pH-fixed titration method for the determination of weak acids and bases has been studied in this paper.It is not necessary to know the ionization constant of weak acid or base and the concentration of titrant. This me...pH-fixed titration method for the determination of weak acids and bases has been studied in this paper.It is not necessary to know the ionization constant of weak acid or base and the concentration of titrant. This method had been applied to determine phenol,4-aminoantipyrine and glycine,whose ionization constants range from 10^(-10)to 10^(-12).The results were satisfactory.展开更多
Validating a method of analysis goes through different steps, which aims at testing the normality of measurements distribution, estimating the uncertainty of the components of a measurement (i.e., accuracy and correc...Validating a method of analysis goes through different steps, which aims at testing the normality of measurements distribution, estimating the uncertainty of the components of a measurement (i.e., accuracy and correctness), and finally, define the control tests of non degradation of the method performances. This paper outlines the steps for validating a biological method of analysis. It involves the construction of an experimental design, a statistical model, and the preparation of an interne laboratory reference material (pilot vaccine). The latter is used to study the impact of deviation and variation factors, in order to, optimize the analytical method, to evaluate the bias (random error), and to calculate the uncertainty of measurement, and make the control charts. This method is applied in the titration of live viral vaccines of Gumboro disease on chicken's embryos fibroblasts. The experimental results show that potential influence factors related to the titration method had no significant influence on the obtained results. Taking into account these results, an operating mode has been elaborated. The finalized method proved to be faithful to standard deviation of repeatability and reproducibility of 0.21 and 0.22, respectively, with a confidence level of 95%. The calculated uncertainty of measurement is equal to 0.2, which represents the average error level of a titer. A homogeneous stock of interne laboratory reference vaccine (MRIL), with an average titer of 5.9 log DIT 50, was produced and the control chart set in away to provide the laboratory with an important tool of control and monitoring of the viral titers evolution in time, as well as, the mastery of the validated titration method performances.展开更多
An equation describing the state of weak acid mixtures was derived from the relationships between mole balance and charge balance. The equation was solved with numerical method and the compositions of the acid mixture...An equation describing the state of weak acid mixtures was derived from the relationships between mole balance and charge balance. The equation was solved with numerical method and the compositions of the acid mixtures were determined. The advantages of this treatment were demonstrated by analyzing binary mixtures of chloroacetic, formic and acetic acids.展开更多
Despite the CaCO<sub>3</sub> estimation using titration method was not reliable, but up to the present time, some soil laboratories in Sudan still used this method. The objective of this study was to compa...Despite the CaCO<sub>3</sub> estimation using titration method was not reliable, but up to the present time, some soil laboratories in Sudan still used this method. The objective of this study was to compare and assess the results of calcimetric and titrimetric methods of quantitative estimation for soil calcium carbonate of different soils in Sudan. 26 soil samples from five soil profiles were collected from different climatological and ecological regions in central Sudan. CaCO<sub>3</sub> equivalent was estimated using calcimeter and titration methods in order to find accurate, rapid and suitable method for soils of Sudan. The results revealed that there are no significant differences between calcimeter and titration methods for calcium carbonate estimation in all studied samples except in samples from Gedaref area. We concluded that when the Calcimeter method used for CaCO<sub>3</sub> estimation, the differences between one person and another in detecting titration end point would be avoided, rapid and accurate results would be obtained compared to titration method. Additionally, time would be saved;fewer amounts of chemicals would be used. From this study, we highly recommend using calcimeter method for CaCO<sub>3</sub> estimation for soils of Sudan.展开更多
It has been found that the two-phase reactions of aqueous HCl, HOAc or H_3PO_4 with primary amine N_ 1923 in chloroform are oscillating reactions. Their power-time curves were measured by the titration microcalorimet...It has been found that the two-phase reactions of aqueous HCl, HOAc or H_3PO_4 with primary amine N_ 1923 in chloroform are oscillating reactions. Their power-time curves were measured by the titration microcalorimetric method, and the induction period (t_ in). The first oscillating period (t_ p.1) and the second oscillating period (t_ p.2) were determined. The apparent activating parameters and the orders of the oscillating systems were calculated and the following relationships were established: for the oscillating system of hydrochloric acid t_ in∝c 0.147_ HClexp(1.35×10 3T), t_ p.1∝c 0.241_ HCl· exp(4.33×10 3T), t_ p.2∝c 0.290_ HClexp(5.59×10 3T); for the oscillating system of acetic acid, t_ in∝c 0.883_ HOAcexp(2.32×10 3T), t_ p.1∝c 0.399_ HOAc· exp(4.50×10 3T), t_ p.2∝c 0.301_ HOAcexp(5.88×10 3T); for the oscillating system of phosphoric acid, t_ in∝c 1.14_ H_3PO_4exp(7.70×10 4T), t_ p.1∝c 1.42_ H_3PO_4exp(1.14×10 4T), t_ p.2∝c 1.47_ H_3PO_4exp(1.27×10 4T).展开更多
