and quantitatively desorbed with 10 mL of 1 mol/L HCl + 0.2 g CS(NH2)2 at a flow-rate of 1 mL/min with recoveries of over 97%. The chelating resin can be reused 7 times without obvious loss of efficiency. Thousand-fold excesses of coexistent ions caused little interference during the enrichment and determination steps. The RSDs for the determination of 50 ng/mL Ru(III) and Au(III), 5.0 ng/mL V(V) and Ti(IV) were in the range of 1.5–4.5%. The recoveries of added standards in a real sample solution are between 96% and 100%, and the results for the ions analyzed in a nickel alloy sample are in good agreement with their reported values.  相似文献   

14.
A new poly(epoxy-melamine) chelating resin is synthesized from epoxy resin and used for the preconcentration and separation of traces of Ru(III), Au(III), V(V) and Ti(IV) ions from sample solutions. The ions analyzed can be quantitatively enriched by the resin at a flow-rate of 2 mL/min at pH 4, and quantitatively desorbed with 10 mL of 1 mol/L HCl + 0.2 g CS(NH2)2 at a flow-rate of 1 mL/min with recoveries of over 97%. The chelating resin can be reused 7 times without obvious loss of efficiency. Thousand-fold excesses of coexistent ions caused little interference during the enrichment and determination steps. The RSDs for the determination of 50 ng/mL Ru(III) and Au(III), 5.0 ng/mL V(V) and Ti(IV) were in the range of 1.5–4.5%. The recoveries of added standards in a real sample solution are between 96% and 100%, and the results for the ions analyzed in a nickel alloy sample are in good agreement with their reported values. Received: 12 May 1997 / Revised: 1 September 1997 / Accepted: 9 October 1997  相似文献   

15.
A novel polyacrylaminothiourea chelating fiber was synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber), which was applied to preconcentrate and separate of trace amount of Au(Ⅲ),Pt(Ⅳ),Pd(Ⅳ) and Ir (Ⅳ) ions from solution of samples.The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 20.0mL/min at pH2, and can also be desorbed with 15 mL of 4mol/L HCl 3% thiourea from the fiber column with recoveries of 96.5%-100%.The chelating fiber can be reused for ten times,the recoveries of these ions are still over 92%,and hundred to thousand times of excess of Fe(Ⅲ),Al(Ⅲ),Ca(Ⅱ),Mg(Ⅱ),Ni(Ⅱ),Mn(Ⅱ),Cu(Ⅱ),Zn(Ⅱ),and Cd(Ⅱ) cause no interference on the determination of the analyzed ions by inductively-coupled plasma atomic emission spectrometry (ICP-AES).The static saturation adsorption capacities of the fiber for the analytes are in the range of 1.15-2.80mmol/g.The relative standard deviations for the determination of 20.0ng/mL each of Au(Ⅲ),Pt(Ⅳ),Pd(Ⅳ)and Ir(Ⅳ) are in the range of 0.7%-3.0%.The recoveries for test from standard additions to real solution samples are between 96% and 100%.The concentration of each ion in powder sample detected by the method is in good agreement with the certified value.  相似文献   

16.
A new epoxy-tannin chelating resin was synthesized from epoxy resin and used for the preconcentration and separation of rare elements. The acidity, rate, reuse, capacity and interference on the adsorption of ions on the resin as well as the conditions of desorption of these ions from the resin were investigated by means of inductively coupled plasma atomic emission spectrometry (ICP-AES). The composition of the resin and mechanism of enrichment for some ions were discussed. The results show that the relative standard deviations for the determination of 50 ng ml−1 Ga(III), In(III), Bi(III) and Sn(IV), 10 ng ml−1 La(III), Y(III), Cr(III), Ti(IV) and V(V) and 1.0 ng ml−1 Be(II) were in the range of 0.5–4.5%. The contents of these elements in a sample solution from a smelter determined by the new method were in agreement with those values obtained by Zeeman atomic absorption spectrometry with an average error <3.4%.  相似文献   

17.
Yatirajam V  Ram J 《Talanta》1974,21(12):1308-1311
A simple and rapid spectrophotometric determination of molybdenum is described. The molybdenum thiosulphate complex is extracted into isoamyl alcohol from 1·0–1·5M hydrochloric acid containing 36–40 mg of Na2S2O3·5H2O per ml. The absorbance at λmax = 475 nm obeys Beer's law over the range 0–32 μg of Mo per ml of solvent phase. Up to 5 mg/ml of Ti(IV), V(V), Cr(VI), Fe(III), Co(II), Ni(II), U(VI), W(VI), Sb(III), 1 mg/ml of Cu(II), Sn(II), Bi(V) and 10 μg/ml of Pt(IV) and Pd(II) do not interfere. Large amounts of complexing agents interfere. The method has been applied to analysis of synthetic and industrial samples.  相似文献   

18.
    
