1、Designation: D1570 95 (Reapproved 2009)Standard Test Methods forSampling and Chemical Analysis of Fatty Alkyl Sulfates1This standard is issued under the fixed designation D1570; 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.1. Scope1.1 These test methods cover the sampling and chemicalanalysis of paste, powder, or liquid detergent fatty alkylsul
3、fates.1.2 The procedures for sampling and analysis appear in thefollowing order:SectionsSampling:Powders and Flakes Packed in Cans or Cartons 4Powders and Flakes in Bulk 5Liquids 6Pastes 7Preparation of Sample 8Moisture by the Distillation Test Method 11-14pH 15Alkalinity 16-19Alcohol-Soluble Matter
4、 20-22Alcohol-Insoluble Matter 23 and24Unsulfated Material 25-28Combined Alcohols 29-32Ester SO3:Method A. Titration Test Method 36 and37SectionsEster SO3:Method B. Gravimetric Test Method 38 and39Sodium Sulfate 40-43Chlorides Calculated as Sodium Chloride (NaCl) 44-471.3 The values stated in either
5、 inch-pound or SI units are tobe regarded separately as the standard. The values given inparentheses are for information only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish ap
6、pro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Material SafetyData Sheets are available for reagents and materials. Reviewthem for hazards prior to usage.2. Referenced Documents2.1 ASTM Standards:2D216 Method for Distillation of Natura
7、l GasolineD1172 Guide for pH of Aqueous Solutions of Soaps andDetergentsD1193 Specification for Reagent WaterSAMPLING3. General Requirement3.1 The seller shall have the option of being represented atthe time of sampling and when he so requests, shall befurnished with a duplicate sample.4. Powders an
8、d Flakes Packed in Cans or Cartons4.1 Take one can or carton at random from not less than 1%of the sellers shipping containers, provided each packagecontains not less than 50 lb (22.7 kg). In the case of smallercontainers, take a can or carton at random from each lot ofcontainers totaling not more t
9、han 5000 lb (2268 kg) or fractionthereof. The gross sample shall in all cases consist of not lessthan three cans or cartons taken at random from separatecontainers. In the case of very large lots where the sampledrawn as above will amount to more than 20 lb (9.1 kg), reducethe percentage of packages
10、 sampled so that the amount drawnwill not exceed 20 lb (9.1 kg). Tightly wrap the individual cansor cartons at once in paraffined paper and seal by rubbing theedges with a heated iron. The inspector shall accurately weigheach wrapped can or carton and record its weight and the dateof weighing on the
11、 wrapper. Place the wrapped cans or cartonsin an airtight container, which should be nearly filled, and1These 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, Sy
12、nthetics, Detergents and theirComponents.Current edition approved Oct. 1, 2009. Published December 2009. Originallyapproved in 1958 as D1570 58 T. Last previous edition approved in 2003 asD1570 95(2003). DOI: 10.1520/D1570-95R09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, o
13、rcontact ASTM Customer Service at 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.which shall then
14、be sealed, marked, and sent to the laboratoryfor test. Samples shall be kept cool until tested.5. Powders and Flakes in Bulk5.1 Take a grab sample of not less than 0.5 lb (227 g) atrandom from not less than 1 % of the sellers shippingcontainers, provided each package contains not less than 100 lb(45
15、.4 kg). In the case of smaller containers, take a grab sampleof not less than 0.5 lb (227 g) 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 (227 g) each taken
16、 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), reduce the percentage of packages sampled so thatthe amount drawn shall not exceed 20 lb (9.1 kg). Theinspector shall rapidly mix the gross sample and place it in
17、 anairtight container, which shall be filled, sealed, marked, accu-rately weighed, with its weight and the date of weighingrecorded on the package, and be sent to the laboratory for test.Samples shall be kept cool until tested.6. Liquids6.1 Take a sample of not less than 0.5 pt (236.6 mL) atrandom f
18、rom 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, take a sample of notless than 0.5 pt (236.6 mL) at random from each lot ofcontainers totaling not more than 1000 gal (3785.4 L) orfraction thereof.
