As a mono-sodium salt form of alendronic acid,alendronate sodium presents multi-level ionization for the dissociation of its four hydroxyl groups.The dissociation constants of alendronate sodium were determined in thi...As a mono-sodium salt form of alendronic acid,alendronate sodium presents multi-level ionization for the dissociation of its four hydroxyl groups.The dissociation constants of alendronate sodium were determined in this work by studying the piecewise linear relationship between volume of titrant and p H value based on acidbase potentiometric titration reaction.The distribution curves of alendronate sodium were drawn according to the determined p Ka values.There were 4 dissociation constants(pKa_1=2.43,pKa_2=7.55,pKa_3=10.80,pKa_4=11.99,respectively) of alendronate sodium,and 12 existing forms,of which 4 could be ignored,existing in different p H environments.展开更多
In water treatment processes and conditioning drinking water, PEs are widely used;however, their environmental impact is still doubtful, since residual concentrations increase organic matter content and represents a p...In water treatment processes and conditioning drinking water, PEs are widely used;however, their environmental impact is still doubtful, since residual concentrations increase organic matter content and represents a potential health hazard. This paper demonstrates a multiparametric study of two colloidal titration methods: spectrophotometric and zeta potential end point detection. The first one was optimized to guarantee the accuracy of cationic commercial PE quantification. It includes the indicator dose optimization using analytical criteria for competing equilibria, a calibration curve for two ranges of CPE concentration (1 - 5 ppm and 5 - 100 ppm) and the interference study of flocculant and Sn in the CPE quantification. The second method provides a physicochemical validation of the electric surface phenomena occurring during the colloidal titration and the end point detection. As an additional contribution the zeta potential titration was discussed and proposed as an alternative method for quantifying CPE when the sample is metal free.展开更多
In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and mate...In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and materials based on coulometric titration GET 176-2010 are given. Primary reference materials certified by coulometric titration in the Ural Scientific and Research Institute for Metrology include eight certified reference materials (CRMs) of pure solid substances (mostly salts of sodium or potassium) and one hydrochloric acid solution CRM. The metrological characteristics of these reference materials and the scheme of their application in titrimetric analysis are shown. The expanded uncertainty of the certified value (mass fraction for the solid substances or molar concentration for the solution) is in the range from 0.018% to 0.05%. Information about two primary reference materials of high purity iron and lead nitrate certified by controlled-potential coulometry with expanded uncertainty from 0.04% to 0.07% is also given.展开更多
The potentiostatic intermittent titration technique(PITT)is widely used to determine the diffusion coefficient of ions in electrode materials for rechargeable batteries such as lithium-ion or sodium-ion batteries,pred...The potentiostatic intermittent titration technique(PITT)is widely used to determine the diffusion coefficient of ions in electrode materials for rechargeable batteries such as lithium-ion or sodium-ion batteries,predicated on the assumption that the insertion/extraction of ions in the host materials is governed by diffusion.However,in practical scenarios,the electrochemical process might be dominated by interfacial reaction kinetics rather than diffusion.The present work derives analytical equations for electric current by considering the finite interfacial reaction kinetics and small overpotentials during PITT measurements and further studies the chemical stress field induced by the interfacial reaction-controlled ion insertion.The exchange current density(j_(0))can be ascertained using the analytical equation,which dictates the magnitude and decay rate of the electric current during a PITT process.The electric current decays more rapidly,and consequently,the lithium concentration reaches equilibrium faster for larger values of j_(0).The magnitude of the chemical stress is independent of j_(0) but depends on the overpotential.展开更多
BACKGROUND Effective pain management after radical gastrectomy is crucial for patient recovery.With the promotion of enhanced recovery after surgery protocols,postoperative pain management has become a core component ...BACKGROUND Effective pain management after radical gastrectomy is crucial for patient recovery.With the promotion of enhanced recovery after surgery protocols,postoperative pain management has become a core component of perioperative care.However,controversy remains regarding the optimal frequency of analgesic titration for pain control.AIM To compare the efficacy of 12-hour vs 24-hour titration regimens in postoperative pain management following radical gastrectomy for gastric cancer.METHODS This retrospective comparative study analyzed data from 120 patients who underwent radical gastrectomy between January 2021 and December 2022,with 52 patients receiving a 12-hour titration regimen and 68 patients receiving a 24-hour titration regimen.All patients received patient-controlled intravenous analgesia containing sufentanil and tropisetron postoperatively with identical initial settings.RESULTS The 12-hour titration group demonstrated significantly lower pain scores at 12 hours postoperatively compared to the 24-hour group(3.2 vs 4.8,P<0.001);total analgesic consumption(morphine equivalents)was reduced by 28.6%(30 mg vs 42 mg,P<0.001);postoperative nausea and vomiting decreased by 50%(15%vs 30%,P=0.02);respiratory depression was less frequent(2%vs 8%,P=0.04);patient satisfaction was higher(85%vs 65%reporting“very satisfied”or“satisfied”,P<0.001);and hospital stay was shortened by 12.5%(4.2 days vs 4.8 days,P=0.02).Cox regression analysis showed that the 12-hour regimen was associated with a lower risk of prolonged high-intensity pain(hazard ratio=0.65,95%confidence interval:0.45-0.93,P=0.02),and multivariate regression analysis confirmed that the 12-hour regimen was an independent predictor of better overall recovery(β=-0.32,P=0.01).CONCLUSION Compared to the 24-hour titration regimen,the 12-hour titration regimen provided more effective control of early postoperative pain after radical gastrectomy,reduced total analgesic consumption,lowered the incidence of related adverse reactions,improved patient satisfaction,and shortened hospital stays.展开更多
