A novel kinetic procedure for determination of trace copper was proposed based on the catalytic effect of Cu 2+ on the aerial oxidation of gallocyanine (GC), by which GC was oxidized and a colourless product was ...A novel kinetic procedure for determination of trace copper was proposed based on the catalytic effect of Cu 2+ on the aerial oxidation of gallocyanine (GC), by which GC was oxidized and a colourless product was produced. The reaction was monitored spectrophotometrically in hexamethylene tetramine hydrochloric acid buffer solution. The calibration graph is linear for 0.05～0.5 μg/ml, and the detection limit is 0 02 μg/ml (Cu 2+ ). The selectivity for copper is satisfied as the interferences of Fe 3+ and Al 3+ could be easily and effectively eliminated by the addition of NH 4HF 2. The method was applied to the determination of copper in soil, tap water and simulated water samples, and the results were satisfactory.展开更多
The simultaneous determination of cobalt, copper and nickel using 1-（2-thiazolylazo）-2-naphthol （first figure of this article） by spectrophotometric method is a difficult problem in analytical chemistry, due to sp...The simultaneous determination of cobalt, copper and nickel using 1-（2-thiazolylazo）-2-naphthol （first figure of this article） by spectrophotometric method is a difficult problem in analytical chemistry, due to spectral interferences. By multivariate calibration methods, such as partial least squares （PLS） regression, it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range. Orthogonal signal correction （OSC） is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis. OSC is a suitable preprocessing method for PLS calibration of mixtures without loss of prediction capacity using spectrophotometric method. In this study, the calibration model is based on absorption spectra in the 550-750-nm range for 21 different mixtures of cobalt, copper and nickel. Calibration matrices were formed from samples containing 0.05-1.05, 0.05-1.30 and 0.05-0.80 μg·mL^-1 for cobalt, copper and nickel, respectively. The root mean square error of prediction （RMSEP） for cobalt, copper and nickel with OSC and without OSC were 0.007, 0.008, 0.011 and 0.031,0.037, 0.032 μg· mL^-1, respectively. This procedure allows the simultaneous determination of cobalt, copper and nickel in synthetic and real samples and good reliability of the determination was proved.展开更多
The Dongfengnanshan Cu polymetallic deposit is one representative deposit of the Tianbaoshan ore district in the Yanbian area, northeast(NE) China. There occur two types of ore bodies in this deposit, the stratiform o...The Dongfengnanshan Cu polymetallic deposit is one representative deposit of the Tianbaoshan ore district in the Yanbian area, northeast(NE) China. There occur two types of ore bodies in this deposit, the stratiform ore bodies and veintype ones, controlled by the Early Permian strata and the Late Hercynian diorite intrusion, respectively. Due to the ambiguous genetic type of the stratiform ore bodies, there has been controversy on the relationship between them and veintype ore bodies. To determine the genetic type of stratiform ore bodies, laser ablation inductively coupled plasma mass spectrometry(LA-ICP-MS) in situ trace elements and S–Pb isotope analysis have been carried on the sulfides in the stratiform ore bodies. Compared with that in skarn, Mississippi Valley-type(MVT), and epithermal deposits, sphalerite samples in the stratiform ore bodies of the Dongfengnanshan deposit are significantly enriched in Fe, Mn, and In, while depleted in Ga, Ge, and Cd, which is similar to the sphalerite in volcanic-associated massive sulfide(VMS) deposits. Co/Ni ratio of pyrrhotites in the stratiform ore bodies is similar to that in VMS-type deposits. The concentrations of Zn and Cd of chalcopyrites are similar to those of recrystallized VMS-type deposits. These characteristics also reflect the intermediate ore-forming temperature of the stratiform ore bodies in this deposit. Sulfur isotope compositions of sulfides are similar to those of VMS-type deposits, reflecting that sulfur originated from the Permian Miaoling Formation. Lead isotope compositions indicate mixed-source for lead. Moreover, the comparison of the Dongfengnanshan stratiform ore bodies with some VMStype deposits in China and abroad, on the trace elements and S–Pb isotope characteristics of the sulfides reveals that the stratiform ore bodies of the Dongfengnanshan deposit belong to the VMS-type, and have closely genetic relationship with the early Permian marine volcanic sedimentary rocks.展开更多
