SAMPLING AND ANALYSIS OF SOAP AND SOAP PRODUCTS AOCS E AOCS Official Method Da 12-48 Rosin, McNicoll Method DEFINITION “This method determines the rosin in furry acids SCOPE Applicable to all soaps and soap produets containing rosin. Replaces Da 12-42. APPARATUS 1. Esterification fask—150 mL round-bottom o Erlenmeyer type. 2. Reflux condenser—water-cooled. Escrification flask and condenser with ground-plass joins ‘ °4o are preferted, 3. Extraction eylinder or Soke fask— (@) Extraction cylinder, 250 ml. capacity, with glass stopper, about 39 mm dia and 355 mm high. (@) The Stokes fask is « 100 mL. roand:bottom flak sealed onto a 150 mL Eelenmeyer flask (See Fig, 1 in AOCS Official Method Da 8-48) 4, Siphon—a two-hole rubber stopper fitted with small diameter glass tubing constructed to permit removal ofthe upper layer from the extraction eyinder or Stokes fas. 5. Buretes—50 ml 6. Separator funnel—500 ml 7. Graduated eylinden—50 and 100 mL 8. Glas beads 9. Beakers—2000 mL, 250 ml. REAGENTS 1. Ethyl alcohol—95%6 (se Notes, Ceution). 2 Sulfuric acid (H,50,). 025 M. 3 Sulfuric acid (H}SO))—I:1, ve with distilled water (se Notes, Caution). 4 Sodium chloride (NaC) solutions—sacraed soltion in water and 10% solution in water, sing reagent grade NaCl 5, Peoleam ether—AOCS Specification 1 2-41 (ce Not, Caution) 6. Methyl orange indicator solution ~0.019%6, prepared by disolving 0.1 g of methyl orange indicator in 100 ml. of distilled Filer paper—qualitave grade, rapid fil Alcoholic potassium hydroxide (KOH) solution, 0.2 M—accurately standardized. See AOCS Specification H 15-52. SDA Formulas 30 and 3A are permitted. Due to the volatility ofthe alcohol, ths olution should be standardized frequently. 9. Naphthalenc-B-sulfonic acid solution—prepared by dissolving 40 g of naphthalene-B-sulfonic acid in| L of absolute methyl alcohol 10, Phenolphthalen indicator solution —I.0%6 in 9596 ethyl alcohol PREPARATION OF FATTY AND ROSIN ACIDS 1. Dissolve 50 g of original test sample in 500 mL of hot water contained in a 1000 mL. beaker or other convenient ‘Note—f che sample contains alcohol, chs must be completely evaporated from the soap solution before proceeding. 2. Add 100 mL of 1:1 sulfuric acid and afew glass beads co minimize bumping and heat gently until the fatty matter collects ina clear layer on the top. 3. Remove the aqueous acid (lower) layer with a siphon, add 300 mL. of hot water, bol gently for afew minus, and again remove the aqueous acid layer witha siphon, 4, Wash the acids chee times in this manner. Complete the acidification and washing in as short a period as possible, keeping, the beaker covered to prevent oxidation ofthe aids, 5. After washing, allow to sele for a few minutes and chen decane the fatty acids carefully o a8 not to include any water. Filter through one or ewo thicknesses of filter paper into a 250 ml. beaker or Soxhlet flask and dry at 105 + 2°C for 45-60 min ‘Nore—An alternate method of drying isto heat the fay acids rapidly on a hot plate to 130%C. Do not hold at this temperature nor rcheat more than once. If watt is sll present after the fist heating, allow to sete, decant the fatty acids, and then refiter and reheat momentarily o 130°C. The acids must be thoroughly dry. Page tof 2[BARC RDNA Sox ANS oar ROOTES — ] |Da 12-48 + Rosin, MeNicoll Method | PROCEDURE 1, Weigh accurately 2 g of faey acids into the esterification ask and add 25 mL of naphthalene-B-sulfonic acid solution. Add a few glass beads o ensure smooth boiling, attach the reflux condenser, and boil for 30 min. 2, Prepate and conduct a blanc determination simuleancously and identical in all respects. 3. Atthe end ofthe boiling period, cool the contents of the flak, add 0.5 mL of indicator, and trate immediately with 0.2 M_ KOH to the fire pink color which persists for 30 sec CALCULATIONS. (SB) x M x 346 Inass of test portion, g rosin, uncorrected (from Calculation, 1) ~ 1.0 (See Numbered Notes 1) 1, Rosin in fate acids, uncorrected, % = 2. Rin a rd 3: Rn inl ingle xn inf i os Caton, 2) 4 Rind apn igi espe = a ogi gl 106 ve SToloeof sian ml fmt bono ann fa cry of ra KO son € Rinses map’ snore » 002909 15 cid hon ASC Oa Net Doo aad SO NOTES Caution Sulfuric acid isa strong acid and will case severe burns. Protective clothing should be worn when working with this acid It is a dehydrating agent and should not be stored in the vicinity of organic materials. Use great caution in ming with water due to hneat evolution chat can cause explosive spatering. Always add the acid co water, never the reverse Petroleum ether is extremely flammable, Avoid static electricity. The explosive limits in air are 1~6%, A Fame hood should bbe used at al times when using pecroleum ether Echyl alcohol (ethanol) i Nammmable, Use an effective fame-removal device when heating or evaporating. ‘Methyi alcohol is flammable and toxic, Avoid contact with eyes, Avoid breathing vapors. Use effective ame-removal device NUMBERED NOTES, 1. Cooperative studies have shown that the MeNicoll method gives results about 1% higher than the amount of actual rosin present, The Technical Commitece recommends, herefore, that 1% be deducted from the percentage rosin found in the Faty acids 2, Wheneve less than 596 rosin is fous setual presence of absence of rosin. Liebermann Storch Tee—Place 1~2 ml of the fatty acids ino ates ube, add 5-10 ml. of acetic anhydride, and warm fon a steam bath. Cool, pour 1-2 ml. into a white porcelain dish, and allow 1 ot 2 drops of H,SO, (sp. . 1:53) to run down, the inside ofthe dish. If rosin is present, a fleeting violet color is produced immediately at the point of contact. The color changes co a brownish tinge. Check the rest using a sample of fart acids to which has been added small amount of rosin ‘Cholesterol and some other substances give a similar test the qualitative Liebermann-Scorch (following) test should be applied co confirm the Page 2 of 2