Amount and properties of roots surface charge are important for nutrient uptake and balance in plants. Roots surface charge markedly varies at different rizosphere conditions (particularly pH and ionic strength), whic...Amount and properties of roots surface charge are important for nutrient uptake and balance in plants. Roots surface charge markedly varies at different rizosphere conditions (particularly pH and ionic strength), which can markedly alter during vegetation season. Among recently available measuring methods, surface charge-pH dependence of roots (as well as other biological objects) is most easily evaluated by potentiometric titration. Use of this method is also easy at different ionic strengths. Potentiometric titration also allows for estimation of the distribution of charge generating surface groups. However, many applications of this method seem to be based either on incorrect methodical or theoretical approaches. In this paper we discuss the methodical and theoretical backgrounds of the titration method. Basing on experimental titration curves of roots of barley grown in nutrient solution, we show inconsistency of surface charge results obtained at different measuring conditions. Limitations of theoretical interpretations of the results are outlined also.展开更多
This study investigated a natural indicator for acid-base titration which is extracted from guinea corn leaves popularly called “waakye leaves” in Ghana. Four types of acid-base titration were studied: strong acid v...This study investigated a natural indicator for acid-base titration which is extracted from guinea corn leaves popularly called “waakye leaves” in Ghana. Four types of acid-base titration were studied: strong acid versus (v/s) strong base, strong acid versus weak base, weak acid versus strong base, and weak acid versus weak base. The indicator color change, pH range and the average titre values were determined for each type of acid-base titration. These values were comparable to those obtained from three standard indicators: methyl orange, methyl red and phenolphthalein. Total flavonoids (TF) and condensed tannin (CT) from the crude leaves extract were determined which might be the major reasons for the activity of the extract as an indicator for simple acid-base titration. The authors suggest that the natural indicator is cheap, available, simple to extract, user and environmentally friendly and could be an excellent replacement for standard indicators.展开更多
Rocky desertification has become a major environmental issue in the karst region of southwestern China.Karst rocky desertification was more severe in regions of limestone soil than in adjacent regions of other soils,d...Rocky desertification has become a major environmental issue in the karst region of southwestern China.Karst rocky desertification was more severe in regions of limestone soil than in adjacent regions of other soils,despite the relatively higher soil organic matter(SOM)content in limestone soil.The underlying mechanism remains ambiguous.We speculated that the geochemical characteristics of limestone soils in the karst region plays an essential role,especially the high calcium content of limestone soil.To test this hypothesis,we collected limestone soil samples from a limestone soil profile in the southwestern China karst region and extracted humic acid(HA)from these limestone soil samples.We investigated the interaction of Ca^(2+)and three HA samples on a joint experimental platform,which consists of an automatic potentiometric titrator,a UV–visible spectrometer,and a Fluorescence spectrometer.HA solutions were titrated by Ca^(2+)and optical spectra of the HA solutions were monitored during the titration experiments.The results indicated that:(1)the interaction of Ca^(2+)and HA is a combined process of adsorption and complexation.Adsorption dominated the overall distribution behavior of Ca^(2+),which could be fit by Langmuir and Freundlich isotherm models.Complexation was distinguished only when the concentration of Ca2+is low;(2)the changes of UV–visible spectroscopy and excitation–emission matrix fluorescencespectroscopy spectra of HA samples when they were binding with Ca^(2+)implied the apparent molecular size and structure of HA became larger and more complex;(3)the combination of Ca^(2+)and HA plays an important role in the SOM preservation of limestone soils but the stability of the Ca–HA association was relatively weak.The present study draws attention to maintaining the relatively higher Ca^(2+)concentration in limestone soils in ecologic restoration attempts in karst regions.展开更多
By using calcium ion selective elatrode (Ca ISE) as indicating electrode, saturated calomel electrode (SCE) as reference electrode and EGTA as titrant, calcium in seawater was determined by potentiometric titration in...By using calcium ion selective elatrode (Ca ISE) as indicating electrode, saturated calomel electrode (SCE) as reference electrode and EGTA as titrant, calcium in seawater was determined by potentiometric titration in borate buffer solution. This method can reduce observation errors in the determination of the endpoint, and thus provide better analytical precision(<0.08%) than present complexometric titration.展开更多
Introduction: Only vindication of a nasal continuous positive airway pressure (CPAP) retitration procedure will be an actual change in the optimal CPAP pressure after that test. The purpose of this study was to identi...Introduction: Only vindication of a nasal continuous positive airway pressure (CPAP) retitration procedure will be an actual change in the optimal CPAP pressure after that test. The purpose of this study was to identify any items in patient characteristics, clinical features, baseline PSG and initial CPAP titration as predictors of change in optimal pressure on CPAP retitration. Methods: 46 patients with obstructive sleep apnea (OSA) were divided in two groups: Group I (optimal pressure was changed on CPAP retitration): N = 30, M 22 and F 8, age 31-72, BMI 26-50 Kg/m2, neck size 15 – 20', tonsillectomy in 8, narrow oropharynx in 15, uvuvlopalatopharyngoplasty (UP3) in 2, abnormal chin in 3, deviated nasal septum (DNS) and prior nose surgery in 1 each, initial CPAP pressure 6-19 cm, sleep efficiency 65%-98%, REM latency 0-304 minutes and residual apnea hypopnea index (AHI) 