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Comparision of methods for sulphide determination
Zlámalová, Magda ; Nesměrák, Karel (advisor) ; Červený, Václav (referee)
The aim of this work is determination of sulphides in a solution by suitable methods and it's subsequent comparison from a point of view to the precision, financial and time demands. Iodometric titration, argentometric titration, and potassium ferricyanide titration were chosen for the determination of sulphides in the solution. Anhydrous sodium sulphide and sodium sulphide hydrate were used as model samples. From the point of view to financial and time demands the most advantageous method was potassium ferricyanide titration and the least advantageous method was iodometric titration. The precision of used methods was dependent on type of used sample. Iodometry was the least precise determination of sulphides in the sample of anhydrous sodium sulphide; the precision of argentometry and potassium ferricyanide titration was comparable. Potassium ferricyanide titration was the most precise determination of sulphides in the sample of sodium sulfide hydrate; the least precise determination was argentometry.
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Study of Factors Influencing the Teduction of Rhenistane
Burešová, Helena ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
The aim of the bachelor thesis was to study the influence of conditions on the reduction of ammonium perrhenate by selected reduction agents. The amount of reduced perrhenate was followed by differential pulse voltammetry (as the decrease of the height of DPV peak). The percentage of reduced perrhenate was expressed as a function of molar ratio of the reduction agent to perrhenate. The following four agents were employed: sodium borohydride, hydroxylamine hydrochloride, hydrazine hydrochloride, and ascorbic acid. An amount of 97.8% of rhenium reduced was achieved by 0.9-fold of molar excess of sodium borohydride in 2 mol dm-3 perchlorid acid. The threefold molar excess of hydroxylamine hydrochloride reduced rhenium by 85% (in medium with pH = 8.5). The threefold molar excess of hydazine hydrochloride reduced rhenium by 68% (in medium with pH = 5.0). Ascorbic acid was the last studied reduction agent; its threefold molar excess reduced rhenium by 98.7%.
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Determination of Heparin by Sequential Injectin Analysis with Spectrophotometric Detection
Lišková, Růžena ; Hraníček, Jakub (advisor) ; Nesměrák, Karel (referee)
In this work the determination of heparin using Sequential Injection Analysis (SIA) technique with spectrophotometric detection was studied. The principle of this method was measuring the decrease of absorbance of phenothiazine dyes in its maximum wavelength caused by its interaction with heparin. The decrease is proportional to concentration of heparin in sample. The aim of this work was to find optimum conditions for determination of heparin by the SIA with spectrophotometric detection and to try to apply this measurement to real sample under these conditions. Three phenothiazine dyes were used: Methylene Blue, Azure A and Azure B and for each of them an optimum concentration was found. Their values were for methylene blue 4.0 ∙ 10-5 mol/dm3 and 5.0 ∙ 10-5 mol/dm3 for Azure A and Azure B. 150 µl was chosen as an optimum amount of heparin and reagent aspirated. Optimum reaction time was 0 s and flow rate during measurement 1.5 ml/min. Working concentration range was found between 0.23 and 15 mg/dm3 for methylene blue, 1.2 and 13 mg/dm3 for Azure A and 0.67 and 12 mg/dm3 for Azure B. Limit of detection varied between 0.09 - 0.35 mg/dm3 and limit of quantification between 0.30 and 1.2 mg/dm3 for different dyes. Relative standard deviation was determined as a measure of repeatability. Its values were...
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Kinetic determination of nitrites with spectrophotometric detection
Vašíčková, Pavla ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
Title: Kinetic determination of nitrites with spectrophotometric detection Annotation: The proposal and optimization of the kinetic determination of nitrites in water samples is the aim of this bachelor thesis. The method is based on the ability of nitrites to catalyze the oxidation of toluidine blue by bromate in acidic media. The course of the reaction is monitored by spectrophotometrically, using a decrease of the absorbance band at 653 nm in the constant period of time from the beginning of the reaction. The dual-chanel manifolds FIA apparatus was proposed and optimized. The calibration dependency in the range of 0,05-1,00 mg ml-1 was measured. The instrumental limit of detection of 0,038 mg ml-1 and limit of quantification of 0,125 mg ml-1 were calculated. The method was applied on real sample of river water. Key words: nitrites, flow-injection analysis, kinetic catalytic methods
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