1、Designation: D 460 91 (Reapproved 2005)Standard Test Methods forSampling and Chemical Analysis of Soaps and SoapProducts1This standard is issued under the fixed designation D 460; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 devel
3、oped 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 Department of Defense.1. Scope1.1 These test methods cover the sampling and chemicalanalysis of cake, powdered, flake, liquid, and pas
4、te 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 9Test
5、 Methods for Chemical AnalysisSafety Precautions 10Purity of Reagents 11Duplicate Tests 12Moisture:Choice of Method 13Method AMatter Volatile at 105C (Oven Method) 14Method BDistillation Method 15-18Total Matter Insoluble in Alcohol 19 and 20Free Alkali or Free Acid 21Matter Insoluble in Water 22Tot
6、al Alkalinity of Matter Insoluble in Alcohol, Alkaline Salts 23Combined Alkali, Total Anhydrous Soap 24 and 25Combined Sodium and Potassium Oxides 26-29Free Alkali and Potassium Carbonate in Potash PasteSoaps 30-32Unsaponified plus Unsaponifiable Matter 33-35Unsaponifiable Matter 36-38Unsaponified M
7、atter 39Rosin (McNicoll Method) 40-43Preparation 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) 50-52Chlorides 53-55Borax 56-58Silica Present as Alkaline Silicates 59 and 60Carbon Dioxi
8、de (Carbonates):Train-Absorption Method 61-64Evolution-Volumetric Method 65-68Phosphates 69-76Tetrasodium Pyrophosphate 77-79Sulfates 80 and 81Glycerine, Sugars, and Starch:Glycerine in the Absence of Sugars 82-84Glycerine in the Presence of Sugars 85 and 86Starch 87 and 88Sugars 89 and 90Volatile H
9、ydrocarbons 91-95Copper (Trace Amounts) 96-102Precision and Bias 1031.3 The values stated in inch-pound units are to be regardedas the standard. The metric equivalents of inch-pound unitsmay be approximate.1.4 This standard does not purport to address all of thesafety concerns, if any, associated wi
10、th 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 10. Material Safety Data Sheets areavailable for reagents and mat
11、erials. Review them for hazardsprior to usage.2. Referenced Documents2.1 ASTM Standards:2D 216 Method for Distillation of Natural GasolineD 459 Terminology Relating to Soaps and Other DetergentsD 1193 Specification for Reagent WaterE1 Specification for ASTM Thermometers3. Significance and Use3.1 Soa
12、p and soap products are widely used. These testmethods are suitable for setting specifications and performingquality control on soap and soap products.1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD1
13、2.12 on Analysis of Soaps and Synthetic Detergents.Current edition approved May 1, 2005. Published June 2005. Originallyapproved in 1937. Last previous edition approved in 1997 as D 460 91(1997).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at
14、serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.SAMPLING4. General Requirements4.1 The seller shall
15、 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 Powdered 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 ship
16、ping 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 atrandom from each lot of containers totaling not more than 5000lb (2268 kg), or fraction thereof. The gross sample shall in allcases consist of not l
17、ess than three cakes (cans or cartons) takenat random from separate containers. To illustrate, if a totalshipment consists of 70 000 lb, all in 1400 containers 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
18、 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, and 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 threecak
19、es (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 (9.1 kg), the percentageof packages sampled shall be reduced so that the amount drawnshall not exceed 20 lb. The individual cakes (cans or cart
20、ons)shall be sealed at once in moisture-proof containers such aspolyethylene bags, or tightly wrapped in paraffined paper andsealed by rubbing the edges with a heated iron. The inspectorshall accurately weigh each wrapped cake (can or carton), andrecord its weight and the date of weighing on the wra
21、pper. Thewrapped cakes (cans or cartons) shall be placed in an airtightcontainer, which should be nearly filled, and which shall thenbe sealed, marked, and sent 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
22、 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 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 totali
23、ng 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 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 pe
24、rcentage 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 an airtightcontainer, which shall be filled, sealed, marked, accuratelyweighed, its weight and the date of weighing recorded on thepackage, an
25、d 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 random 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 smalle
26、r 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 thereof.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