0-23/hour. Group II (optimal pressure unchanged after CPAP retitration): N = 16, M 11 and 5 F, age 32-69, BMI 23-62 Kg/m2, neck size 14.5-20', tonsillectomy in 6, narrow oropharynx in 5, abnormal chin in 4, corrective nasal surgery in 2, DNS in 1, initial CPAP pressure 8-13 cm of H2O, sleep efficiency 69%-95%, REM latency 0-270 minutes and residual AHI 0-19/hour. The statistical analyses were performed using two-tailed Fisher’s t test and unpaired t test. A p value of <0.05 was considered statistically significant. Results: Patient characteristics (age, gender, neck size, and BMI), clinical features (tonsillar status, oropharyngeal narrowing, chin abnormality, DNS/nasal surgery or UP3), baseline PSG or initial CPAP titration (sleep efficiency, REM latency, residual AHI and initial CPAP pressure) did not differ significantly between the 2 groups (p = 0.09-0.99). Conclusion: Patient characteristics, clinical features or variables on baseline PSG and initial CPAP titration do not predict a change in optimal pressure on CPAP retitration. The results suggest that 1) Significant weight change;2) Patient’s subjective feeling of pressure being too high or insufficient;3) Residual or recurrent daytime sleepiness uncorrected by interface readjustments;4)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
Polyphenols are naturally occurring compounds found largely in fruits, vegetables, cereals and beverages. Currently, there is much interest in the potential health benefits of dietary plant polyphenols as antioxidants...Polyphenols are naturally occurring compounds found largely in fruits, vegetables, cereals and beverages. Currently, there is much interest in the potential health benefits of dietary plant polyphenols as antioxidants. The effect of polyphenols on human cancer cells is most often protective and induces a reduction in the number of tumors or rate of growth. During our course of study on anticancer prodrugs, twelve triphenylmethanol and one tris(2-(hydroxymethyl) phenol derivatives were synthesized as a carrier of several drugs with optimized lipophilicity. Besides application of these compounds as a foundation for anticancer drug delivery systems, these compounds were evaluated as indicators for the acid-base volumetric titration of a standard solution of hydrochloric acid with a standard solution of sodium hydroxide. The experiments indicated a moderate-to-sharp color transition of the solutions near the neutralization point for most indicators. These indicators may have potential applications for acid-base titrations in a narrow range.展开更多
The mixed dissociation constant of azathioprine—chemically 6-(3-methyl-5-nitroimidazol-4-yl)sulfanyl-7H- purine at various ionic strengths I of range 0.01-0.2, and at temperatures of 25℃ and 37℃, was determined wit...The mixed dissociation constant of azathioprine—chemically 6-(3-methyl-5-nitroimidazol-4-yl)sulfanyl-7H- purine at various ionic strengths I of range 0.01-0.2, and at temperatures of 25℃ and 37℃, was determined with the use of two different multiwavelength and multivariate treatments of spectral data, SPECFIT32 and SQUAD(84) nonlinear regression analyses and INDICES factor analysis according to a general rule. First, the number of components is determined, and then the spectral responses and concentrations of the components are calculated. Concurrently, the experimental determination of the thermodynamic dissociation constant was in agreement with its computational prediction of the PALLAS programme based on knowledge of the chemical structures of the drug. The factor analysis in the INDICES programme predicts the correct number of two light-absorbing species L- and HL. The thermodynamic dissociation constant of azathioprine was estimated by nonlinear regression of {pKa, I} data, = 8.07(1) at 25℃ and 7.84(1) at 37℃, where the figure in brackets is the standard deviation in last significant digits. The reliability of the dissociation constants of azathioprine was proven with goodness-of-fit tests of the multiwavelength spectrophotometric pH-titration data.展开更多
Impedance titration was used to determine the surface dissociation characteristics of short-chain carboxyl mercaptan self-assembled monolayers （SAMs）. Based on the change of the cyclic voltammetric peak current and ...Impedance titration was used to determine the surface dissociation characteristics of short-chain carboxyl mercaptan self-assembled monolayers （SAMs）. Based on the change of the cyclic voltammetric peak current and the charge-transfer resistance, which was related to pH value of the solution, the surface pKa of mercaptoacetic acid（MA）, 3-mercaptopropionic acid（MPA） and ω-mercaptohexanic acid（MHA） self-assembled membranes, with ionic strength being 0.1 mol/L, were determined to be 5.20, 4.80, 7.40, respectively. In addition, factors such as time needed for assembling, structure of monolayers and ionic strength, which effected the surface pKa, were studied as well. Such surface pKa shifts were sufficiently explained by interactions between interfacial molecules and hydrophobicity.展开更多
Bacterial small laccases(SLAC) are promising industrial biocatalysts due to their ability to oxidize a broad range of substrates with exceptional thermostability and tolerance for alkaline p H. Electron transfer betwe...Bacterial small laccases(SLAC) are promising industrial biocatalysts due to their ability to oxidize a broad range of substrates with exceptional thermostability and tolerance for alkaline p H. Electron transfer between substrate, copper centers, and O2is one of the key steps in the catalytic turnover of SLAC. However, limited research has been conducted on the electron transfer pathway of SLAC and SLAC-catalyzed reactions, hindering further engineering of SLAC to produce tunable biocatalysts for novel applications. Herein, the combinational use of electron paramagnetic resonance(EPR) and ultraviolet-visible(UV-vis) spectroscopic methods coupled with redox titration were employed to monitor the electron transfer processes and obtain further insights into the electron transfer pathway in SLAC. The reduction potentials for type 1 copper(T1Cu), type 2 copper(T2Cu) and type 3copper(T3Cu) were determined to be 367 ± 2 mV, 378 ± 5 m V and 403 ± 2 mV,respectively. Moreover, the reduction potential of a selected substrate of SLAC, hydroquinone(HQ), was determined to be 288 mV using cyclic voltammetry(CV). In this way, an electron transfer pathway was identified based on the reduction potentials. Specifically,electrons are transferred from HQ to T1Cu, then to T2Cu and T3Cu, and finally to O2.Furthermore, superhyperfine splitting observed via EPR during redox titration indicated a modification in the covalency of T2Cu upon electron uptake, suggesting a conformational alteration in the protein environment surrounding the copper sites, which could potentially influence the reduction potential of the copper sites during catalytic processes. The results presented here not only provide a comprehensive method for analyzing the electron transfer pathway in metalloenzymes through reduction potential measurements, but also offer valuable insights for further engineering and directed evolution studies of SLAC in the aim for biotechnological and industrial applications.展开更多
