PERIODATE–PERMANGANATE OXIDATIONS: III. DETERMINATION OF ISOPROPYLIDENE GROUPS

1955 ◽  
Vol 33 (11) ◽  
pp. 1714-1719 ◽  
Author(s):  
E. Von Rudloff
Keyword(s):  
Aqueous Solutions ◽  
Quantitative Yield ◽  
Simultaneous Estimation ◽  
Colorimetric Determination ◽  
Double Bonds ◽  
Methylene Groups ◽  
Insoluble Compounds

The reaction of the periodate–permanganate reagent with olefinic double bonds was applied to the determination of isopropylidene groups. The oxidation of compounds containing such groups gave a quantitative yield of acetone which could be readily determined by known iodometric and colorimetric procedures. Use of aqueous solutions of pyridine or dioxane as solvent permitted analysis of water-insoluble compounds. The colorimetric determination of acetone was then preferred. This method also allowed a simultaneous estimation of terminal methylene groups. The content of isopropylidene groups of commercial samples of three terpenes of the geraniol type was determined.

scholarly journals Spectrofluorimetric Determination of Warfarin Sodium by Using N1-Methylnicotinamide Chloride as a Fluorigenic Agent

2005 ◽  
Vol 88 (2) ◽  
pp. 455-461 ◽  
Author(s):  
Mohamed A El Dawy ◽  
Mokhtar M Mabrouk ◽  
Riad A El Barbary
Keyword(s):  
Aqueous Solutions ◽  
Human Plasma ◽  
Plasma Samples ◽  
Spiked Human Plasma ◽  
Human Plasma Samples ◽  
Warfarin Sodium ◽  
Spectrofluorimetric Method ◽  
Spectrofluorimetric Determination ◽  
Methylene Groups

Abstract A spectrofluorimetric method is described for the determination of drugs containing active methylene groups adjacent to carbonyl groups. The method was applied successfully to the determination of warfarin sodium in laboratory-prepared mixtures, in commercial tablets, and in spiked human plasma samples. Finally, the method was applied to the determination of the steady-state concentration of warfarin sodium in the blood of a hospitalized patient. The method involves the reaction of warfarin sodium with 0.2 ml (0.4 × 10−3M) N1-methylnicotinamide chloride reagent in the presence of 3 mL 1.0N NaOH and cooling in ice for 8 min, followed by adjustment of the pH to 2.0, using formic acid and heating for 4 min, whereby a highly fluorescent reaction product is produced. The optimal wavelengths of excitation and emission were determined by using a synchronous wavelength search and found to be 284 and 354 nm, respectively. The standard curves were linear over a concentration range of 50–1500 ng/mL in both aqueous solutions and spiked human plasma samples. The mean recoveries (± standard deviation) were 101.157 (±1.33) and 95.73 (±1.88%) for aqueous solutions and spiked human plasma samples, respectively. The method showed good specificity and precision. The proposed method is simple and economical because of its minimal instrumentation and chemicals requirements. Nevertheless, it is highly sensitive, specific, and reproducible. Accordingly, it is suitable for quality-control applications, drug monitoring, and bioavailability and bioequivalency studies.

PERIODATE–PERMANGANATE OXIDATIONS: II. DETERMINATION OF TERMINAL METHYLENE GROUPS

1955 ◽  
Vol 33 (11) ◽  
pp. 1710-1713 ◽  
Author(s):  
R. U. Lemieux ◽  
E. Von Rudloff
Keyword(s):  
Quantitative Yield ◽  
Permanganate Oxidation ◽  
Initial Stage ◽  
Methylene Groups ◽  
Methylene Group

The periodate–permanganate oxidation of a terminal methylene group can be made to produce formaldehyde in high although not quantitative yield. Since the yields compare favorably with those obtained by ozonolysis, the reagent can serve as the basis for a convenient micromethod for the estimation of terminal methylene groups. The less than theoretical yields of formaldehyde are believed mainly due to the conversion of the olefin in part to α-hydroxyaldehyde in the initial stage of the reaction.

scholarly journals Analytical Microsystem for the Monitoring and Analysis of Cobalt in Aqueous Solutions Using LTCC Technology

2017 ◽  
Vol 58 (4) ◽  
Author(s):  
Olga Natalia Bustos López ◽  
Francisco Valdés Perezgasga ◽  
Héctor Aurelio Moreno Casillas ◽  
Julián Alonso Chamarro ◽  
Hesner Coto Fuentes
Keyword(s):  
Aqueous Solutions ◽  
Continuous Flow ◽  
Flow System ◽  
Detection System ◽  
Light Emitting Diode ◽  
Colorimetric Determination ◽  
Light Emitting ◽  
Design And Implementation ◽  
Optical Detection System