27、drawing the sample from the container selected, thecontents of the container shall be thoroughly agitated. Theinspector shall thoroughly mix the gross sample, place it inclean, dry cans or bottles, which shall be completely filled andsecurely stoppered with clean corks or caps, then sealed,marked, a
28、nd 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 random from not lessthan 1 % of the sellers shipping containers, provided eachpackage contains not less than 50 lb (22.7 kg). In the case ofsmaller
29、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 shall in allcases consist of not less than three cans or cartons taken atrandom from separate containers. In the case of very large lotswhere
30、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 exceed 20 lb. Thesamples shall be wrapped, sealed, marked, and sent to thelaboratory for test.8.2 When Packed in BulkA trier sample3of not less than
31、0.5 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 case 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 500
32、0 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 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
33、that theamount drawn shall not exceed 10 lb. The inspector shallpromptly place the gross sample in a clean, dry, airtight andwatertight 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 foodcho
34、pper. In the case of large samples, it is permissible toquarter the bars and grind one quarter from each bar. However,each ground sample should consist of at least 3 lb (1.36 kg).3A trier sample is obtained by inserting a trier into the material. A trier is ahalf-round steel cylinder12 to34 in. (12.
35、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 thematerial being sampled is obtained.D 460 91 (2005)2Mix all ground samples thoroughly on
36、 a clean, dry, nonabsor-bent, impervious surface with a spatula. Divide into fourquarters and discard the two opposite quarters. Combine,remix, and requarter the remaining two quarters. Continue inthis manner until the sample is reduced to approximately 2 lb(0.91 kg). Place this portion in a clean,
37、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 Powdered and Chip SoapsRapidly disintegrate andmix the sample of powdered, flake, or chip soap. If desired,quarter down to about 1 lb (454 g). Weig
38、h 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, other than a thorough mixing, is necessary unless it isreceived during very cold weather, when it should be allowedto stand at least 1 h aft
39、er 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 soapproducts thoroughly by kneading and quarter down to about 1lb (454 g). Weigh at once all portions for analysis, preservingthe remainder in a
40、n airtight container in a cool place.METHODS FOR CHEMICAL ANALYSIS10. Hazards10.1 PrecautionAll reagents and chemicals should behandled with care. Before using any chemical, read and followall safety precautions and instructions on the manufacturerslabel. Clean up any spill immediately. Consult the
41、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. Purity of Reagents11.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatal
42、l reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lesseni
43、ng theaccuracy of the determination.11.2 Unless otherwise indicated, references to water shall beunderstood to mean Type III reagent water conforming toSpecification D 1193.12. Duplicate Tests12.1 When a determination shows nonconformity with thespecifications a duplicate test shall be made.MOISTURE
44、13. 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 accurate results are desired. These exceptionsinclude the following:13.1.1 For soaps containing appreciable amounts of sodiumsilicate, the d
45、istillation method (Sections 15-18) is preferred.13.1.2 Soaps of linseed and other oxidizing oils absorboxygen, and if the oven method is used may gain weight nearthe end of the test. Therefore, either an inert atmosphere orvacuum oven should be used. The distillation method is alsoapplicable to the
46、se 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 oven method. The distillationmethod is preferred for most accurate results on these types ofsoaps.Method AMatter Volatile at 105C (Oven M
47、ethod)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 weight 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)
48、 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 reflux condenserdischarging into a trap and connected to the flask. Theconnections between the trap and the condenser and flask shallbe int
49、erchangeable ground joints. The trap serves to collect andmeasure the condensed water and to return the solvent to theflask. A suitable assembly of the apparatus is illustrated in Fig.1.15.1.1 Flask, 500-mL, of either the shortneck, round-bottomtype or the Erlenmeyer type.15.1.2 Heat SourceThe source of heat may be either anoil bath (stearic acid, paraffin wax, etc.), or an electric heaterprovided with a sliding rheostat or other means of heat control.15.1.3 CondenserA water-cooled glass reflux condenser(Fig. 1), having a jacket approximately 400 mm in leng
