THE POLAROGRAPHIC DETERMINATION OF TITANIUM IN STEELS AND NICKEL-BASE ALLOYS

1952 ◽  
Vol 30 (9) ◽  
pp. 661-667 ◽  
Author(s):  
R. P. Graham ◽  
A. Hitchen ◽  
J. A. Maxwell

Titanium in steels and nickel-base alloys can conveniently be determined polarographically after electrolysis of a solution of the alloy in a mercury-cathode cell. A well-formed wave, the height of which is directly proportional to the concentration of titanium in the solution, is recorded using a supporting electrolyte that is 1.0 M in tartaric acid, 0.5 M in sulphuric acid, and 1.2 M in ammonium sulphate.The method is one of good precision and yields values in excellent agreement with those given by umpire methods for samples of basic open-hearth steel, 18-11 chromium-nickel steel, Monel, Inconel "W", and Nimonic 75 and 80.

1988 ◽  
Vol 71 (4) ◽  
pp. 857-859
Author(s):  
Walter Holak ◽  
John J Specchio

Abstract When lead and cadmium were determined in samples of canned food by the AOAC anodic stripping voltammetric method, an interference was observed which was believed to be tin(IV). This interference could cause false positive results for lead and cadmium. The electroactivity of tin(IV) was suppressed by increasing the concentration of tartaric acid in the supporting electrolyte from 0.005M to 0.1M after mixing with an equal volume of sample solution.


1950 ◽  
Vol 28f (5) ◽  
pp. 128-133 ◽  
Author(s):  
B. R. Potts

A simple, rapid polarographic procedure for the determination of titanium in paint pigments has been developed, using a sulphuric acid – tartaric acid medium. The accuracy and precision of the method are satisfactory for routine testing operations. The interference of other common pigment ingredients is discussed, and a procedure suggested for the removal of copper and antimony prior to analysis.


2019 ◽  
Vol 15 (5) ◽  
pp. 535-541 ◽  
Author(s):  
Fariba Pourkarim ◽  
Ali Shayanfar ◽  
Maryam Khoubnasabjafari ◽  
Fariborz Akbarzadeh ◽  
Sanaz Sajedi-Amin ◽  
...  

Background:Developing a simple analysis method for quantification of drug concentration is one of the essential issues in pharmacokinetic and therapeutic drug monitoring studies.Objective:A fast and reliable dispersive liquid-liquid microextraction procedure was employed for preconcentration of verapamil in exhaled breath condensate (EBC) samples and this was followed by the determination with high-performance liquid chromatography-ultraviolet detection.Methods:A reverse-phase high-performance liquid chromatography (RP-HPLC) combined with a dispersive liquid-liquid microextraction method (DLLME) was applied for quantification of verapamil in the EBC samples. The developed method was validated according to FDA guidelines.Results:Under the optimum conditions, the method provided a linear range between 0.07 and 0.8 µg.mL-1 with a coefficient of determination of 0.998. The intra- and inter-day relative standard deviation and relative error values of the method were below 15%, which indicated good precision and accuracy. The proposed method was successfully applied for the analysis of verapamil in two real samples with concentrations of 0.07 and 0.09 µg.mL-1.Conclusion:The established HPLC-UV-DLLME method could be applied for the analysis of verapamil in human EBC samples.


2020 ◽  
Vol 16 ◽  
Author(s):  
Sheng-Yun Li ◽  
Fang Tian

: A spectrophotometry was investigated for the determination of epsilon aminocaproic acid (EACA) with p-nitrophenol (PNP). The method was based on a charge transfer (CT) complexation of this drug as n-electron donor with π-acceptor PNP. Experiment indicated that the CT complexation was carried out at room temperature for 10 minutes in dimethyl sulfoxide solvent. The spectrum obtained for EACA/PNP system showed the maximum absorption band at wavelength of 425 nm. The stoichiometry of the CT complex was found to be 1:1 ratio by Job’s method between the donor and the acceptor. Different variables affecting the complexation were carefully studied and optimized. At the optimum reaction conditions, Beer’s law was obeyed in a concentration limit of 1~6 µg mL-1. The relative standard deviation was less than 2.9%. The apparent molar absoptivity was determined to be 1.86×104 L mol-1cm-1 at 425 nm. The CT complexation was also confirmed by both FTIR and 1H NMR measurements. The thermodynamic properties and reaction mechanism of the CT complexation have been discussed. The developed method could be applied successfully for the determination of the studied compound in its pharmaceutical dosage forms with a good precision and accuracy compared to official method as revealed by t- and F-tests.


