A Drastic Saponification Method for Difficultly Saponifiable Esters

Shaefer, W. E.; Piccard, Jean

doi:10.1021/ac50125a004

Cited by 9 publications

(1 citation statement)

References 8 publications

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“…Methyl abietate is very difficult to saponify (1,10). The present method failed for this compound even after heating at 130 °O.…”

Section: Methodsmentioning

confidence: 70%

Microdetermination of Saponification Equivalent

VanEtten¹

1951

Anal. Chem.

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available, samples were taken for analysis which has been previously analyzed for sulfur by the gravimetric barium sulfate method of the American Society for Testing Materials (4)• The results are shown in Table III. The average deviation was found to be 0.03%. DISCUSSIONVery erratic sulfur values were found using the original Lindberg high frequency unit. These poor results were traced to the aluminum alloy dome cap and the metal spring of the dispersion plug, and were probably due to the attack of the metallic parts by the sulfur dioxide liberated during the combustion. On substitution of a borosilicate glass dome cap, accurate sulfur values were once more obtained.A plug of glass wool was found to be very efficient in removing the metallic oxides from the gas stream.If the amount of Alundum placed on top of the charge is too light, large amounts of metallic oxides will be volatilized, if it is too heavy, the molten oxides will spatter. The correct amount was found to be that which just covered the charge so that the underlying metals did not show through.The sulfur values for the coal and coke samples are in good agreement when the errors (S) in the determination of sulfur as barium sulfate are considered.

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“…Methyl abietate is very difficult to saponify (1,10). The present method failed for this compound even after heating at 130 °O.…”

Section: Methodsmentioning

confidence: 70%

Microdetermination of Saponification Equivalent

VanEtten¹

1951

Anal. Chem.

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Analysenmethoden für die Verarbeitungshilfsmittel für die Plaste

Thinius

1952

Analytische Chemie Der Plaste (Kunststoff-Analyse)

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Saponification value determination of difficultly saponifiable drying oil products

Shaw

Formo

1954

J Americ Oil Chem Soc

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ConclusionsThe use of n‐butyl alcohol as a solvent for saponification of a representative series of drying oils has been studied. It appears from this work that n‐butyl alcoholic potassium hydroxide reagent, containing 5% of water added to the reaction mixture, gives very acceptable results based upon calculated saponification values.With the exception of maleic‐modified oils of certain types, the solvent system of ethyl alcohol‐pyridine exhibits excellent results based upon calculated values. However it has the disadvantages that it is a two‐solvent system, and the pyridine must be of reagent grade to avoid end‐point difficulties.The end‐point in the butyl alcohol system is not as sharp as the normal saponification end‐point in ethyl alcohol. This may be caused by the two‐phase nature of the titration mixture. Addition of ethyl alcohol to the n‐butyl alcoholic saponification reaction mixture gives improvement, although the end‐point is not as sharp as in the regular ethyl alcohol system. Work is continuing on methods for improvement of the end‐point.

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A Drastic Saponification Method for Difficultly Saponifiable Esters

Cited by 9 publications

References 8 publications

Microdetermination of Saponification Equivalent

Microdetermination of Saponification Equivalent

Analysenmethoden für die Verarbeitungshilfsmittel für die Plaste

Saponification value determination of difficultly saponifiable drying oil products

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