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SCOPE Applicable to soda soap products, except those containing borax. For potash soaps see AOCS Official
Method Da 5-44. Replaces Da 4a-42.
APPARATUS
1. Erlenmeyer flask—250 mL.
2. Gooch crucible or filter paper—the filter paper must impart no acidity or alkalinity to neutral alcohol when
poured through it. A Gooch crucible may be prepared with any suitable glass-fiber filter medium. The filter paper
is washed with distilled water, alcohol, and petroleum ether, and then dried at 105 ± 2 °C before using.
3. Watch glasses.
4. Steam bath or water bath.
REAGENTS
1. Ethyl alcohol—95%. SDA Formulas 30 and 3A are permitted (see AOCS Laboratory Safety). Add 3–5 drops phe-
nolphthalein indicator solution. Boil and neutralize with dilute sodium hydroxide (NaOH), 0.1–0.2 M solution,
All rights reserved. No part of this method may be reproduced or transmitted in any form or by any means without written permission of the publisher.
PROCEDURE
1. Proceed as directed in AOCS Official Method Da 3-48, Procedure, 1 and 2.1,2
2. Collect the filtrate and washings in a 250 mL Erlenmeyer flask, heat to incipient boiling on either a steam or a water
bath, and add 0.5 mL of phenolphthalein indicator solution.
3. Titrate immediately with standard acid if alkaline or with standard alkali if acidic. Use 0.1 M for samples contain-
ing small amounts of free acid or free alkali (10% or less) and 0.25 M for all other samples.
CALCULATIONS
NOTES
1 Soaps containing little or no alkaline salts need not be filtered as directed in AOCS Official Method Da 3-48 as noted
in Procedure, 2, before proceeding with the determination of free acid or free alkali. However, when substances such
as silicates, phosphates, or other similar salts that influence the titration are present, filtration is essential. Carbonates,
up to 0.5% as Na2CO3, do not affect the determination appreciably and may be omitted, providing a carbonate deter-
mination on a separate sample indicates the quantity not to be in excess of this amount.
2 Avoid exposure to carbonation at any time since this will seriously affect results.
All rights reserved. No part of this method may be reproduced or transmitted in any form or by any means without written permission of the publisher.
Tetrachloroethylene (perchloroethylene) is a colorless, volatile, nonflammable liquid stances. Perform manipulations under a properly operating fume hood. Take partic-
chlorinated hydrocarbon that will emit toxic fumes of phosgene when exposed to ular precautions, such as the use of a glove box, when toxins are in dry form, because
sunlight or flames. It is an irritant to eyes and skin. The TLV is 50 ppm in air. of their electrostatic nature and resulting tendency to disperse in working areas. Swab
accidental spills of toxin with 5% NaOCl bleach. Rinse all glassware exposed to tox-
Tetrahydrofuran is a highly flammable liquid and a dangerous fire risk. The flammable ins with 1% NaOCl bleach solution and then wash thoroughly with warm water.
limits in air are 2–11%. It is toxic by ingestion and inhalation. The TLV in air is 200
ppm. It tends to form peroxides upon storage in air.
REFERENCES
Toluene is a highly flammable liquid and a dangerous fire risk. Explosive limits in air
are 1.27–7%. It is toxic by ingestion, inhalation, and skin absorption. The TLV is Official Methods of Analysis, Association of Official Analytical Chemists, 14th edn.,
100 ppm in air. A fume hood should be used at all times when using toluene. 1984, pp. 1010–1015.
Trichloroethane is a synthetic, light-sensitive, volatile, colorless, liquid miscible with Standard Methods for the Analysis of Oils, Fats and Derivatives, 7th edn., Blackwell
many nonpolar organic solvents. It is an irritant to eyes and skin. The TLV is 350 Scientific Publications, 1987.
ppm in air.
Hawley’s Condensed Chemical Dictionary, 11th edn., revised by N. I. Sax and R. J.
Xylene is flammable and a dangerous fire risk. The TLV is 100 ppm in air. Lewis, Jr., 1987.