Albitite often accompanies with various metal and gem mineral deposits and a large number of occurrences have been reported globally, including the South Qinling orogen, China. The Xiaozhen copper deposit is a typical...Albitite often accompanies with various metal and gem mineral deposits and a large number of occurrences have been reported globally, including the South Qinling orogen, China. The Xiaozhen copper deposit is a typical deposit in the North Daba Mountain area of the South Qinling orogen whose distribution is controlled by albitite veins and fractures. As there are few studies on the petrogenesis of albitite in Xiaozhen copper deposit, this paper focuses on the petrogenesis of albitite and its mineralization age. Detailed fieldwork and mineral microscopic observations initially suggest that albitite from the Xiaozhen copper deposit is igneous in origin. Further zircon trace element geochemistry studies indicate that these zircons have high Th/U ratios（〉0.5）, low La content, high（Sm/La）N and Ce/Ce＊values, and a strong negative Eu anomaly, which are commonly seen in magmatic zircons. The chondrite–normalized rare earth element（REE） patterns are consistent with magmatic zircons from throughout the world, and they fall within or near the field of magmatic zircons on discriminant diagrams. The calculated average apparent Ti–in–zircon temperature for young zircons is 780°C, consistent with magmatic zircon crystallization temperatures. Therefore, zircon geochemistry indicates that the albitite origin is magmatic. SIMS U–Pb dating on nine magmatic zircons yielded a concordia age of 154.8±2.2 Ma, which represents the formation of albitite and the metallogenic age. More importantly, it is consistent with the ages of Yanshanian magmatism and metallogenesis in the South Qinling orogen, so formation of the Xiaozhen copper deposit may be a closely related geological event.展开更多
A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements...A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.展开更多
Reagents are optimized for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in zinc sulfate solution, which contains an extremely large excess of Zn^(2+). First, the reagents and their d...Reagents are optimized for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in zinc sulfate solution, which contains an extremely large excess of Zn^(2+). First, the reagents and their doses for the experiment are selected according to the characteristics of the zinc sulfate solution. Then, the reagent doses are optimized by analyzing the influence of reagent dose on the polarographic parameters(i.e. half-wave potential E_(1/2) and limiting diffusion current I_p). Finally, the optimization results are verified by simultaneously determining trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of an extremely large excess of Zn^(2+). The determination results indicate that the optimized reagents exhibit wide linearity, low detection limits, high accuracy and good precision for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of an extremely large excess of Zn^(2+).展开更多
Determination of trace rare earth elements(REEs)in 99. 999% purity yttrium oxide using the inductively coupled plasma mass spectrometric technique (ICPMS) has been developed. Instrumental parameters and factors affeci...Determination of trace rare earth elements(REEs)in 99. 999% purity yttrium oxide using the inductively coupled plasma mass spectrometric technique (ICPMS) has been developed. Instrumental parameters and factors affecitng analytical results have been studied and then optimized.Samples are analyzed directly following an acid digestion without separation or preconcentration and with limit of detection of 0. 003～0. 02 ng/ml, precision of ±5. 4%(cofficient of variation)and recovery of 90～115%. Correction for isobaric interferences from oxide ions and hydroxide ions is made mathematically. Special internal standard procedures are used to compensate drift in metal:metal oxide ratios and sensitivity. The analytical results of several samples are accurate as compared with inductively coupled plasma atomic emission spectrometry (ICPAES) and spark source mass spectrometry (SSMS).展开更多