Objective:There are some anthraquinones,anthraquinones and flavonones in Sennae Folium which exhibited significant acidity,such as sennoside A/B and sennoside C/D.The current strategies used in separating these compon...Objective:There are some anthraquinones,anthraquinones and flavonones in Sennae Folium which exhibited significant acidity,such as sennoside A/B and sennoside C/D.The current strategies used in separating these components are mainly based on conventional column chromatography which is time consuming,laborious and costly.This study is aimed at exploring a method of precipitation extraction of acid components in Sennae Folium.Using alkaloid as a"hook",it is reasonable to use the principle of"acid-alkali complexation"to"fish"the acidic components in Sennae Folium.Methods:Isothermal titration calorimeter(ITC)was used to measure the extraction efficiency of different alkaloids.Then,alkaloid determined by ITC was mixed with extracting solution of Sennae Folium to form complex.High performance liquid chromatography coupled with mass spectrometry(HPLC-MS2)was used to investigate the ingredients"fished"by berberine(Ber).The mechanism of"fishing"process was explained by ITC,optical activity,fluorescence spectrometry and scanning electron microscope.Results:The ITC results proved that the choice of"hook"was particularly important in the process of"fishing".Among the hooks,the fishing efficiency of the isoquinoline alkaloids(Ber)was the highest,reaching 10.3%.Nine ingredients were detected and determined by HPLC-MS2,and the main components were sennoside A/B and sennoside C/D.Based on ITC test of Ber and sennoside A,the combination mechanism of the two ingredients was a chemical reaction with a nearly binding ratio(2:1).Fluorescence and optical properties of the active ingredients were changed after complexation.By scanning electron microscope,we found that two types of components had obviously self-assembled behavior during the formation process.Conclusion:Ber successfully"fished"the main acidic components,sennoside A/B and sennoside C/D,from Sennae Folium.Combined with different characterizations,the"fishing"process was determined as a chemical association reaction induced by electrostatic interaction orπ-πstacking.Therefore,with special identification ability,the"fishing"process had the potential of practical application.展开更多
文摘pH-fixed titration method for the determination of weak acids and bases has been studied in this paper.It is not necessary to know the ionization constant of weak acid or base and the concentration of titrant. This method had been applied to determine phenol,4-aminoantipyrine and glycine,whose ionization constants range from 10^(-10)to 10^(-12).The results were satisfactory.
文摘Validating a method of analysis goes through different steps, which aims at testing the normality of measurements distribution, estimating the uncertainty of the components of a measurement (i.e., accuracy and correctness), and finally, define the control tests of non degradation of the method performances. This paper outlines the steps for validating a biological method of analysis. It involves the construction of an experimental design, a statistical model, and the preparation of an interne laboratory reference material (pilot vaccine). The latter is used to study the impact of deviation and variation factors, in order to, optimize the analytical method, to evaluate the bias (random error), and to calculate the uncertainty of measurement, and make the control charts. This method is applied in the titration of live viral vaccines of Gumboro disease on chicken's embryos fibroblasts. The experimental results show that potential influence factors related to the titration method had no significant influence on the obtained results. Taking into account these results, an operating mode has been elaborated. The finalized method proved to be faithful to standard deviation of repeatability and reproducibility of 0.21 and 0.22, respectively, with a confidence level of 95%. The calculated uncertainty of measurement is equal to 0.2, which represents the average error level of a titer. A homogeneous stock of interne laboratory reference vaccine (MRIL), with an average titer of 5.9 log DIT 50, was produced and the control chart set in away to provide the laboratory with an important tool of control and monitoring of the viral titers evolution in time, as well as, the mastery of the validated titration method performances.
文摘An equation describing the state of weak acid mixtures was derived from the relationships between mole balance and charge balance. The equation was solved with numerical method and the compositions of the acid mixtures were determined. The advantages of this treatment were demonstrated by analyzing binary mixtures of chloroacetic, formic and acetic acids.