Paraquat （PQ）, a nonselective herbicide, is non-fluorescent in aqueous solutions. Thus, its determination through direct fluorescent methods is not feasible. The supramolecular inclusion interaction of PQ with cucur...Paraquat （PQ）, a nonselective herbicide, is non-fluorescent in aqueous solutions. Thus, its determination through direct fluorescent methods is not feasible. The supramolecular inclusion interaction of PQ with cucurbit[7]uril was studied by a fluorescent probe titration method. Significant quenching of the fluorescence intensity of the cucurbit[7]uril-coptisine fluorescent probe was observed with the addition of PQ. A new fluorescent probe titration method with high selectivity and sensitivity at the ng/mL level was developed to determine PQ in aqueous solutions with good precision and accuracy based on the significant quenching of the supramolecular complex fluorescence intensity. The proposed method was successfully used in the determination of PQ in lake water, tap water, well water, and ditch water in an agricultural area, with recoveries of 96.73% to 105.77%. The fluorescence quenching values （AF） showed a good linear relationship with PQ concentrations from 1.0 × 10^-8 to 1.2× 10^-5 mol/L with a detection limit of 3.35 x 10-9 mol/L. In addition, the interaction models of the supramolecular complexes formed between the host and the vip were established using theoretical calculations. The interaction mechanism between the cucurbit[7]uril and PQ was confirmed by 1H NMR spectroscopy.展开更多
The stability constants and thermodynamic functions for complexes of lanthanum with eight kind of amino acids according to 1∶1 and 1∶2 in proportion have been determined by titration calorimeter at 298.15 K. The ent...The stability constants and thermodynamic functions for complexes of lanthanum with eight kind of amino acids according to 1∶1 and 1∶2 in proportion have been determined by titration calorimeter at 298.15 K. The enthalpy change makes a predominant contribution to the stability of these complexes. The ring in amino acid associated with lanthanum ion helps to enhance the stability of complexes. Steric effects between rings in complexes leads to that the equilibrium constants of reaction of the complexes (1∶2) is much less than that of the complexes (1∶1).展开更多
Objective: to compare the difference between potentiometric titration and indicator titration in the determination of total organic acids in hawthorn. Methods: potentiometric titration and indicator titration were use...Objective: to compare the difference between potentiometric titration and indicator titration in the determination of total organic acids in hawthorn. Methods: potentiometric titration and indicator titration were used to determine the content of total organic acids in different batches of hawthorn, and the differences in precision, repeatability, stability and recovery between the two methods were compared. Results: the repeatability and stability of potentiometric titration were higher than that of indicator titration. The recovery rate of potentiometric titration was 97.61%, and that of indicator titration was 96.96%. Potentiometric titration is easier to eliminate the interference of Hawthorn water extract color on titration end point. Conclusion: potentiometric titration is better than indicator method in the determination of total organic acids in hawthorn with color interference.展开更多
The precursors of La0.7Sr0.3-xCaxCo0.9Fe0.1O3-δ(LSCCF, x=0.05, 0.10, 0.15, 0.20) as the cathode materials for intermediate temperature solid oxide fuel cell (ITSOFC) were prepared by reverse titration co-precipitatio...The precursors of La0.7Sr0.3-xCaxCo0.9Fe0.1O3-δ(LSCCF, x=0.05, 0.10, 0.15, 0.20) as the cathode materials for intermediate temperature solid oxide fuel cell (ITSOFC) were prepared by reverse titration co-precipitation method with metal-nitrates as starting materials and mixed alkali (NaOH and Na2CO3) as a precipitating agent. The formation process of LSCCF from the precursors was monitored by TG-DSC, and the crystal structure and particles morphology of the precursors which were calcined at 600, 800, 1000 ℃ for 3 h were characterized using XRD, SEM technologies. Compared with the solid state reaction of constituent oxides, when the pH value of the precipitating solution was in the range of 9.1～9.5, the LSCCF powders from the precursors caclined at 800 ℃ for 3 h had high purity, homogeneous and single perovskite phase. The electrical conductivity of the LSCCF samples sintered at 1200 ℃ for 3 h, which was measured as a function of temperatures from 100 to 800 ℃ by DC four-probe method in air, decreased with x from 0.05 to 0.20. The value of electrical conductivity was almost equal because of Ca2+, Sr2+ co-dopant resulting in the 'mix effect' while x=0.10 or 0.15. The electrical conductivity of all doped samples was higher than 100 S·cm-1 at intermediate temperatures from 500 to 800 ℃, and there was good compatibility between the LSCCF cathode and Ce0.8Sm0.2O2 electrolyte.展开更多
基金the support of Key Laboratory of Chinese Medicine Preparation of Solid Dispersion,Gansu Longshenrongfa Pharmaceutical Industry Co.,Ltd.,Gansu Province,China
文摘As a mono-sodium salt form of alendronic acid,alendronate sodium presents multi-level ionization for the dissociation of its four hydroxyl groups.The dissociation constants of alendronate sodium were determined in this work by studying the piecewise linear relationship between volume of titrant and p H value based on acidbase potentiometric titration reaction.The distribution curves of alendronate sodium were drawn according to the determined p Ka values.There were 4 dissociation constants(pKa_1=2.43,pKa_2=7.55,pKa_3=10.80,pKa_4=11.99,respectively) of alendronate sodium,and 12 existing forms,of which 4 could be ignored,existing in different p H environments.