Ten male buffalo calves were randomly allotted into five groups of two each. Four groups were fed with cadmium, molybdenum, cadmium-molybdenum, and copper-cadmium-molybdenum respectively for 130 days to determine the ...Ten male buffalo calves were randomly allotted into five groups of two each. Four groups were fed with cadmium, molybdenum, cadmium-molybdenum, and copper-cadmium-molybdenum respectively for 130 days to determine the elements' metabolic interactions in calves. These results indicated that cadmium and molybdenum could increase the accumulation of molybdenum and cadmium in liver and kidneys in buffalo calves, but copper could not. reduce to normal the levels of molybdenum and cadmium in liver and kidneys caused by cadmium-molybdenum. In addition, we found the copper concentrations in liver and kindeys was significantly greater in treatment calves than in controls.展开更多
Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. Th...Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. The ternary complex Cu(I)-DMP-ClO4 was extracted quantitatively into molten naphthalene in the range of pH from 5 to 6 at 85 C-. Absorbance was spectrophotometrically determined at 459 nm against the reagent blank after the solid naphthalene layer was anhydrously dissolved in chloroform. Beer's law is obeyed over a concentration range of 0.5-70 mug/mL. The molar absorptivity and Sandell's sensitivity are 1.0x10(4) L/(mol(.)cm) and 0.0099 mug(.)cm(2) respectively. In addition, the various conditions on determination and the interference of coexisted ions were discussed, and the method was applied to the determination of copper ion both in tea samples and cadmium sulfate reagents. The results are in good agreement with those obtained by ICP AES method.展开更多
Based on selective volatilization taking place among elements in graphite furnace, a new method for direct determination of trace titanium in high purity yttrium oxide by fluorination electrothermal vaporization(FETV)...Based on selective volatilization taking place among elements in graphite furnace, a new method for direct determination of trace titanium in high purity yttrium oxide by fluorination electrothermal vaporization(FETV)/ICP AES has been proposed. The vaporization behavior of the analyte and matrix element was studied in detail. Various factors of influence on vaporization of analyte were also investigated. Under optimal experimental conditions, the detection limit(3 σ ) of Ti is 1 0 ng/ml, and the RSD is 2 3%( n =10, c =0 2 μg/ml). The proposed method is simple, rapid and sensitive, and pretreatment is not necessary. This method can be used to directly determine trace refractory impurity titanium in high purity powder sample(Y 2O 3). The recovery for sample analysis is more than 96%.展开更多
A stripping method for the determination of hypoxanthine in the presence of copper at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of hypoxanthine-copp...A stripping method for the determination of hypoxanthine in the presence of copper at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of hypoxanthine-copper at the thin-film mercury electrode followed by a fast linear scan voltammetric measurement of the surface species. Optimum experimental conditions were found to be the use of 1.0 × 10﹣3 mol·L﹣1 NaOH solution as electrolyte supporting, an accumulation potential of ﹣0.50 V and a linear scan rate of 200 mV·s﹣1. The response of hypoxanthine-copper is linear over the concentration ranges of 10 - 60 ppb. For an accumulation time of 30 minutes, the detection limit was found to be 250 ppt (1.8 × 10﹣9 mol·L﹣1). Adequate conditions for measuring the hypoxanthine in the presence of metal ions, xanthine, uric acid and other nitrogenated bases were also investigated. The utility of the method is demonstrated by the presence of hypoxanthine associated in ATP or ssDNA.展开更多
A fluoroimmunoassay method using unlabeled europium chelate is described.The principle is similar to that of fluoroimmunoassay method using lanthanide chelate as labels.The procedure is simple because labeling process...A fluoroimmunoassay method using unlabeled europium chelate is described.The principle is similar to that of fluoroimmunoassay method using lanthanide chelate as labels.The procedure is simple because labeling process is omitted.The detection limit is about 10^(10) mol/L antigen.The relative standard deviation of immunoassay is less than 10%.The recoveries of human serum albumin and estradiol protein conjugate are 96-105% and 111% respectively.展开更多
A new reagent 2-QADN2,7 has been synthesized and its electroana- lytical characteristics have been studied.The procedure of the adsorptive voltammetric determination of copper,nickel,cohalt and cadmium was worked out.