2020 ◽  
Vol 16 ◽  
Author(s):  
Biljana Nigović ◽  
Iva Šimunić ◽  
Ana Mornar

Background: Ondansetron and paracetamol are often co-administrated to prevent and treat nausea and vomiting caused by anaesthesia and to control of postoperative pain. In addition, ondansetron is used as the first-line antiemetic in paracetamol overdose. Therefore, selective and sensitive method for their simultaneous analysis is of a great importance. The electroanalytical methods are highly sensitive and offer many possibilities for new sensor platform design. However, at present, no electroanalytical method for simultaneous determination of these drugs has been proposed. Objective: The aim of this study was to develop a novel nanosensor for selective monitoring of ondansetron and paracetamol in pharmaceutical and biological samples without expensive and time-consuming pretreatments. Methods: The graphitized multi-walled carbon nanotubes embedded in a cation exchange polymer matrix was selected, among various surface functionalizations evaluated, to design novel sensor. Based on its excellent sensing performance, the first electroanalytical method was developed for rapid concurrent determination of investigated drugs. Results: The scanning electron microscopy study showed interlinked nanoporous network structure and highly enlarged active surface. The developed sensor facilitated electron transfer in the oxidation of both drugs and tremendously enhanced the adsorption capacity for ondasetron, thus exhibiting significant increase of drug responses and sensitivity. To obtain much sensitive response of investigated drugs the effect of pH values of supporting electrolyte, dispersed nanomaterial amount, the cation exchange polymer concentration, drop-casting volume of nanocomposite suspension, accumulation potential and deposition time on the peak current was evaluated. The developed electroanalytical method was validated and practical utility of the proposed nanosensor was tested. Conclusion: The developed sensor is promising sensing platform with a fast response time for analysis of ondansetron and paracetamol at very different concentration levels found in their fixed-dose combination and human serum sample after recommended daily doses showing its potential usage in pharmaceutical quality control and clinical research.


1991 ◽  
Vol 56 (1) ◽  
pp. 112-129 ◽  
Author(s):  
Takashi Kakiuchi ◽  
Mitsugi Senda

We have estimated the degree of polarizability of a polarized oil-water interface used as a working interface and that of the nonpolarizability of a nonpolarized interface used as a reference oil-water interface from the numerical calculation of dc and ac current vs potential behavior at both interfaces. Theoretical equations of dc and ac currents for simultaneous cation and anion transfer of supporting electrolytes have been derived for the planar stationary interface for reversible and quasi-reversible cases. In the derivation, the migration effect and the coupling of the cation and anion transfer have been incorporated. The transfer of ions constituting a supporting electrolyte contributes to the total admittance of the interface even in the region where the interface may be considered as polarized in dc sense, as pointed out first by Samec et al. (J. Electroanal. Chem. 126, 121 (1981)). Moreover, the reference oil-water interface is not ideally reversible, so that the contribution from this interface to the measured admittance cannot be negligible, unless the area of the reference oil-water interface is much larger than that of the working oil-water interface. The effect of non-ideality of the reference oil-water interface on the determination of double layer capacitances and kinetic parameters of charge transfer at the working oil-water interface has been estimated.


1987 ◽  
Vol 33 (8) ◽  
pp. 1427-1430 ◽  
Author(s):  
R Sakuma ◽  
T Nishina ◽  
M Kitamura

Abstract We evaluated six deproteinizing methods for determination of uric acid in serum by "high-performance" liquid chromatography with ultraviolet detection: those involving zinc hydroxide, sodium tungstate, trichloroacetic acid, perchloric acid, acetonitrile, and centrifugal ultrafiltration (with Amicon MPS-1 devices). We used a Toyosoda ODS-120A reversed-phase column. The mobile phase was sodium phosphate buffer (40 mmol/L, pH 2.2) containing 20 mL of methanol per liter. Absorbance of the eluate was monitored at 284 nm. The precipitation method with perchloric acid gave high recoveries of uric acid and good precision, and results agreed with those by the uricase-catalase method of Kageyama (Clin Chim Acta 1971;31:421-6).


Processes ◽  
2021 ◽  
Vol 9 (6) ◽  
pp. 1072
Author(s):  
Mohammad Reza Zaker ◽  
Clémence Fauteux-Lefebvre ◽  
Jules Thibault

Sulphuric acid (H2SO4) is one of the most produced chemicals in the world. The critical step of the sulphuric acid production is the oxidation of sulphur dioxide (SO2) to sulphur trioxide (SO3) which takes place in a multi catalytic bed reactor. In this study, a representative kinetic rate equation was rigorously selected to develop a mathematical model to perform the multi-objective optimization (MOO) of the reactor. The objectives of the MOO were the SO2 conversion, SO3 productivity, and catalyst weight, whereas the decisions variables were the inlet temperature and the length of each catalytic bed. MOO studies were performed for various design scenarios involving a variable number of catalytic beds and different reactor configurations. The MOO process was mainly comprised of two steps: (1) the determination of Pareto domain via the determination a large number of non-dominated solutions, and (2) the ranking of the Pareto-optimal solutions based on preferences of a decision maker. Results show that a reactor comprised of four catalytic beds with an intermediate absorption column provides higher SO2 conversion, marginally superior to four catalytic beds without an intermediate SO3 absorption column. Both scenarios are close to the ideal optimum, where the reactor temperature would be adjusted to always be at the maximum reaction rate. Results clearly highlight the compromise existing between conversion, productivity and catalyst weight.


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