文摘In water treatment processes and conditioning drinking water, PEs are widely used;however, their environmental impact is still doubtful, since residual concentrations increase organic matter content and represents a potential health hazard. This paper demonstrates a multiparametric study of two colloidal titration methods: spectrophotometric and zeta potential end point detection. The first one was optimized to guarantee the accuracy of cationic commercial PE quantification. It includes the indicator dose optimization using analytical criteria for competing equilibria, a calibration curve for two ranges of CPE concentration (1 - 5 ppm and 5 - 100 ppm) and the interference study of flocculant and Sn in the CPE quantification. The second method provides a physicochemical validation of the electric surface phenomena occurring during the colloidal titration and the end point detection. As an additional contribution the zeta potential titration was discussed and proposed as an alternative method for quantifying CPE when the sample is metal free.
文摘In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and materials based on coulometric titration GET 176-2010 are given. Primary reference materials certified by coulometric titration in the Ural Scientific and Research Institute for Metrology include eight certified reference materials (CRMs) of pure solid substances (mostly salts of sodium or potassium) and one hydrochloric acid solution CRM. The metrological characteristics of these reference materials and the scheme of their application in titrimetric analysis are shown. The expanded uncertainty of the certified value (mass fraction for the solid substances or molar concentration for the solution) is in the range from 0.018% to 0.05%. Information about two primary reference materials of high purity iron and lead nitrate certified by controlled-potential coulometry with expanded uncertainty from 0.04% to 0.07% is also given.
基金supported by the National Natural Science Foundation of China(No.12374003)the Guangdong Basic and Applied Basic Research Foundation(No.2024A1515030256)the Shenzhen Science and Technology Program(Grant Nos.JCYJ20220531095208019 and GXWD20231129103124001).
文摘The potentiostatic intermittent titration technique(PITT)is widely used to determine the diffusion coefficient of ions in electrode materials for rechargeable batteries such as lithium-ion or sodium-ion batteries,predicated on the assumption that the insertion/extraction of ions in the host materials is governed by diffusion.However,in practical scenarios,the electrochemical process might be dominated by interfacial reaction kinetics rather than diffusion.The present work derives analytical equations for electric current by considering the finite interfacial reaction kinetics and small overpotentials during PITT measurements and further studies the chemical stress field induced by the interfacial reaction-controlled ion insertion.The exchange current density(j_(0))can be ascertained using the analytical equation,which dictates the magnitude and decay rate of the electric current during a PITT process.The electric current decays more rapidly,and consequently,the lithium concentration reaches equilibrium faster for larger values of j_(0).The magnitude of the chemical stress is independent of j_(0) but depends on the overpotential.
基金Supported by Wenzhou Science and Technology Bureau,No.Y20220877.
文摘BACKGROUND Effective pain management after radical gastrectomy is crucial for patient recovery.With the promotion of enhanced recovery after surgery protocols,postoperative pain management has become a core component of perioperative care.However,controversy remains regarding the optimal frequency of analgesic titration for pain control.AIM To compare the efficacy of 12-hour vs 24-hour titration regimens in postoperative pain management following radical gastrectomy for gastric cancer.METHODS This retrospective comparative study analyzed data from 120 patients who underwent radical gastrectomy between January 2021 and December 2022,with 52 patients receiving a 12-hour titration regimen and 68 patients receiving a 24-hour titration regimen.All patients received patient-controlled intravenous analgesia containing sufentanil and tropisetron postoperatively with identical initial settings.RESULTS The 12-hour titration group demonstrated significantly lower pain scores at 12 hours postoperatively compared to the 24-hour group(3.2 vs 4.8,P<0.001);total analgesic consumption(morphine equivalents)was reduced by 28.6%(30 mg vs 42 mg,P<0.001);postoperative nausea and vomiting decreased by 50%(15%vs 30%,P=0.02);respiratory depression was less frequent(2%vs 8%,P=0.04);patient satisfaction was higher(85%vs 65%reporting“very satisfied”or“satisfied”,P<0.001);and hospital stay was shortened by 12.5%(4.2 days vs 4.8 days,P=0.02).Cox regression analysis showed that the 12-hour regimen was associated with a lower risk of prolonged high-intensity pain(hazard ratio=0.65,95%confidence interval:0.45-0.93,P=0.02),and multivariate regression analysis confirmed that the 12-hour regimen was an independent predictor of better overall recovery(β=-0.32,P=0.01).CONCLUSION Compared to the 24-hour titration regimen,the 12-hour titration regimen provided more effective control of early postoperative pain after radical gastrectomy,reduced total analgesic consumption,lowered the incidence of related adverse reactions,improved patient satisfaction,and shortened hospital stays.