The indirect voltammetric determination of trace sulfate (2.0×10^(-6)～4.0×10^(-5) mol/L ) with the adsorptive complex wave of lead(Ⅱ)-tetrakis (4-trimethylammonium phenyl) porphyrin (PbTTMAPP) is reported....The indirect voltammetric determination of trace sulfate (2.0×10^(-6)～4.0×10^(-5) mol/L ) with the adsorptive complex wave of lead(Ⅱ)-tetrakis (4-trimethylammonium phenyl) porphyrin (PbTTMAPP) is reported.This method has been used for the analysis of natural waters with satisfactory results.展开更多
The derivative fluorimetric characteristics of Tb—SDS and Tb—SDS—phenanthroline systems have been studied. The optimum conditions were obtained. The 2nd—derivative spectrofluorimetric method in the systems has bee...The derivative fluorimetric characteristics of Tb—SDS and Tb—SDS—phenanthroline systems have been studied. The optimum conditions were obtained. The 2nd—derivative spectrofluorimetric method in the systems has been applied to the determination of trace amounts of terbium, in rare earth ore and their oxides. The results are satisfactory.展开更多
On-line dissolution of solid metal sample can be carried out by electrolysis under the control of flow injection analyzer(FIA),and the dissolved sample can be transferred to atomic spectrometer for the direct analysis...On-line dissolution of solid metal sample can be carried out by electrolysis under the control of flow injection analyzer(FIA),and the dissolved sample can be transferred to atomic spectrometer for the direct analysis.The hyphenated technique of FIA on-line electrolytic dissolution of alloy and atomic absorption spectrometer(AAS)detection is developed.The research is focused on the effects of electrolyte composition and electrolysis parameters on the sample dissolving,as well as the quantitative analysis of Cu in Al alloy samples.展开更多
A fluoroimmunoassay method using unlabeled Terbium chelate is described.The principle is similar to that of fluoroimmunoassay method using lanthanide chelate as labels.The procedure is simpte because labeling process ...A fluoroimmunoassay method using unlabeled Terbium chelate is described.The principle is similar to that of fluoroimmunoassay method using lanthanide chelate as labels.The procedure is simpte because labeling process is unnecessary.The recovery of HSA and albumin in urine is 107% and 95% respectively.The standard deviation is tess than 10%.展开更多
Macroporous amino-carboxvlic chelating resin of acrylic acid series may concentrate trace rare earth in the presence of 0.1 mol/l α-hydroxy-isobutyric acid at pH 4.5.With 0.10 mol/l HCl as eluant rare earth may be el...Macroporous amino-carboxvlic chelating resin of acrylic acid series may concentrate trace rare earth in the presence of 0.1 mol/l α-hydroxy-isobutyric acid at pH 4.5.With 0.10 mol/l HCl as eluant rare earth may be eluted quantitatively and separated from Ca,Mg,Fe and Cu.This method is used to determine trace amount of rare earth in human hair,stone (in kidney and bladder),peanut,grape,strawberry,cucumber,pig liver and other biological samples.展开更多
Terbium can form a ternary complex having a ratio of 1:1:1 with acetylacetone and EDTA. By adding cetyl pyridinium chloride into the above system, a marked enhancement of fluorescence intensity is observed and the ter...Terbium can form a ternary complex having a ratio of 1:1:1 with acetylacetone and EDTA. By adding cetyl pyridinium chloride into the above system, a marked enhancement of fluorescence intensity is observed and the ternary complex becomes more stable than before. For analytical application, the derivative spectrofluorimetric method has high sensitivity and the effect of foreign ions is very low. The optimum conditions were obtained. The calibration graph is linear over 5～100μg/mL.展开更多
In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a stron...In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a [R+] [BiI4-] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called 搕hin-layer resin phase?or 搑esin phase? and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer抯 law over the concentration range 0.01ug/ml^1.20ug/ml of bismuthous(III). It has a molar absorptivity of 7.1×105 [L/mol穋m]. It indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the measurements of 0.5ug/ml Bi(III). The detection limit of Bismuthous(III) is 1.4×10-8mol/L. The method has applied to the analysis Bi(III) in environmental water samples.展开更多
文摘A novel kinetic procedure for determination of trace copper was proposed based on the catalytic effect of Cu 2+ on the aerial oxidation of gallocyanine (GC), by which GC was oxidized and a colourless product was produced. The reaction was monitored spectrophotometrically in hexamethylene tetramine hydrochloric acid buffer solution. The calibration graph is linear for 0.05～0.5 μg/ml, and the detection limit is 0 02 μg/ml (Cu 2+ ). The selectivity for copper is satisfied as the interferences of Fe 3+ and Al 3+ could be easily and effectively eliminated by the addition of NH 4HF 2. The method was applied to the determination of copper in soil, tap water and simulated water samples, and the results were satisfactory.