<p>This work is focused on the design and implementation of a microsystem for continuous colorimetric determination of cobalt in aqueous solutions in real time.  The main goal is the colorimetric determination of cobalt by adapting colorimetric methodologies used in discontinuous analysis systems to a continuous flow system and its subsequent miniaturization using the LTCC (Low Temperature Co-fired Ceramics) technology. The measure absorbance was recorded using an optical detection system based on a LED (Light Emitting Diode) with a wavelength of 540 nm. </p>

Collaborative Study of the Colorimetric Determination of Zirconium in Antiperspirant Aerosols

1977 ◽  
Vol 60 (3) ◽  
pp. 663-668
Author(s):  
Paul Beavin
Keyword(s):  
Statistical Evaluation ◽  
Collaborative Study ◽  
Colorimetric Determination ◽  
Fusion Procedure ◽  
Coefficients Of Variation ◽  
Zirconium Compounds ◽  
Insoluble Form ◽  
Standard Deviations ◽  
Insoluble Compounds

Abstract A previously published method for determining zirconium in antiperspirant aerosols was collaboratively studied by 7 laboratories. The method consists of 2 procedures: a rapid dilution procedure for soluble zirconium compounds or a lengthier fusion procedure for total zirconium (soluble and insoluble compounds), followed by colorimetric determination. The collaborators were asked to perform the following: Spiking materials representing 4 levels of soluble zirconium were added to weighed portions of a zirconium-free cream base concentrate and the portions were assayed by the dilution procedure. Spiking materials representing 4 levels of zirconium in either the soluble or the insoluble form (or as a mixture) were also added to portions of the same concentrate and these portions were assayed by the fusion procedure. They were also asked to concentrate and assay, by both procedures, 2 cans each of 2 commercial aerosol antiperspirants containing zirconyl hydroxychloride. The average per cent recoveries and standard deviations for spiked samples were 99.8–100.2 and 1.69–2.71, respectively, for soluble compounds determined by the dilution procedure, and 93.8–97.4 and 3.09–4.78, respectively, for soluble and/or insoluble compounds determined by the fusion procedure. The average per cent zirconium found by the dilution procedure in the 2 commercial aerosol products was 0.751 and 0.792, respectively, with coefficients of variation of 2.94 and 2.53%, respectively. Insufficient collaborative results were received for the fusion procedure for statistical evaluation. The dilution procedure has been adopted as official first action.

Determination of Zirconium, Hafnium, Niobium, Tantalum, Molybdenum and Tungsten in Aqueous Solutions by Radioisotopic Excited X-Ray Fluorescence

1971 ◽  
Vol 15 ◽  
pp. 209-227
Author(s):  
Frank L. Chan ◽  
W. Barclay Jones
Keyword(s):  
Aqueous Solutions ◽  
List Type ◽  
Concentrated Solutions ◽  
Chemical Methods ◽  
X Ray ◽  
Liquid Cell ◽  
Iodine 125 ◽  
Insoluble Compounds ◽  
Channel Analyzer

Previous investigations on the quantitative determination of sulfur, chlorine, potassium, calcium, scandium and titanium in aqueous solutions by a radioisotopic excited fluorescent spectrometer has been extended to include other elements which are very difficult to separate and determine quantitatively by chemical methods. Six elements taken for the investigation and some of the results to be presented in this paper are: (1)zirconium,(2)hafnium,(3)niobium,(4)tantalum,(5)molybdenum and(6)tungsten. As in previous investigations, aqueous solutions have been used because of the ease in obtaining exact concentrations and homogeneous mixtures of the elements under investigation.In the earlier investigations which have been reported in this conference, lighter elements (atomic numbers ranging from 16 to 22) were used for the investigation. In the present studies, however, comparatively heavier elements have been used. Therefore a radioisotope such as iron 55 used earlier is not suitable because it cannot excite the K x-ray of these elements. To excite the K and L of these elements, we use the radioisotope iodine 125. The advantage of using this radioisotope is that it is inexpensive and commercially available although its half-life is comparatively short.The spectrometer used with further improvements has been described and presented earlier. We used a multi-channel analyzer of 1000 in the present investigation, A liquid cell was specially designed for thisr study. Chemicals used for preparation of solutions were of reagent grades. Some of them had to be specially prepared. For example, hafnium, often contaminated with zirconium, was specially prepared and checked spectroscopically. Some difficulties have been encountered in preparing concentrated solutions such as niobium and tantalum due to the inherit characteristics of these elements to form insoluble compounds. Procedures will be described for the preparation of these solutions. Instruments used and results will be presented in this paper.

A Method for the Colorimetric Determination of β-Glucuronidase in Urine, Serum, Tissue; Assay of Enzymatic Activity in Health and Disease

1959 ◽  
Vol 36 (2) ◽  
pp. 193-201 ◽  
Author(s):  
Julius A. Goldbarg ◽  
Esteban P. Pineda ◽  
Benjamin M. Banks ◽  
Alexander M. Rutenburg
Keyword(s):  
Enzymatic Activity ◽  
Colorimetric Determination ◽  
Health And Disease ◽  
Urine Serum
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