Oxygen in Organic Compounds

Aluise, V. A.; Hall, Robert T.; Staats, J. C.; Becker, W.

doi:10.1021/ac60005a024

Cited by 54 publications

(11 citation statements)

References 6 publications

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“…The method that has won great popularity for the direct determination of oxygen is the one first developed by Sehütze ( 202) and later modified by Zimmermann (271) and Unterzaucher (235). It is the latter's modification that has been developed in this country by Aluise et al (5). The essential features of this determination consist in decomposition of the sample in a stream of nitrogen made oxygen-free by passage over heated copper and the ultimate conversion of all the oxygen of the organic compound to carbon monoxide by passing the gases over heated charcoal which must be maintained at 1100°C.…”

Section: Oxygenmentioning

confidence: 99%

Organic Microchemistry

Willits¹

1949

Anal. Chem.

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MICROCHEMICALanalyses of organic compounds still follow largely the pattern set by Fritz Pregl. Considerable strides have been made during the past 6 years, as evidenced by the increase in the number of microchemical laboratories and the wider application of microanalytical chemical techniques. During the late twenties and early thirties, microanalytical methods were but little used in the United States except in the Atlantic Coast states. Ten years later these methods had been introduced into the midwestern states, and today micromethods are in use in analytical laboratories throughout the country.The keen interest shown in the development of microchemical analysis is exhibited by the establishment of a committee on the performance of microchemical balances (A. H. Corwin of Johns Hopkins University, chairman); a revival of the committee on standardization of microchemical apparatus (A. Steyermark, chairman); and the re-establishment of a referee on the standardization of microchemical methods by the Association of Official Agricultural Chemists. The British Standards Institute has formed a subcommittee to standardize microchemical apparatus, and the work of this subcommittee is well advanced. Microchemistry has gone a long way since Pregl devised this scheme of analysis, for it is no longer limited to the analysis of material available in only small amounts. Instead, it has an accepted place, along with micromethods, for the analysis of materials available in large amounts. The micromethod is superior, in that it is faster, more economical of reagents, and in many instances more precise and accurate.

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Section: Oxygenmentioning

confidence: 99%

Organic Microchemistry

Willits¹

1949

Anal. Chem.

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“…This error attains greater relative significance when applied to compounds containing low amounts of oxygen. Aluise et al (2) have indeed shown that more precise and ac-if components of the residue undergo change in weigh t during ashing. The Unterzaucher method, although generally satisfactory, gives incorrect results on organic products containing inorganic carbonates or oxides.…”

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confidence: 95%

Direct Microdetermination of Oxygen in Organic Compounds. Comparison Between Unterzaucher and ter Meulen Methods

Maylott¹,

Lewis²

1950

Anal. Chem.

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into a 125-ml. iodine flask containing 5 ml. of Clorox solution. Transfer the contents of the tube to the flask with 25 to 30 ml. of distilled water and add 5 ml. of the phosphate buffer solution. Heat the solution just to boiling on a not plate adjusted to bring it to an incipient boil in 8 to 10 minutes. Remove the flask from the hot plate, immediately add 3 ml. of the sodium formate solution, and swirl gently. Allow to stand 3 to 4 minutes, then cool to room temperature in running cold water. Add 5 ml. of 9 N sulfuric acid, 0.5 gram of potassium iodide, and 2 drops of the ammonium molybdate and titrate rapidly with 0.015 N sodium thiosulfate. Add 2 drops of amylose (or other starch indicator) just before reaching the colorless end point.A blank determination should be made with all reagents; however, the blank need not be digested. The blank value varied from 0.04 to 0.2 ml. of 0.015 N thiosulfate, depending on the bottle of Clorox used.The calculations are made as follows:net ml. of 0.015 N thiosulfate X 79.916 X 0.015 X 100 /0 sample weight (mg.)In a large group of samples the working time, aside from weighing, is about 25 minutes per determination.The data in Table I show satisfactory precision and accuracy for a group of organic bromine compounds containing chlorine, iodine, and nitrogen. Unreported data indicate that iodine is quantitatively determined by the method. Therefore, it is an interfering element. The iodine may, however, be determined in a separate portion of the sample by the Carius-iodometric method for iodine (7) and the bromine content of the sample may then be calculated from the results of the analyses by the two methods.The method has not been applied to biological materials. The lyophilization technique described previously (7) should be applicable to many such samples.

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“…It is also of interest to note that Aluise and his coworkers (11) in 1947 were troubled with a variable blank in the oxygen determination which they could not explain. They attributed it to impurities in the nitrogen carrier which somehow got by the hot copper in their purifying train.…”

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confidence: 99%