文摘The simultaneous determination of cobalt, copper and nickel using 1-（2-thiazolylazo）-2-naphthol （first figure of this article） by spectrophotometric method is a difficult problem in analytical chemistry, due to spectral interferences. By multivariate calibration methods, such as partial least squares （PLS） regression, it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range. Orthogonal signal correction （OSC） is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis. OSC is a suitable preprocessing method for PLS calibration of mixtures without loss of prediction capacity using spectrophotometric method. In this study, the calibration model is based on absorption spectra in the 550-750-nm range for 21 different mixtures of cobalt, copper and nickel. Calibration matrices were formed from samples containing 0.05-1.05, 0.05-1.30 and 0.05-0.80 μg·mL^-1 for cobalt, copper and nickel, respectively. The root mean square error of prediction （RMSEP） for cobalt, copper and nickel with OSC and without OSC were 0.007, 0.008, 0.011 and 0.031,0.037, 0.032 μg· mL^-1, respectively. This procedure allows the simultaneous determination of cobalt, copper and nickel in synthetic and real samples and good reliability of the determination was proved.
基金supported by the National Natural Science Foundation of China (NSFC) (No. 41772062)
文摘The Dongfengnanshan Cu polymetallic deposit is one representative deposit of the Tianbaoshan ore district in the Yanbian area, northeast(NE) China. There occur two types of ore bodies in this deposit, the stratiform ore bodies and veintype ones, controlled by the Early Permian strata and the Late Hercynian diorite intrusion, respectively. Due to the ambiguous genetic type of the stratiform ore bodies, there has been controversy on the relationship between them and veintype ore bodies. To determine the genetic type of stratiform ore bodies, laser ablation inductively coupled plasma mass spectrometry(LA-ICP-MS) in situ trace elements and S–Pb isotope analysis have been carried on the sulfides in the stratiform ore bodies. Compared with that in skarn, Mississippi Valley-type(MVT), and epithermal deposits, sphalerite samples in the stratiform ore bodies of the Dongfengnanshan deposit are significantly enriched in Fe, Mn, and In, while depleted in Ga, Ge, and Cd, which is similar to the sphalerite in volcanic-associated massive sulfide(VMS) deposits. Co/Ni ratio of pyrrhotites in the stratiform ore bodies is similar to that in VMS-type deposits. The concentrations of Zn and Cd of chalcopyrites are similar to those of recrystallized VMS-type deposits. These characteristics also reflect the intermediate ore-forming temperature of the stratiform ore bodies in this deposit. Sulfur isotope compositions of sulfides are similar to those of VMS-type deposits, reflecting that sulfur originated from the Permian Miaoling Formation. Lead isotope compositions indicate mixed-source for lead. Moreover, the comparison of the Dongfengnanshan stratiform ore bodies with some VMStype deposits in China and abroad, on the trace elements and S–Pb isotope characteristics of the sulfides reveals that the stratiform ore bodies of the Dongfengnanshan deposit belong to the VMS-type, and have closely genetic relationship with the early Permian marine volcanic sedimentary rocks.
基金supported by the fundamental research funds for central public welfare research institutes (grant: K1313)National Natural Science Foundation of China (grant: 41302080)the geological survey project of China (grant: 1212011121091)
文摘Albitite often accompanies with various metal and gem mineral deposits and a large number of occurrences have been reported globally, including the South Qinling orogen, China. The Xiaozhen copper deposit is a typical deposit in the North Daba Mountain area of the South Qinling orogen whose distribution is controlled by albitite veins and fractures. As there are few studies on the petrogenesis of albitite in Xiaozhen copper deposit, this paper focuses on the petrogenesis of albitite and its mineralization age. Detailed fieldwork and mineral microscopic observations initially suggest that albitite from the Xiaozhen copper deposit is igneous in origin. Further zircon trace element geochemistry studies indicate that these zircons have high Th/U ratios（〉0.5）, low La content, high（Sm/La）N and Ce/Ce＊values, and a strong negative Eu anomaly, which are commonly seen in magmatic zircons. The chondrite–normalized rare earth element（REE） patterns are consistent with magmatic zircons from throughout the world, and they fall within or near the field of magmatic zircons on discriminant diagrams. The calculated average apparent Ti–in–zircon temperature for young zircons is 780°C, consistent with magmatic zircon crystallization temperatures. Therefore, zircon geochemistry indicates that the albitite origin is magmatic. SIMS U–Pb dating on nine magmatic zircons yielded a concordia age of 154.8±2.2 Ma, which represents the formation of albitite and the metallogenic age. More importantly, it is consistent with the ages of Yanshanian magmatism and metallogenesis in the South Qinling orogen, so formation of the Xiaozhen copper deposit may be a closely related geological event.
