1、Designation: D460 91 (Reapproved 2014)Standard Test Methods forSampling and Chemical Analysis of Soaps and SoapProducts1This standard is issued under the fixed designation D460; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.These methods are identical in substance with the standard methods of the American Oil Chemists Society which were develope
3、d bythe Committee on Soap Analysis A-1 of that Society, and with those of the American Chemical Society.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 These test methods cover the sampling and chemicalanalysis of cake, powdered, flake, liquid, and p
4、aste soaps, andsoap products.1.2 The test methods appear in the following order:SAMPLINGSectionGeneral Requirements 4Cake Soaps, Flake and Powdered Soap Products whenPacked in Cans or Cartons 5Flake and Powdered Soap Products when in Bulk 6Liquid Soap 7Paste Soap Products 8Preparation of Samples 9Te
5、st Methods for Chemical AnalysisSafety Precautions 10Purity of Reagents 11Duplicate Tests 12Moisture:Choice of Method 13Method AMatter Volatile at 105C (Oven Method) 14Method BDistillation Method 1518Total Matter Insoluble in Alcohol 19 and 20Free Alkali or Free Acid 21Matter Insoluble in Water 22To
6、tal Alkalinity of Matter Insoluble in Alcohol, Alkaline Salts 23Combined Alkali, Total Anhydrous Soap 24 and 25Combined Sodium and Potassium Oxides 2629Free Alkali and Potassium Carbonate in Potash PasteSoaps 3032Unsaponified plus Unsaponifiable Matter 3335Unsaponifiable Matter 3638Unsaponified Matt
7、er 39Rosin (McNicoll Method) 4043Preparation of Total Fatty Matter, Fatty and Rosin Acids,and Unsaponified Matter 44 and 45Titer Test 46 and 47Acid Number of Fatty Acids 48 and 49Iodine Number (Wijs Method) 5052Chlorides 5355Borax 5658Silica Present as Alkaline Silicates 59 and 60Carbon Dioxide (Car
8、bonates):Train-Absorption Method 6164Evolution-Volumetric Method 6568Phosphates 6976Tetrasodium Pyrophosphate 7779Sulfates 80 and 81Glycerine, Sugars, and Starch:Glycerine in the Absence of Sugars 8284Glycerine in the Presence of Sugars 85 and 86Starch 87 and 88Sugars 89 and 90Volatile Hydrocarbons
9、9195Copper (Trace Amounts) 96 102Precision and Bias 1031.3 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.4 This standard does not pur
10、port to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 1
11、0. Material Safety Data Sheets areavailable for reagents and materials. Review them for hazardsprior to usage.2. Referenced Documents2.1 ASTM Standards:2D216 Method for Distillation of Natural GasolineD459 Terminology Relating to Soaps and Other DetergentsD1193 Specification for Reagent Water1These
12、test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved Jan. 1, 2014. Published February 2014. Origi
13、nallyapproved in 1937. Last previous edition approved in 1997 as D460 91(2005).DOI: 10.1520/D0460-91R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standard
14、s Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E1 Specification for ASTM Liquid-in-Glass Thermometers3. Significance and Use3.1 Soap and soap products are widely used. These testmethods are
15、suitable for setting specifications and performingquality control on soap and soap products.SAMPLING4. General Requirements4.1 The seller shall have the option of being represented atthe time of sampling, and when he so requests shall befurnished with a duplicate sample.5. Cake Soaps, Flake and Powd
16、ered Soap ProductsWhen Packed in Cans or Cartons5.1 One cake (can or carton) shall be taken at random fromnot less than 1 % of the sellers shipping containers, providedeach package contains not less than 50 lb (22.7 kg). In the caseof smaller containers, a cake (can or carton) shall be taken atrando
17、m from each lot of containers totaling not more than 5000lb (2268 kg), or fraction thereof. The gross sample shall in allcases consist of not less than three cakes (cans or cartons) takenat random from separate containers. To illustrate, if a totalshipment consists of 70 000 lb, all in 1400 containe
18、rs weigh-ing 50 lb each, then 14 containers are chosen at random andone cake taken from each for a total sample of 14 cakes. If atotal shipment of 70 000 lb includes containers weighing lessthan 50 lb, then the shipment must be divided into 14 lots ofcontainers weighing approximately 5000 lb each, a
