ANALYSIS OF SOAP CONTAININC SYNTHETIC DETERCENTS

AOS* AOCS Official Method Db 2-48

Reapproved 2009

Alcohol-Sol uble and Alcohol-l nsol uble Matter

DEFINITION
This method determines the alcohol-soluble and alcohol-insoluble matter in the sample.
1. The alcohol-soluble matter will contain all of the anhydrous (real) soap, and some inorganic salts. Most,
if not all, of the sodium chloride will be included. This method is satisfactory for the approximate
determination of soap (when buyer and selier agree) with products which contain a high percentage of
alcohol-insoluble matter such as cleansers, soap powders, scouring compounds, and pastes.
2. The alcohol-insoluble matter will contain most of the alkali salts such as carbonates, borates, silicates,
and phosphates as weli as sulfates and starch. This method may be used for the approximate determi-
nation of these constituents. These salts are not entirely insoluble in alcohol so for the most accurate
results, use separate portions of the sample and follow the specific method for each constituent.
SCOPE
Applicable to all soap and soap products containing synthetic detergents. Replaces Da3-42.

APPARATUS
1. Beakers or Erlenmeyer flasks-25O mL.
2. Filter paper-the filter paper must imparr no acidiry or alkalinity to neutral alcohol when poured through it. Place filter
paper in a weighing bottle or metal container (seamless container with tight-fitting slipover cover) and dry in an air oven at
105 t 2"C with cover removed. Remove from the oven, replace cover, cool to room temperature in a desiccator, and weigh.
Reweigh after filtration (see Procedure,T) in the same container.
3. \fatch glasses.
4. Air oven-maintained at 105 t 2'C. AOCS Specification H 3-45.
5. Filter flask-500 mL.

REAGENTS
1. Ethyl alcohol-95% or absolute. SDA Formulas 30 and 3A are permitted (see Notes, Caution). Add 3-5 drops of phenol-
phthalein indicator solution. Boil and neutralize with dilute sodium hydroxide (NaOH), 0.1-0.2 M solution, to a faint pink
color just before using.
2. Phenolphthalein indicatsl 56lu1i6n-7o/o in 95o/o alcohol.

PROCEDURE
1. \Weigh a test portion of such size that it will yield 0.1-1.0 g of alcohol-insoluble matter. Place in 250 mL flask or beaker, add
200 mL of alcohol, cover with a watch glass, and heat on a steam bath with frequent stirring until the soap is dissolved.
2. Filter into a filter flask through the tared filter paper with the aid of vacuum, retaining in the beaker as much of the residue
as possible. Repeat this extraction and decantation three times, using 25 mL of hot alcohol each time.
3. After decanrarion, evaporate (see Notes, Caution) any aicohol remaining in the beaker on a steam or water bath and then
dissolve the residue in the smallest possible amount of distilled water. Usually 5 mL is sufficient.
4. Add 500 mL of absolute alcohol slowly, stirring vigorously, to reprecipitate the insoluble matter. Heat to boiling on a steam
or water bath and filter through the paper or crucible.
5. Wash all of the residue into fie filter and wash the filter several times with hot95o/o alcohol to remove all of the alcohol-soluble matter.
6. Combine the alcohol filtrate (see Procedure, 2) and the washings (see Procedure, J) in x 616d 250 mL beaker and evaporate on a stearn or
water bath. Dry to constant weight in an oven at 105 t 2"C. Cool to room temperature in a desiccator and weigh. See Calculations, 1.
7. Dry the residue on the tared filter paper in an oven at 105 t 2"C for 3 hr. Cool to room temperature in a desiccator and
weigh. See Calculations, 2.

CALCULATIONS
mass' g of residue in beaker
1. Alcohor-soluble matter, oro
- t too
mass tes( ponion. g
mass' g ofinsoluble matter
2. Alcohor-insoruble marrer, oro
- * ,oo
mass test ponion, g

NOTES
Caution
Ethanol (ethyl aicohol) is flammable. Use a properly operating fume hood when heating or evaporating.

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