文摘Despite the CaCO<sub>3</sub> estimation using titration method was not reliable, but up to the present time, some soil laboratories in Sudan still used this method. The objective of this study was to compare and assess the results of calcimetric and titrimetric methods of quantitative estimation for soil calcium carbonate of different soils in Sudan. 26 soil samples from five soil profiles were collected from different climatological and ecological regions in central Sudan. CaCO<sub>3</sub> equivalent was estimated using calcimeter and titration methods in order to find accurate, rapid and suitable method for soils of Sudan. The results revealed that there are no significant differences between calcimeter and titration methods for calcium carbonate estimation in all studied samples except in samples from Gedaref area. We concluded that when the Calcimeter method used for CaCO<sub>3</sub> estimation, the differences between one person and another in detecting titration end point would be avoided, rapid and accurate results would be obtained compared to titration method. Additionally, time would be saved;fewer amounts of chemicals would be used. From this study, we highly recommend using calcimeter method for CaCO<sub>3</sub> estimation for soils of Sudan.
基金ProjectsupportedbytheNaturalScienceFoundationofShandongProvince (No .Y2 0 0 0B0 3)
文摘It has been found that the two-phase reactions of aqueous HCl, HOAc or H_3PO_4 with primary amine N_ 1923 in chloroform are oscillating reactions. Their power-time curves were measured by the titration microcalorimetric method, and the induction period (t_ in). The first oscillating period (t_ p.1) and the second oscillating period (t_ p.2) were determined. The apparent activating parameters and the orders of the oscillating systems were calculated and the following relationships were established: for the oscillating system of hydrochloric acid t_ in∝c 0.147_ HClexp(1.35×10 3T), t_ p.1∝c 0.241_ HCl· exp(4.33×10 3T), t_ p.2∝c 0.290_ HClexp(5.59×10 3T); for the oscillating system of acetic acid, t_ in∝c 0.883_ HOAcexp(2.32×10 3T), t_ p.1∝c 0.399_ HOAc· exp(4.50×10 3T), t_ p.2∝c 0.301_ HOAcexp(5.88×10 3T); for the oscillating system of phosphoric acid, t_ in∝c 1.14_ H_3PO_4exp(7.70×10 4T), t_ p.1∝c 1.42_ H_3PO_4exp(1.14×10 4T), t_ p.2∝c 1.47_ H_3PO_4exp(1.27×10 4T).
基金funded by Beijing Natural Science Foundation(No.7202116)National Natural Science Foundation of China(No.81603256)+2 种基金Project of China Association of Chinese Medicine(CACM-2018-QNRC2B08)the Fundamental Research Funds for the Central Universities(BUCM-2019-JCRC002,2019-JYB-TD005,and BUCM-2018-2021)Beijing Key Laboratory for Basic and Development Research on Chinese Medicine(Beijing,100102)。
文摘Objective:There are some anthraquinones,anthraquinones and flavonones in Sennae Folium which exhibited significant acidity,such as sennoside A/B and sennoside C/D.The current strategies used in separating these components are mainly based on conventional column chromatography which is time consuming,laborious and costly.This study is aimed at exploring a method of precipitation extraction of acid components in Sennae Folium.Using alkaloid as a"hook",it is reasonable to use the principle of"acid-alkali complexation"to"fish"the acidic components in Sennae Folium.Methods:Isothermal titration calorimeter(ITC)was used to measure the extraction efficiency of different alkaloids.Then,alkaloid determined by ITC was mixed with extracting solution of Sennae Folium to form complex.High performance liquid chromatography coupled with mass spectrometry(HPLC-MS2)was used to investigate the ingredients"fished"by berberine(Ber).The mechanism of"fishing"process was explained by ITC,optical activity,fluorescence spectrometry and scanning electron microscope.Results:The ITC results proved that the choice of"hook"was particularly important in the process of"fishing".Among the hooks,the fishing efficiency of the isoquinoline alkaloids(Ber)was the highest,reaching 10.3%.Nine ingredients were detected and determined by HPLC-MS2,and the main components were sennoside A/B and sennoside C/D.Based on ITC test of Ber and sennoside A,the combination mechanism of the two ingredients was a chemical reaction with a nearly binding ratio(2:1).Fluorescence and optical properties of the active ingredients were changed after complexation.By scanning electron microscope,we found that two types of components had obviously self-assembled behavior during the formation process.Conclusion:Ber successfully"fished"the main acidic components,sennoside A/B and sennoside C/D,from Sennae Folium.Combined with different characterizations,the"fishing"process was determined as a chemical association reaction induced by electrostatic interaction orπ-πstacking.Therefore,with special identification ability,the"fishing"process had the potential of practical application.