19、nd one caketaken from each lot, again for a total sample size of 14 cakes.The gross sample shall in all cases consist of not less than threecakes (cans or cartons) taken at random from separate contain-ers. In the case of very large lots where the sample drawn asabove will amount to more than 20 lb
20、(9.1 kg), the percentageof packages sampled shall be reduced so that the amount drawnshall not exceed 20 lb. The individual cakes (cans or cartons)shall be sealed at once in moisture-proof containers such aspolyethylene bags, or tightly wrapped in paraffined paper andsealed by rubbing the edges with
21、 a heated iron. The inspectorshall accurately weigh each wrapped cake (can or carton), andrecord its weight and the date of weighing on the wrapper. Thewrapped cakes (cans or cartons) shall be placed in an airtightcontainer, which should be nearly filled, and which shall thenbe sealed, marked, and s
22、ent to the laboratory for test. Samplesshall be kept cool until tested.6. Flake and Powdered Soap Products When in Bulk6.1 A grab sample of not less than 0.5 lb (227 g) shall betaken at random from not less than 1 % of the sellers shippingcontainers, provided each package contains not less than 100
23、lb(45.4 kg). In the case of smaller containers, a grab sample ofnot less than 0.5 lb shall be taken at random from each lot ofcontainers totaling not more than 10 000 lb (4536 kg) orfraction thereof. The gross sample shall in all cases consist ofnot less than three grab samples of 0.5 lb each taken
24、at randomfrom separate containers. In the case of very large lots wherethe sample drawn as above will amount to more than 20 lb (9.1kg), the percentage of packages sampled shall be reduced sothat the amount drawn shall not exceed 20 lb. The inspectorshall rapidly mix the gross sample and place it in
25、 an airtightcontainer, which shall be filled, sealed, marked, accuratelyweighed, its weight and the date of weighing recorded on thepackage, and sent to the laboratory for test. Samples shall bekept cool until tested.7. Liquid Soap7.1 A sample of not less than 0.5 pt (236.6 mL) shall betaken at rand
26、om from not less than 1 % of the sellers shippingcontainers, provided each package contains not less than 10 gal(37.9 L). In the case of smaller containers, a sample of not lessthan 0.5 pt shall be taken at random from each lot of containerstotaling not more than 1000 gal (3785.4 L) or fraction ther
27、eof.The gross sample shall in all cases consist of not less than threesamples of 0.5 pt each taken at random from separate contain-ers. Before drawing the sample from the container selected, thecontents of the container shall be thoroughly agitated. Theinspector shall thoroughly mix the gross sample
28、, place it inclean, dry cans or bottles, which shall be completely filled andsecurely stoppered with clean corks or caps, then sealed,marked, and sent to the laboratory for test.8. Paste Soap Products8.1 When Packed in Cans or Cartons of 5 lb (2.27 kg) orLessOne can or carton shall be taken at rando
29、m from not lessthan 1 % of the sellers shipping containers, provided eachpackage contains not less than 50 lb (22.7 kg). In the case ofsmaller containers, a can or carton shall be taken at randomfrom each lot of containers totaling not more than 5000 lb(2268 kg) or fraction thereof. The gross sample
30、 shall in allcases consist of not less than three cans or cartons taken atrandom from separate containers. In the case of very large lotswhere the sample drawn as above will amount to more than 20lb (9.1 kg), the percentage of packages sampled shall bereduced so that the amount drawn shall not excee
31、d 20 lb. Thesamples shall be wrapped, sealed, marked, and sent to thelaboratory for test.8.2 When Packed in BulkA trier sample3of not less than0.5 lb (227 g) shall be taken at random from not less than 1 %of the sellers shipping containers, provided each packagecontains not less than 50 lb. In the c
32、ase of smaller containers,a trier sample3of not less than 0.5 lb shall be taken at randomfrom each lot of containers totaling not more than 5000 lb orfraction thereof. The gross sample shall in all cases consist ofnot less than three 0.5-lb samples, each taken at random fromseparate containers. With
33、 very large lots where the sampledrawn as above will amount to more than 10 lb (4.5 kg), thepercentage of packages sampled shall be reduced so that theamount drawn shall not exceed 10 lb. The inspector shallpromptly place the gross sample in a clean, dry, airtight and3A trier sample is obtained by i