文摘A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.
基金Projects(61533021,61321003,61273185)supported by the National Natural Science Foundation of ChinaProject(2015CX007)supported by the Innovation-driven Plan in Central South University,ChinaProject(13JJ8003)supported by the Joint Fund of Hunan Provincial Natural Science Foundation of China
文摘Reagents are optimized for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in zinc sulfate solution, which contains an extremely large excess of Zn^(2+). First, the reagents and their doses for the experiment are selected according to the characteristics of the zinc sulfate solution. Then, the reagent doses are optimized by analyzing the influence of reagent dose on the polarographic parameters(i.e. half-wave potential E_(1/2) and limiting diffusion current I_p). Finally, the optimization results are verified by simultaneously determining trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of an extremely large excess of Zn^(2+). The determination results indicate that the optimized reagents exhibit wide linearity, low detection limits, high accuracy and good precision for the simultaneous determination of trace amounts of Cu^(2+), Cd^(2+) and Co^(2+) in the presence of an extremely large excess of Zn^(2+).
文摘Determination of trace rare earth elements(REEs)in 99. 999% purity yttrium oxide using the inductively coupled plasma mass spectrometric technique (ICPMS) has been developed. Instrumental parameters and factors affecitng analytical results have been studied and then optimized.Samples are analyzed directly following an acid digestion without separation or preconcentration and with limit of detection of 0. 003～0. 02 ng/ml, precision of ±5. 4%(cofficient of variation)and recovery of 90～115%. Correction for isobaric interferences from oxide ions and hydroxide ions is made mathematically. Special internal standard procedures are used to compensate drift in metal:metal oxide ratios and sensitivity. The analytical results of several samples are accurate as compared with inductively coupled plasma atomic emission spectrometry (ICPAES) and spark source mass spectrometry (SSMS).
文摘Ten male buffalo calves were randomly allotted into five groups of two each. Four groups were fed with cadmium, molybdenum, cadmium-molybdenum, and copper-cadmium-molybdenum respectively for 130 days to determine the elements' metabolic interactions in calves. These results indicated that cadmium and molybdenum could increase the accumulation of molybdenum and cadmium in liver and kidneys in buffalo calves, but copper could not. reduce to normal the levels of molybdenum and cadmium in liver and kidneys caused by cadmium-molybdenum. In addition, we found the copper concentrations in liver and kindeys was significantly greater in treatment calves than in controls.
基金This research was financially supported by the project KJCXGC-01 of Northwest Normal University, China.
文摘Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. The ternary complex Cu(I)-DMP-ClO4 was extracted quantitatively into molten naphthalene in the range of pH from 5 to 6 at 85 C-. Absorbance was spectrophotometrically determined at 459 nm against the reagent blank after the solid naphthalene layer was anhydrously dissolved in chloroform. Beer's law is obeyed over a concentration range of 0.5-70 mug/mL. The molar absorptivity and Sandell's sensitivity are 1.0x10(4) L/(mol(.)cm) and 0.0099 mug(.)cm(2) respectively. In addition, the various conditions on determination and the interference of coexisted ions were discussed, and the method was applied to the determination of copper ion both in tea samples and cadmium sulfate reagents. The results are in good agreement with those obtained by ICP AES method.
文摘Based on selective volatilization taking place among elements in graphite furnace, a new method for direct determination of trace titanium in high purity yttrium oxide by fluorination electrothermal vaporization(FETV)/ICP AES has been proposed. The vaporization behavior of the analyte and matrix element was studied in detail. Various factors of influence on vaporization of analyte were also investigated. Under optimal experimental conditions, the detection limit(3 σ ) of Ti is 1 0 ng/ml, and the RSD is 2 3%( n =10, c =0 2 μg/ml). The proposed method is simple, rapid and sensitive, and pretreatment is not necessary. This method can be used to directly determine trace refractory impurity titanium in high purity powder sample(Y 2O 3). The recovery for sample analysis is more than 96%.