19、 The gross sample shall in all cases consist ofnot less than three samples of 0.5 pt (236.6 mL) each taken atrandom from separate containers. Before drawing the samplefrom the container selected, thoroughly agitate the contents ofthe container. The inspector shall thoroughly mix the grosssample, pla
20、ce it in clean, dry cans or bottles, which shall becompletely filled and securely stoppered with clean corks orcaps, then sealed, marked, and sent to the laboratory for test.7. Pastes7.1 Pastes Packed in Cans or Cartons of 5 lb (2.27 kg) orLessTake one can or carton at random from not less than 1 %o
21、f the sellers shipping containers, provided each packagecontains not less than 50 lb (22.7 kg). In the case of smallercontainers, take a can or carton at random from each lot ofcontainers totaling not more than 5000 lb (2268 kg) or fractionthereof. The gross sample shall in all cases consist of not
22、lessthan three cans or cartons taken at random from separatecontainers. In the case of very large lots where the sampledrawn as above will amount to more than 20 lb (9.1 kg), reducethe percentage of packages sampled so that the amount drawnshall not exceed 20 lb (9.1 kg). The samples shall be wrappe
23、d,sealed, marked, and sent to the laboratory for test.7.2 Pastes Packed in BulkTake a “trier” sample (Note 1)of not less than 0.5 lb (227 g) at random from not less than 1 %of the sellers shipping containers, provided each packagecontains not less than 50 lb (22.7 kg). In the case of smallercontaine
24、rs, take a “trier” sample of not less than 0.5 lb (227 g)at random from each lot of containers totaling not more than5000 lb (2268 kg) or fraction thereof. The gross sample shall inall cases consist of not less than three 0.5-lb (227-g) samples,each taken at random from separate containers. With ver
25、y largelots where the sample drawn as above will amount to more than10 lb (4.5 kg), reduce the percentage of packages sampled sothat the amount drawn shall not exceed 10 lb (4.5 kg). Theinspector shall promptly place the gross sample in a clean, dry,airtight and watertight container, which shall be
26、filled, sealed,marked, and sent to the laboratory for test.NOTE 1A trier sample is obtained by inserting a “trier” into thematerial. A trier is a half-round steel cylinder12 to34 in. (12.7 to 19 mm)in diameter, 6 to 36 in. (152 to 914 mm) in length, pointed on one end andhaving a grip handle on the
27、other end. After insertion, the trier is turnedtwo or three times, and upon removal a core of the material being sampledis obtained.8. Preparation of Sample8.1 Powders and FlakesMinimizing exposure to air, rap-idly disintegrate and mix the sample of powdered, flake, orchip product. If desired, quart
28、er down to about 1 lb (453.6 g).Weigh at once all portions for analysis, preserving the remain-der in an airtight container in a cool place.8.2 LiquidsNo preparation of the sample of liquid, otherthan a thorough mixing, is necessary unless it is receivedduring very cold weather, when it should be al
29、lowed to standat least 1 h after it has warmed to room temperature (20 to30C) before it is tested, particularly for its lathering qualities(Note 2).8.3 PastesStore preferably in glass. If crystals separate,melt on water bath.NOTE 2If pastes or liquids are known to be acidic, and decompositionof samp
30、le can result from heating, the samples shall be adequately labeledfor precautionary treatment and warmed to room temperature or othermaximum temperature as agreed upon for mixing and sampling.D1570 95 (2009)2TEST METHODS OF CHEMICALANALYSIS9. Purity of Reagents9.1 Reagent grade chemicals shall be u
31、sed in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.3Other grades may be used, pro-vided it is first ascertained that the reage
32、nt is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.9.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD1193.10. Duplicate Tests10.1 When a determination shows nonconformity with th
33、especifications, a duplicate test shall be made.MOISTURE BY THE DISTILLATION TEST METHOD11. Apparatus11.1 The apparatus shall consist of a glass flask heated bysuitable means and provided with a reflux condenser discharg-ing into a trap and connected to the flask. The connectionsbetween the trap and
34、 the condenser and flask shall be inter-changeable 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.1.11.1.1 FlaskA 1000-mL flask of either the short-neck,round-bottom type or th
