The feasibility of using electrodes modified with polyaniline incorporated carbon particles films for improving the precision of coulometric titration is demonstrated. The problem of large deviation produced during de...The feasibility of using electrodes modified with polyaniline incorporated carbon particles films for improving the precision of coulometric titration is demonstrated. The problem of large deviation produced during determining polyisoprene by coulometric titration with direct titration technique(double Pt electrodes indicating electrode) has been solved. In the titration process, polyisoprene alcohol, an electro-inactive species, is adsorbed on the surface of the bare Pt electrode, which inhibits the electrode reaction of Br - and Br 2. Therefore, when the titration reaches the end-point, the detected current will slowly change with time, which can make the repeatability of end-point poor. The atomic force microscopic images show the morphology of the electrode surface of adsorbing polyisoprene alcohol. The application of the chemically modified electrode instead of the bare Pt electrode to indicating the end-point has been investigated. The results show that the Pt electrode coated with polyaniline incorporated carbon particles films is an excellent indicator electrode. This electrode has advantages that the indicating signals are sharp and repeatable at end-point. The precision and the accuracy of the determination of polyisoprene alcohol are satisfactory.展开更多
This paper reports the determination of stability constants for complexes of Cd(Ⅱ)with Gly, Ala,Val,Asp,Gly—Asp,Asp Gly,Gly—Gly and Gly—Gly—Gly using both micro—pH—metric titra- tions and the application of con...This paper reports the determination of stability constants for complexes of Cd(Ⅱ)with Gly, Ala,Val,Asp,Gly—Asp,Asp Gly,Gly—Gly and Gly—Gly—Gly using both micro—pH—metric titra- tions and the application of convolution—deconvolution cyclic voltammetry at 25℃ and I=0.10 mol· dm^(-3)(KNO_3).Stability constants were calculated from pH—metric data using the SUPERQUAD com- puter program and cyclic voltammograms were collected,stored and manipulated using the EG and G CONDECON 300 software.A considerably larger ligand:metal ratio(e,g.50:1)was possible using voltammetry.Evaluation of results from the two techniques suggests that stability constants for the species[CdL_2]and[CdL_3]are reliable when calculated fromvoltammetry while those for[CdL]are more reliable when determined by pH-metric titration.展开更多
This paper reports a new method of titration for very weak acids and bases using the appearance of incisions on oscillopolarogram to indicate the end-point.This method has the advantages of rapidity,simplicity,no indi...This paper reports a new method of titration for very weak acids and bases using the appearance of incisions on oscillopolarogram to indicate the end-point.This method has the advantages of rapidity,simplicity,no indicator needed as well as good precision.展开更多
The pKa and the isosbestic point of the universal pH indicator Carlo Ebra 1-11 (catalog number 45712) were determined using UV-Vis spectrophotometry. Aqueous buffer solutions with pHs ranging from 3.83 to 10.85 were m...The pKa and the isosbestic point of the universal pH indicator Carlo Ebra 1-11 (catalog number 45712) were determined using UV-Vis spectrophotometry. Aqueous buffer solutions with pHs ranging from 3.83 to 10.85 were mixed. Four methods—two graphical and two mathematical— were used to estimate the acid dissociation constant (pKa) and isosbestic point using absorbance measurements. The equation for the dependence of the absorbance on pH at λ = 600 nm was obtained using calibration curves. The resulting average pKa of the four methods was 8.277 with a standard deviation of 0.1728. The results obtained using the mathematical methods were very similar, with a deviation of 0.0014;the average pKa determined using these methods was 8.263 ± 0.001. The literature contains no previous reports of the pKa of this indicator. The isosbestic point occurs at a wavelength of 494 nm, with an absorbance of 0.46.展开更多