文摘A stripping method for the determination of hypoxanthine in the presence of copper at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of hypoxanthine-copper at the thin-film mercury electrode followed by a fast linear scan voltammetric measurement of the surface species. Optimum experimental conditions were found to be the use of 1.0 × 10﹣3 mol·L﹣1 NaOH solution as electrolyte supporting, an accumulation potential of ﹣0.50 V and a linear scan rate of 200 mV·s﹣1. The response of hypoxanthine-copper is linear over the concentration ranges of 10 - 60 ppb. For an accumulation time of 30 minutes, the detection limit was found to be 250 ppt (1.8 × 10﹣9 mol·L﹣1). Adequate conditions for measuring the hypoxanthine in the presence of metal ions, xanthine, uric acid and other nitrogenated bases were also investigated. The utility of the method is demonstrated by the presence of hypoxanthine associated in ATP or ssDNA.
基金This work was supported by National Natural Science Foundation of China.
文摘A fluoroimmunoassay method using unlabeled europium chelate is described.The principle is similar to that of fluoroimmunoassay method using lanthanide chelate as labels.The procedure is simple because labeling process is omitted.The detection limit is about 10^(10) mol/L antigen.The relative standard deviation of immunoassay is less than 10%.The recoveries of human serum albumin and estradiol protein conjugate are 96-105% and 111% respectively.
文摘A new reagent 2-QADN2,7 has been synthesized and its electroana- lytical characteristics have been studied.The procedure of the adsorptive voltammetric determination of copper,nickel,cohalt and cadmium was worked out.
文摘The indirect voltammetric determination of trace sulfate (2.0×10^(-6)～4.0×10^(-5) mol/L ) with the adsorptive complex wave of lead(Ⅱ)-tetrakis (4-trimethylammonium phenyl) porphyrin (PbTTMAPP) is reported.This method has been used for the analysis of natural waters with satisfactory results.
基金Project supported by the National Natural Science Foundation of China
文摘The derivative fluorimetric characteristics of Tb—SDS and Tb—SDS—phenanthroline systems have been studied. The optimum conditions were obtained. The 2nd—derivative spectrofluorimetric method in the systems has been applied to the determination of trace amounts of terbium, in rare earth ore and their oxides. The results are satisfactory.
文摘On-line dissolution of solid metal sample can be carried out by electrolysis under the control of flow injection analyzer(FIA),and the dissolved sample can be transferred to atomic spectrometer for the direct analysis.The hyphenated technique of FIA on-line electrolytic dissolution of alloy and atomic absorption spectrometer(AAS)detection is developed.The research is focused on the effects of electrolyte composition and electrolysis parameters on the sample dissolving,as well as the quantitative analysis of Cu in Al alloy samples.
基金supported by National Commission of Natural Science Foundation of China.
文摘A fluoroimmunoassay method using unlabeled Terbium chelate is described.The principle is similar to that of fluoroimmunoassay method using lanthanide chelate as labels.The procedure is simpte because labeling process is unnecessary.The recovery of HSA and albumin in urine is 107% and 95% respectively.The standard deviation is tess than 10%.
文摘Macroporous amino-carboxvlic chelating resin of acrylic acid series may concentrate trace rare earth in the presence of 0.1 mol/l α-hydroxy-isobutyric acid at pH 4.5.With 0.10 mol/l HCl as eluant rare earth may be eluted quantitatively and separated from Ca,Mg,Fe and Cu.This method is used to determine trace amount of rare earth in human hair,stone (in kidney and bladder),peanut,grape,strawberry,cucumber,pig liver and other biological samples.
基金Project supported by the National Natural Science Foundation of China
文摘Terbium can form a ternary complex having a ratio of 1:1:1 with acetylacetone and EDTA. By adding cetyl pyridinium chloride into the above system, a marked enhancement of fluorescence intensity is observed and the ternary complex becomes more stable than before. For analytical application, the derivative spectrofluorimetric method has high sensitivity and the effect of foreign ions is very low. The optimum conditions were obtained. The calibration graph is linear over 5～100μg/mL.
文摘In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a [R+] [BiI4-] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called 搕hin-layer resin phase?or 搑esin phase? and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer抯 law over the concentration range 0.01ug/ml^1.20ug/ml of bismuthous(III). It has a molar absorptivity of 7.1×105 [L/mol穋m]. It indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the measurements of 0.5ug/ml Bi(III). The detection limit of Bismuthous(III) is 1.4×10-8mol/L. The method has applied to the analysis Bi(III) in environmental water samples.
