A simple potentiometric method for the determination of reducing substances in urine with a copper-selective electrode

A potentiometric method for the determination of reducing substances in urine is described. Samples are treated with Stanley—Benedict reagent and the unused copper(II) is determined with a copper(II)-selective electrode by the standard addition technique. Glucose in the range 25–200 μg in 0.1ml samples can be determined with an average error of about 2%. The recovery of added glucose for six samples was 96–107% (average 100.5%). Comparison with the conventional titrimetric method shows good agreement. The effect of other non-glucose reducing substances present in urine is reported.     

Continuous-flow potentiometric determination of creatinine in urine with a picrate ion-selective electrode

A completely automated potentiometric method for the determination of creatinine in urine is described. Creatinine reacts with picrate in alkaline media (Jaffé reaction) in a flow system, and the decrease in picrate activity is continuously monitored with a picrateselective flow-through electrode. Creatinine in urine, in the range 0.5–3 g/liter, was determined in a sample volume of 0.15 ml, with a relative standard deviation of about 1%. Forty samples per hour can be analyzed without previous dilution or pretreatment. Recovery of creatinine added to urine samples ranged from 90 to 111% with an average of 96.7%. The method compares favorably with a photometric method. The proposed automated method is suitable for routine clinical measurements and screening tests.     

Flow-injection analysis with the iron-induced perbromate-iodide reaction: spectrophotometric determination of iron

Total iron is determined by a flow-injection spectrophotometric technique. The production of I(-)(3) from the iron(II)- or iron(III)-induced perbromate-iodide reaction is monitored at 353 nm. Calibration graphs are linear from 10 to 100 ng/ml with correlations up to 0.9998 and can be extended up to 10 microg/ml by appropriate adjustment of conditions. The average sampling rate is 30 samples/hr. Detection limits and relative standard deviations compare well with those of other FIA methods.     

Kinetic potentiometric determination of citric acid with a perbromate-selective electrode

Citric acid is determined in the 96–960-μg range with relative errors of about 1% by means of its iron(II)-induced reaction with perbromate. Each analysis takes about 8 min. Tartaric and lactic acids interfere.     

EDTA titration of calcium and magnesium with a calcium-selective electrode

Direct semi-automatic and automatic derivative potentiometric EDTA procedures for the determination of calcium and/or magnesium with a calcium-selective electrode are described. Calcium is titrated in the presence of magnesium at pH 12.0 and the total calcium and magnesium is determined at pH 9.7. Calcium in the range 1-8 mg and magnesium in the range 0.7-5 mg are determined semi-automatically with average errors of about 0.2 and 0.3% respectively and automatically with average errors of 0.4 and 0.7%. Titration times vary from a few seconds to a few minutes.     

Enzymatic fluorimetric determination of the individual bile acids in blood serum

An enzymatic fluorimetric method is described for the determination of total bile acids (cholic acid and deoxycholic acid), primary bile acids (cholic and chen acids and individual bile acids in serum without prior separation of the acids. Total and primary bile acids are determined by equilibrium procedures by conver of the 3α- and 7α-hydroxy bile acids to 3-oxo and 7-oxo bile acids by α-NAD⁺, in the presence of 3α- and 7α-hydroxysteroid dehydrogenase (HSD), respectively, and measurement of the generated NADH fluorimetrically. Chenodeoxycholic acid is determined with 7α-HSD in the presence of cholic and deoxycholic acids by a differential kinetic procedure, and cholic and deoxycholic acids are calculated by difference. Interferents are removed by treatment of serum with Sachrom rein. Only 1.00 ml of serum is required. Low cost, simplicity and reliability are the main features of the method. The recovery of bile acids added to serum averaged 103% (range 83–122%). The method is suitable for routine use in small clinical laboratories.     

Kinetic study and analytical application of the iodate-hypophosphite reaction in strongly acidic solutions

The iodate—hypophosphite reaction in strongly acidic solutions was studied spectrophotometrically. Reaction rate constants and the activation energy of the reaction are reported. A method for determining hypophosphite on the basis of this reaction is described. Hypophosphite in the range 0.06–4 mg (10^-3–6·10^-2 M) can be determined with a relative error and relative standard deviation of 2—3%.     

Titrimetric determination of thiourea and silver with a picrate ion selective electrode

Summary A method has been developed for the semiautomatic potentiometric titration of thiourea with silver nitrate and of silver with thiourea, in the presence of picrate ions, using a picrate ion selective electrode. Thiourea in the range 15–1500g and silver in the range 200–1800g were determined with relative errors and relative standard deviation of about 1%.

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Zusammenfassung Eine halbautomatische potentiometrische Titrationsmethode für Thioharnstoff mit Silbernitrat bzw. umgekehrt in Gegenwart von Pikrationen mit Hilfe einer selektiven Pikratelektrode wurde entwickelt. 15–1500g Thioharnstoff bzw. 200–1800g Silber wurden mit einem relativen Fehler und einer relativen Standardabweichung von etwa ±1% bestimmt.

     

Construction and analytical applications of an improved liquid-membrane electrode for salicylate

The construction and analytical applications of an improved liquid-membrane electrode for salicylate are described. Tests of various combinations of symmetrical tetraalkylammonium salicylates and solvents showed that the best liquid ion-exchanger was tetraoctylammonium salicylate in p-nitrocumene. Electrode response is Nernstian down to 2 × 10^?5 M. Major interferences are perchlorate and periodate; the working pH range is 6–9. The electrode is useful for direct potentiometric determinations of salicylate in pharmaceutical preparations.