SAMPLING AND ANALYSIS OF SOAP AND SOAP PROBUCTS: CAS, OCS E AOCS Official Method Da 3-48 | Alcohol-Soluble and Alcohol-Insoluble Matter | DEFINITION ‘This method determines the alcohol-soluble and alcohol-insoluble matter in the sample. 1. Thealcohol soluble mater will contain all of te anhydrous (eal) soap and some inorganic salts. Most, if not all, of the sodium chloride willbe included. This method is satisfactory for the approximate determination of soap (when buyer and seller agree) with produets which contain a high percentage of sleakol-iuoluhle mater sich ac cleanser nap powder, scouring compounds. and pastes 2. The alcohol-insoluble matter will contain most of the alkaline salts such as carbonates, borates, sli- cates, and phosphates, as well a sulfates and starch. This method may be used forthe approximate derermination of these constituents. These salts are not entirely insoluble in alcohol, so for the most accurate results, use separate portions ofthe sample and follow the specific method for each SCOPE ‘Applicable to soap and soap products, Replaces Da 3-42. ‘APPARATUS 1. Beakers or Eelenmeyer flasks —250 ml. 2. Fler paper—the filter paper must impart no acidity or alhaliity to neutral alcohol when neutral alcohol is poured through i Place filter paper ina weighing bottle or metal container (seamless, with tight fting slip cover) and dry in an oven at 105 2 °C With cover removed. Remave from oven, replace cover, cool to room temperature in a desiccator, and weigh. Reweigh alier fir: ‘ion (see Procedure, 5) inthe same container. Watch gases Air oven-—maintained at 105 + 2°C, AOCS Specification H 3-45. Filter flask—500 mL Funinel—fitted with rubber stopper to fit the neck of the Filter flask Rotary evaporator: ‘Vacuum puimp ot aspizator. 9, Round bottom flask-—250 mL. with 24/40 glass joins REAGENTS 1. Ethyl aleohol—95% and absolue ethyl alcohol (ee Note, Caution). SDA Formulas 30 and 3A are permitted. Add 3-5 drops (of 1% phenolphthalein indicator solution. Boil and neutralize with dilure sodium hydroxide (NaOH), 0.1-0.2 M solutic toa fine pink color just before using 2. Phenolphthalein indicator solution 1% in 95% alcoho PROCEDURE 1. Weigh atest portion of such size that it will yield 0.1-1.0 g of alcohol-insoluble matte. Place in 250 mi flask or beaker, add 200 mi of alcohol, cover with a watch glas, and heaton a steam bath with frequent stirring until the soap is dissolved 2, Filter into a fas chrough the tare filter paper withthe aid of vacuum, retaining in the beaker as much of che residue as posible. Repeat this eazaction and decantation thece times using 25 ml. of hot alcohol each time 3. Wash all of the residue into the filter and wash the filter several times with hot 95% alcohol ro remove al of che aleohol- soluble matter, 4, Combine the alcohol filtrate (sep 2) and washings (step 3) ina tared 250 mL round bottom flask and evaporate with a rocary ‘evaporator Dry co constant weight in an oven at 103 # 2°C. Cool to room temperature in a desiccator and weigh smass of residue in flask, Aleohol-soluble matter, x 100 ‘mass OF test portion, g 5. Dry the residue on the tare filter paper in an oven at 105 °C for 3 hr. Cool to room temperature in a desicator and weigh ‘mass of insoluble matter, ‘mass of test portion, g Alcohol-insoluble matter, % NOTES Caution Ethanol (ethyl alcobol) is flammable. Use effective fume-removal device when heating or evaporating Page 11