35、e Erlenmeyer type.11.1.2 Heat Source, either an oil bath (stearic acid, paraffinwax, etc.), or an electric heater provided with a sliding rheostator other means of heat control.11.1.3 CondenserA water-cooled glass reflux condenser(Fig. 1), having a jacket approximately 1534 in. (400 mm) inlength, wi
36、th an inner tube38 to12 in. (9.5 to 12.7 mm) inoutside diameter, and not less than14-in. (6-mm) insidediameter, shall be used. The end of the condenser to be insertedin the trap may be ground off at an angle of 30 from thevertical axis of the condenser. When inserted into the trap, thetip of the con
37、denser shall be about14 in. (6 mm) above thesurface of the liquid in the trap after the distillation conditionshave been established. Fig. 1 shows a conventional sealed-intype of condenser, but any other condenser fulfilling thedetailed requirements of this paragraph may be used.11.1.4 TrapFor great
38、est accuracy several trap sizes areallowable, depending upon the percentage of moisture ex-pected:Moisture Expected, % Size of Trap, mL0to5,incl 5Over 5 to 17, incl 10Over 17 to 30, incl 10Over 30 to 50, incl 25Over 50 to 70, incl 25Over 70 to 85, incl 25Traps made of well-annealed glass, constructe
39、d essentiallyas shown in Fig. 1, and graduated to contain one of thefollowing specified volumes at 20C shall be used:11.1.4.1 5-mL TrapSubdivided into 0.1-mLdivisions witheach 1-mL line numbered (5 mL at top). The error in anyindicated capacity may not be greater than 0.05 mL.11.1.4.2 10-mL TrapSubd
40、ivided from 0 to 1 mL in 0.1-mL divisions from 1 to 10 mL in 0.2-mL divisions.11.1.4.3 25-mL TrapSubdivided from 0 to 1 mL in 0.1-mL divisions and from 1 to 25 mL in 0.2-mL divisions.NOTE 3The condenser and trap should be thoroughly cleaned beforeuse.12. Solvent12.1 Xylene (or Toluene)Saturate xylen
41、e (or toluene) withwater by shaking with a small quantity of water and distill. Usethe distillate for the determination.13. Procedure13.1 Transfer to the 1000-mL flask, equipped with the sizeof trap specified in 11.1.4, an amount of sample according tothe percentage of moisture expected, as follows:
42、Moisture Expected, % Weight of Sample to be Used, gA0 to 5, incl 50 6 5Over 5 to 17, incl 50 6 5Over 17 to 30, incl 40 6 4Over 30 to 50, incl 30 6 3Over 50 to 70, incl 30 6 3Over 70 to 85, incl 25 6 2AWeighed to the nearest 0.25 g.3Reagent Chemicals, American Chemical Society Specifications , Americ
43、anChemical 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)
44、, Rockville,MD.FIG. 1 Assembly of Distillation ApparatusD1570 95 (2009)3Add immediately about 100 mL of xylene or toluene. Placea small, thin sheet of long-fiber, chemical-resistant glass 3284on the surface of the toluene. The glass wool should bethoroughly dried in the oven and held in the desiccat
45、or beforeuse.13.2 Connect the flask and receiver to the condenser andpour sufficient xylene or toluene down the condenser tube tocause a slight overflow through the side tube. Wrap the flaskand tube leading to the receiver with asbestos cloth, so thatrefluxing will be under better control.13.3 Heat
46、the oil bath with a gas burner or other source ofheat, or apply heat directly to the flask with an electric heaterand distill slowly. The rate at the start should be approximately100 drops/min. When the greater part of the water has distilledover, increase the distillation rate to 200 drops/min unti
47、l nomore water is collected. Purge the reflux condenser during thedistillation with 5-mL portions of xylene (or toluene) to washdown any moisture adhering to the walls of the condenser. Thewater in the receiver may be made to separate from the xylene(or toluene) by using a spiral copper or nichrome
48、wire. Movethe wire up and down in the condenser occasionally, thuscausing the water to settle at the bottom of the receiver. Refluxfor at least 2 h, and shut off the heat at the end of this period.13.4 Wash down condenser with 1 mL of absolute ethanol(CH3CH2OH). Adjust the temperature of the distill
49、ate to 20Cand read the volume of water.14. Calculation14.1 Calculate the percentage of moisture as follows:Moisture, % 5 V 3 0.998!/W 3 100 (1)where:V = volume of water, mL at 20C, andW = weight of the sample, g.pH15. Procedure15.1 Determine pH in accordance with Test Method D1172,except that the measurement shall be made 10 min afteradjusting the solution of the sample to volume.ALKALINITY16. Apparatus16.1 Buret.16.2 Beaker, 400-mL.17. Reagents17.1 Hydrochloric or Sulfuric Acid, StandardPrepare andstandardize 1 N hydrochloric acid or sulfuric
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