Zusammenfassung Fluorone, Verbindungen des 2,3,7-Trihydroxyisoxanthenons-(6), eignen sich als empfindliche Reagentien für die spektralphotometrische Analyse zahlreicher Metallionen im sichtbaren Teil des Spektrums. Neben einigen grundsätzlichen Anmerkungen zur Herstellung, zu den Eigenschaften und Reaktionen der Fluorone mit Metallionen wird die Verwendung des Cyclohexylfluorons (CHF) für die photometrische Bestimmung von Cu(II)-Ion beschrieben; hierbei ergibt sich ein molarer Extinktionskoeffizient von 191000 l/Mol · cm und eine Standardabweichung von ±0,2 ng/ml. Der Anwendungsbereich liegt bei 6–60 ng Cu/ml. Bi, Fe(II/III) und Sb müssen zuvor abgetrennt werden.
Fluorones — reagents for photometric analysisPhotometric determination of copper
Summary Fluorones, derivates of 2,3,7-trihydroxyisoxanthenone-(6), are sensitive reagents for the spectrophotometric determination of many metal ions in aqueous solution. Besides some principal remarks on the synthesis, properties and reactions of fluorones, the application of cyclohexylfluorone for the determination of Cu(II) ion is described in detail. This method is applicable in the concentration range 6–60 ng of Cu/ml. The molar absorptivity is 1910001/Mol · cm and the standard deviation is ±0.2 ng/ml. Bi, Fe(II, III) and Sb have to be separated prior to the determination.
  相似文献   

19.
Summary A new chelating resin has been synthesized by modification of aminated macroporous poly(vinyl chloride) resin with pyrocatechol violet. The conditions for quantitative sorption of traces of Ti(IV), Zr(IV) and Ga(III) and quantitative elution of Ti(IV) and Zr(IV) are investigated. Accordingly, the collector can quantitatively adsorb traces of the above analytes at pH 2.0–6.0. Interferences of coexistent ions with traces of Ti(IV) and Zr(IV) can be neglected. After trace matrix separations by that collector, Ti and Zr determinations in real samples (e.g. steel, geochemical materials) can be performed with satisfactory results.  相似文献   

20.
A novel poly(acryl-p-toluenesulfonamideamidine-p-toluenesulfonylamide) chelating fiber containing S, N and O elements was synthesized from polyacrylonitrile fiber and p-toluenesulfonamide and used for the preconcentration and separation for traces of Ru(III), Rh(III), Au(III) and Pd(IV) ions from waste water and ore sample solution. The synthesis of this fiber was simple and rapid. The results indicate that 100ngmL–1 of these ions can be quantitatively enriched by the chelating fiber at a flow rate of 6mLmin–1 and a pH of 4 and desorbed quantitatively with 20mL of 6molL–1 HCl and 5% CS(NH2)2 solution at 50°C (with recovery>95%). A 50 to 1000-fold excess of Ca2+, Mg2+, Mn2+, Co2+, Fe3+, Cu2+, Zn2+, and Al3+ ions caused little interference in the concentration and determination of the analyzed ions. When the fiber had been reused twenty times, the recoveries of the ions enriched by the fiber were still over 96%. The saturated adsorption capacities of the fiber were in the range of 22–96mgg–1. The relative standard deviation (RSD) of the method was between 0.70% and 0.84%. Recoveries of a standard added to actual samples were in range of 95–101%. The results obtained for these ions in real solution samples were basically in agreement with the given values, the average errors being below 5.0%. FT-IR spectra show that the existence of –SO2–Ar, HN=C–NH–, O=C–NH– and –NH–SO2 functional groups are verified in the chelating fiber. The experiments show that the method is rapid, precise, simple and convenient.  相似文献   

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