文摘Amount and properties of roots surface charge are important for nutrient uptake and balance in plants. Roots surface charge markedly varies at different rizosphere conditions (particularly pH and ionic strength), which can markedly alter during vegetation season. Among recently available measuring methods, surface charge-pH dependence of roots (as well as other biological objects) is most easily evaluated by potentiometric titration. Use of this method is also easy at different ionic strengths. Potentiometric titration also allows for estimation of the distribution of charge generating surface groups. However, many applications of this method seem to be based either on incorrect methodical or theoretical approaches. In this paper we discuss the methodical and theoretical backgrounds of the titration method. Basing on experimental titration curves of roots of barley grown in nutrient solution, we show inconsistency of surface charge results obtained at different measuring conditions. Limitations of theoretical interpretations of the results are outlined also.
文摘This study investigated a natural indicator for acid-base titration which is extracted from guinea corn leaves popularly called “waakye leaves” in Ghana. Four types of acid-base titration were studied: strong acid versus (v/s) strong base, strong acid versus weak base, weak acid versus strong base, and weak acid versus weak base. The indicator color change, pH range and the average titre values were determined for each type of acid-base titration. These values were comparable to those obtained from three standard indicators: methyl orange, methyl red and phenolphthalein. Total flavonoids (TF) and condensed tannin (CT) from the crude leaves extract were determined which might be the major reasons for the activity of the extract as an indicator for simple acid-base titration. The authors suggest that the natural indicator is cheap, available, simple to extract, user and environmentally friendly and could be an excellent replacement for standard indicators.
基金supported by the National Natural Science Foundation of China (U1701241, U1612441,41773147, and 41273149)the Science Foundation of Guizhou(20113109) 。
文摘Rocky desertification has become a major environmental issue in the karst region of southwestern China.Karst rocky desertification was more severe in regions of limestone soil than in adjacent regions of other soils,despite the relatively higher soil organic matter(SOM)content in limestone soil.The underlying mechanism remains ambiguous.We speculated that the geochemical characteristics of limestone soils in the karst region plays an essential role,especially the high calcium content of limestone soil.To test this hypothesis,we collected limestone soil samples from a limestone soil profile in the southwestern China karst region and extracted humic acid(HA)from these limestone soil samples.We investigated the interaction of Ca^(2+)and three HA samples on a joint experimental platform,which consists of an automatic potentiometric titrator,a UV–visible spectrometer,and a Fluorescence spectrometer.HA solutions were titrated by Ca^(2+)and optical spectra of the HA solutions were monitored during the titration experiments.The results indicated that:(1)the interaction of Ca^(2+)and HA is a combined process of adsorption and complexation.Adsorption dominated the overall distribution behavior of Ca^(2+),which could be fit by Langmuir and Freundlich isotherm models.Complexation was distinguished only when the concentration of Ca2+is low;(2)the changes of UV–visible spectroscopy and excitation–emission matrix fluorescencespectroscopy spectra of HA samples when they were binding with Ca^(2+)implied the apparent molecular size and structure of HA became larger and more complex;(3)the combination of Ca^(2+)and HA plays an important role in the SOM preservation of limestone soils but the stability of the Ca–HA association was relatively weak.The present study draws attention to maintaining the relatively higher Ca^(2+)concentration in limestone soils in ecologic restoration attempts in karst regions.
文摘By using calcium ion selective elatrode (Ca ISE) as indicating electrode, saturated calomel electrode (SCE) as reference electrode and EGTA as titrant, calcium in seawater was determined by potentiometric titration in borate buffer solution. This method can reduce observation errors in the determination of the endpoint, and thus provide better analytical precision(<0.08%) than present complexometric titration.