34、nserting a trier into the material. A trier is ahalf-round steel cylinder12 to34 in. (12.7 to 19.1 mm) in diameter, 6 to 36 in. (152to 914 mm) in length, pointed on one end and having a grip handle on the other end.After insertion, the trier is turned two or three times, and upon removal a core of t
35、hematerial being sampled is obtained.D460 91 (2014)2watertight container, which shall be filled, sealed, marked, andsent to the laboratory for test.9. Preparation of Samples9.1 Cake SoapGrind all bars through a suitable foodchopper. In the case of large samples, it is permissible toquarter the bars
36、and grind one quarter from each bar. However,each ground sample should consist of at least 3 lb (1.36 kg).Mix all ground samples thoroughly on a clean, dry,nonabsorbent, impervious surface with a spatula. Divide intofour quarters and discard the two opposite quarters. Combine,remix, and requarter th
37、e remaining two quarters. Continue inthis manner until the sample is reduced to approximately 2 lb(0.91 kg). Place this portion in a clean, dry sample container.Close tightly and label completely for identification. This is thesample for analysis and must be preserved in a cool dry place.9.2 Powdere
38、d and Chip SoapsRapidly disintegrate andmix the sample of powdered, flake, or chip soap. If desired,quarter down to about 1 lb (454 g). Weigh at once all portionsfor analysis, preserving the remainder in an airtight containerin a cool place.9.3 Liquid SoapNo preparation of the sample of liquidsoap,
39、other than a thorough mixing, is necessary unless it isreceived during very cold weather, when it should be allowedto stand at least 1 h after it has warmed to room temperature(20 to 30C) before it is tested, particularly for its latheringqualities.9.4 Paste Soap ProductsMix the sample of paste soap
40、products thoroughly by kneading and quarter down to about 1lb (454 g). Weigh at once all portions for analysis, preservingthe remainder in an airtight container in a cool place.METHODS FOR CHEMICAL ANALYSIS10. Hazards10.1 PrecautionAll reagents and chemicals should behandled with care. Before using
41、any chemical, read and followall safety precautions and instructions on the manufacturerslabel. Clean up any spill immediately. Consult the MaterialSafety Data Sheet for specific handling and disposal informa-tion.10.2 Use of glass wool in place of asbestos cloth isrecommended where applicable.11. P
42、urity of Reagents11.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available
43、.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.11.2 Unless otherwise indicated, references to water shall beunderstood to mean Type III reagent water conforming toSpecific
44、ation D1193.12. Duplicate Tests12.1 When a determination shows nonconformity with thespecifications a duplicate test shall be made.MOISTURE13. Choice of Test Method13.1 The oven method described in Section 14 is generallyapplicable to all soaps, but certain exceptions to this methodmust be made if a
45、ccurate results are desired. These exceptionsinclude the following:13.1.1 For soaps containing appreciable amounts of sodiumsilicate, the distillation method (Sections 1518) is preferred.13.1.2 Soaps of linseed and other oxidizing oils absorboxygen, and if the oven method is used may gain weight nea
46、rthe end of the test. Therefore, either an inert atmosphere orvacuum oven should be used. The distillation method is alsoapplicable to these types of soap.13.1.3 Soaps containing appreciable amounts of glycerin,such as cold-made and semiboiled (including paste soaps),usually give high results by the
47、 oven method. The distillationmethod is preferred for most accurate results on these types ofsoaps.Method AMatter Volatile at 105C (Oven Method)14. Procedure14.1 Weigh 5 6 0.01 g of the sample in a porcelain or glassdish about 6 to 8 cm in diameter and about 2 to 4 cm in depth,and dry to constant we
48、ight in an air oven at a temperature of105 6 2C. Constant weight is attained when successiveheating for 1-h periods shows a loss (or gain) of not more than0.1 %.Method BDistillation Method15. Apparatus15.1 The apparatus required consists of a glass flask heatedby suitable means and provided with a r
49、eflux condenser4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D460 91 (2014)3discharging into a trap and connected to the flask. Theconnections between the trap and the condenser and flask shallbe interchange