Residual moisture is a key quality control parameter for lyophilized biologicals, as high moisture can correlate with poor stability. Coulometric Karl Fischer titration is the most widely used technology to determine ...Residual moisture is a key quality control parameter for lyophilized biologicals, as high moisture can correlate with poor stability. Coulometric Karl Fischer titration is the most widely used technology to determine residual water content;some chemicals are known to cause problems with Karl Fischer titration, but these chemicals do not usually occur in biologics. Three biological samples, of fibrinogen, heparin and Haemophilus influenza b polysaccharide, have caused particular issue in our hands by routine Karl Fischer analysis, illustrating different limitations with this method. The use of thermogravimetric analysis, with evolved gas mass spectrometric monitoring, is described here as a successful alternative for moisture analysis in these materials.展开更多
基金Supported by the Science and Technology Comm ission of Henan Province and Education Com mission of HenanProvince
文摘The feasibility of using electrodes modified with polyaniline incorporated carbon particles films for improving the precision of coulometric titration is demonstrated. The problem of large deviation produced during determining polyisoprene by coulometric titration with direct titration technique(double Pt electrodes indicating electrode) has been solved. In the titration process, polyisoprene alcohol, an electro-inactive species, is adsorbed on the surface of the bare Pt electrode, which inhibits the electrode reaction of Br - and Br 2. Therefore, when the titration reaches the end-point, the detected current will slowly change with time, which can make the repeatability of end-point poor. The atomic force microscopic images show the morphology of the electrode surface of adsorbing polyisoprene alcohol. The application of the chemically modified electrode instead of the bare Pt electrode to indicating the end-point has been investigated. The results show that the Pt electrode coated with polyaniline incorporated carbon particles films is an excellent indicator electrode. This electrode has advantages that the indicating signals are sharp and repeatable at end-point. The precision and the accuracy of the determination of polyisoprene alcohol are satisfactory.
文摘This paper reports the determination of stability constants for complexes of Cd(Ⅱ)with Gly, Ala,Val,Asp,Gly—Asp,Asp Gly,Gly—Gly and Gly—Gly—Gly using both micro—pH—metric titra- tions and the application of convolution—deconvolution cyclic voltammetry at 25℃ and I=0.10 mol· dm^(-3)(KNO_3).Stability constants were calculated from pH—metric data using the SUPERQUAD com- puter program and cyclic voltammograms were collected,stored and manipulated using the EG and G CONDECON 300 software.A considerably larger ligand:metal ratio(e,g.50:1)was possible using voltammetry.Evaluation of results from the two techniques suggests that stability constants for the species[CdL_2]and[CdL_3]are reliable when calculated fromvoltammetry while those for[CdL]are more reliable when determined by pH-metric titration.
文摘This paper reports a new method of titration for very weak acids and bases using the appearance of incisions on oscillopolarogram to indicate the end-point.This method has the advantages of rapidity,simplicity,no indicator needed as well as good precision.
文摘The pKa and the isosbestic point of the universal pH indicator Carlo Ebra 1-11 (catalog number 45712) were determined using UV-Vis spectrophotometry. Aqueous buffer solutions with pHs ranging from 3.83 to 10.85 were mixed. Four methods—two graphical and two mathematical— were used to estimate the acid dissociation constant (pKa) and isosbestic point using absorbance measurements. The equation for the dependence of the absorbance on pH at λ = 600 nm was obtained using calibration curves. The resulting average pKa of the four methods was 8.277 with a standard deviation of 0.1728. The results obtained using the mathematical methods were very similar, with a deviation of 0.0014;the average pKa determined using these methods was 8.263 ± 0.001. The literature contains no previous reports of the pKa of this indicator. The isosbestic point occurs at a wavelength of 494 nm, with an absorbance of 0.46.
文摘Residual moisture is a key quality control parameter for lyophilized biologicals, as high moisture can correlate with poor stability. Coulometric Karl Fischer titration is the most widely used technology to determine residual water content;some chemicals are known to cause problems with Karl Fischer titration, but these chemicals do not usually occur in biologics. Three biological samples, of fibrinogen, heparin and Haemophilus influenza b polysaccharide, have caused particular issue in our hands by routine Karl Fischer analysis, illustrating different limitations with this method. The use of thermogravimetric analysis, with evolved gas mass spectrometric monitoring, is described here as a successful alternative for moisture analysis in these materials.