文摘Introduction: Only vindication of a nasal continuous positive airway pressure (CPAP) retitration procedure will be an actual change in the optimal CPAP pressure after that test. The purpose of this study was to identify any items in patient characteristics, clinical features, baseline PSG and initial CPAP titration as predictors of change in optimal pressure on CPAP retitration. Methods: 46 patients with obstructive sleep apnea (OSA) were divided in two groups: Group I (optimal pressure was changed on CPAP retitration): N = 30, M 22 and F 8, age 31-72, BMI 26-50 Kg/m2, neck size 15 – 20', tonsillectomy in 8, narrow oropharynx in 15, uvuvlopalatopharyngoplasty (UP3) in 2, abnormal chin in 3, deviated nasal septum (DNS) and prior nose surgery in 1 each, initial CPAP pressure 6-19 cm, sleep efficiency 65%-98%, REM latency 0-304 minutes and residual apnea hypopnea index (AHI) 0-23/hour. Group II (optimal pressure unchanged after CPAP retitration): N = 16, M 11 and 5 F, age 32-69, BMI 23-62 Kg/m2, neck size 14.5-20', tonsillectomy in 6, narrow oropharynx in 5, abnormal chin in 4, corrective nasal surgery in 2, DNS in 1, initial CPAP pressure 8-13 cm of H2O, sleep efficiency 69%-95%, REM latency 0-270 minutes and residual AHI 0-19/hour. The statistical analyses were performed using two-tailed Fisher’s t test and unpaired t test. A p value of <0.05 was considered statistically significant. Results: Patient characteristics (age, gender, neck size, and BMI), clinical features (tonsillar status, oropharyngeal narrowing, chin abnormality, DNS/nasal surgery or UP3), baseline PSG or initial CPAP titration (sleep efficiency, REM latency, residual AHI and initial CPAP pressure) did not differ significantly between the 2 groups (p = 0.09-0.99). Conclusion: Patient characteristics, clinical features or variables on baseline PSG and initial CPAP titration do not predict a change in optimal pressure on CPAP retitration. The results suggest that 1) Significant weight change;2) Patient’s subjective feeling of pressure being too high or insufficient;3) Residual or recurrent daytime sleepiness uncorrected by interface readjustments;4)
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Polyphenols are naturally occurring compounds found largely in fruits, vegetables, cereals and beverages. Currently, there is much interest in the potential health benefits of dietary plant polyphenols as antioxidants. The effect of polyphenols on human cancer cells is most often protective and induces a reduction in the number of tumors or rate of growth. During our course of study on anticancer prodrugs, twelve triphenylmethanol and one tris(2-(hydroxymethyl) phenol derivatives were synthesized as a carrier of several drugs with optimized lipophilicity. Besides application of these compounds as a foundation for anticancer drug delivery systems, these compounds were evaluated as indicators for the acid-base volumetric titration of a standard solution of hydrochloric acid with a standard solution of sodium hydroxide. The experiments indicated a moderate-to-sharp color transition of the solutions near the neutralization point for most indicators. These indicators may have potential applications for acid-base titrations in a narrow range.
基金financial support of the Grant Agency IGA MZCR(Grant No NS9831-4/2008)the Czech Ministry of Education(Grant No MSM0021627502)
文摘The mixed dissociation constant of azathioprine—chemically 6-(3-methyl-5-nitroimidazol-4-yl)sulfanyl-7H- purine at various ionic strengths I of range 0.01-0.2, and at temperatures of 25℃ and 37℃, was determined with the use of two different multiwavelength and multivariate treatments of spectral data, SPECFIT32 and SQUAD(84) nonlinear regression analyses and INDICES factor analysis according to a general rule. First, the number of components is determined, and then the spectral responses and concentrations of the components are calculated. Concurrently, the experimental determination of the thermodynamic dissociation constant was in agreement with its computational prediction of the PALLAS programme based on knowledge of the chemical structures of the drug. The factor analysis in the INDICES programme predicts the correct number of two light-absorbing species L- and HL. The thermodynamic dissociation constant of azathioprine was estimated by nonlinear regression of {pKa, I} data, = 8.07(1) at 25℃ and 7.84(1) at 37℃, where the figure in brackets is the standard deviation in last significant digits. The reliability of the dissociation constants of azathioprine was proven with goodness-of-fit tests of the multiwavelength spectrophotometric pH-titration data.
基金Supported by the Natural Science Project of Hubei Provin-cial Department of Education (2005D6002)
文摘Impedance titration was used to determine the surface dissociation characteristics of short-chain carboxyl mercaptan self-assembled monolayers （SAMs）. Based on the change of the cyclic voltammetric peak current and the charge-transfer resistance, which was related to pH value of the solution, the surface pKa of mercaptoacetic acid（MA）, 3-mercaptopropionic acid（MPA） and ω-mercaptohexanic acid（MHA） self-assembled membranes, with ionic strength being 0.1 mol/L, were determined to be 5.20, 4.80, 7.40, respectively. In addition, factors such as time needed for assembling, structure of monolayers and ionic strength, which effected the surface pKa, were studied as well. Such surface pKa shifts were sufficiently explained by interactions between interfacial molecules and hydrophobicity.
基金supported by the National Natural Science Foundation of China (21825703, 21927814)the National Key R&D Program of China (2019YFA0405600, 2019YFA0706900, 2021YFA1200104, 2022YFC3400500)+3 种基金the Strategic Priority Research Program of Chinese Academy of Sciences (XDB0540200, XDB37040201)Plans for Major Provincial Science&Technology Projects (202303a07020004)Basic Research Program Based on Major Scientific Infrastructures,CAS (JZHKYPT-2021-05)the Youth Innovation Promotion Association,CAS (2022455)
文摘Bacterial small laccases(SLAC) are promising industrial biocatalysts due to their ability to oxidize a broad range of substrates with exceptional thermostability and tolerance for alkaline p H. Electron transfer between substrate, copper centers, and O2is one of the key steps in the catalytic turnover of SLAC. However, limited research has been conducted on the electron transfer pathway of SLAC and SLAC-catalyzed reactions, hindering further engineering of SLAC to produce tunable biocatalysts for novel applications. Herein, the combinational use of electron paramagnetic resonance(EPR) and ultraviolet-visible(UV-vis) spectroscopic methods coupled with redox titration were employed to monitor the electron transfer processes and obtain further insights into the electron transfer pathway in SLAC. The reduction potentials for type 1 copper(T1Cu), type 2 copper(T2Cu) and type 3copper(T3Cu) were determined to be 367 ± 2 mV, 378 ± 5 m V and 403 ± 2 mV,respectively. Moreover, the reduction potential of a selected substrate of SLAC, hydroquinone(HQ), was determined to be 288 mV using cyclic voltammetry(CV). In this way, an electron transfer pathway was identified based on the reduction potentials. Specifically,electrons are transferred from HQ to T1Cu, then to T2Cu and T3Cu, and finally to O2.Furthermore, superhyperfine splitting observed via EPR during redox titration indicated a modification in the covalency of T2Cu upon electron uptake, suggesting a conformational alteration in the protein environment surrounding the copper sites, which could potentially influence the reduction potential of the copper sites during catalytic processes. The results presented here not only provide a comprehensive method for analyzing the electron transfer pathway in metalloenzymes through reduction potential measurements, but also offer valuable insights for further engineering and directed evolution studies of SLAC in the aim for biotechnological and industrial applications.
基金supported by the National Natural ScienceFoundation of China (No. 21171110)the Research Fund for the Doctoral Program of Higher Education of China (No. 20091404110001)
文摘Paraquat （PQ）, a nonselective herbicide, is non-fluorescent in aqueous solutions. Thus, its determination through direct fluorescent methods is not feasible. The supramolecular inclusion interaction of PQ with cucurbit[7]uril was studied by a fluorescent probe titration method. Significant quenching of the fluorescence intensity of the cucurbit[7]uril-coptisine fluorescent probe was observed with the addition of PQ. A new fluorescent probe titration method with high selectivity and sensitivity at the ng/mL level was developed to determine PQ in aqueous solutions with good precision and accuracy based on the significant quenching of the supramolecular complex fluorescence intensity. The proposed method was successfully used in the determination of PQ in lake water, tap water, well water, and ditch water in an agricultural area, with recoveries of 96.73% to 105.77%. The fluorescence quenching values （AF） showed a good linear relationship with PQ concentrations from 1.0 × 10^-8 to 1.2× 10^-5 mol/L with a detection limit of 3.35 x 10-9 mol/L. In addition, the interaction models of the supramolecular complexes formed between the host and the vip were established using theoretical calculations. The interaction mechanism between the cucurbit[7]uril and PQ was confirmed by 1H NMR spectroscopy.
基金Supported by the National Nature Science Foundation of China(29873036)
文摘The stability constants and thermodynamic functions for complexes of lanthanum with eight kind of amino acids according to 1∶1 and 1∶2 in proportion have been determined by titration calorimeter at 298.15 K. The enthalpy change makes a predominant contribution to the stability of these complexes. The ring in amino acid associated with lanthanum ion helps to enhance the stability of complexes. Steric effects between rings in complexes leads to that the equilibrium constants of reaction of the complexes (1∶2) is much less than that of the complexes (1∶1).
文摘Objective: to compare the difference between potentiometric titration and indicator titration in the determination of total organic acids in hawthorn. Methods: potentiometric titration and indicator titration were used to determine the content of total organic acids in different batches of hawthorn, and the differences in precision, repeatability, stability and recovery between the two methods were compared. Results: the repeatability and stability of potentiometric titration were higher than that of indicator titration. The recovery rate of potentiometric titration was 97.61%, and that of indicator titration was 96.96%. Potentiometric titration is easier to eliminate the interference of Hawthorn water extract color on titration end point. Conclusion: potentiometric titration is better than indicator method in the determination of total organic acids in hawthorn with color interference.
基金the National High-Tech Development Plan (2006AA05Z417)the Natural Science Foundation of Lia-oning Province (20062145)the Education department of Liaoning Province (05L073)
文摘The precursors of La0.7Sr0.3-xCaxCo0.9Fe0.1O3-δ(LSCCF, x=0.05, 0.10, 0.15, 0.20) as the cathode materials for intermediate temperature solid oxide fuel cell (ITSOFC) were prepared by reverse titration co-precipitation method with metal-nitrates as starting materials and mixed alkali (NaOH and Na2CO3) as a precipitating agent. The formation process of LSCCF from the precursors was monitored by TG-DSC, and the crystal structure and particles morphology of the precursors which were calcined at 600, 800, 1000 ℃ for 3 h were characterized using XRD, SEM technologies. Compared with the solid state reaction of constituent oxides, when the pH value of the precipitating solution was in the range of 9.1～9.5, the LSCCF powders from the precursors caclined at 800 ℃ for 3 h had high purity, homogeneous and single perovskite phase. The electrical conductivity of the LSCCF samples sintered at 1200 ℃ for 3 h, which was measured as a function of temperatures from 100 to 800 ℃ by DC four-probe method in air, decreased with x from 0.05 to 0.20. The value of electrical conductivity was almost equal because of Ca2+, Sr2+ co-dopant resulting in the 'mix effect' while x=0.10 or 0.15. The electrical conductivity of all doped samples was higher than 100 S·cm-1 at intermediate temperatures from 500 to 800 ℃, and there was good compatibility between the LSCCF cathode and Ce0.8Sm0.2O2 electrolyte.
