1、Designation: D 1570 95 (Reapproved 2003)Standard Test Methods forSampling and Chemical Analysis of Fatty Alkyl Sulfates1This standard is issued under the fixed designation D 1570; 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.1. Scope1.1 These test methods cover the sampling and chemicalanalysis of paste, powder, or liquid detergent fatty alkyl
3、sulfates.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 Mat
4、ter 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 eit
5、her 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
6、 appro-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:D 216 Method for Distillation of Nat
7、ural Gasoline2D 1172 Test Method for pH of Aqueous Solutions of Soapsand Detergents3D 1193 Specification for Reagent Water4SAMPLING3. 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
8、.4. Powders and 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 total
9、ing not more than 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 percenta
10、ge of packages 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 w
11、eighing on the 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 of Soaps and Syn
12、thetic Detergents.Current edition approved April 15, 1995. Published June 1995. Originallypublished as D 1570 58 T. Last previous edition D 1570 89.2Discontinued 1988, see 1987 Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 15.04.4Annual Book of ASTM Standards, Vol 11.0
13、1.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.which shall then 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.
14、5 lb (227 g) atrandom 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, 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 (45
15、36 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 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 pac
16、kages sampled so thatthe amount drawn shall not exceed 20 lb (9.1 kg). Theinspector shall rapidly mix the gross sample and place it in 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
17、 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 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, take a sample
18、 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. 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 sampl
19、efrom the container selected, thoroughly agitate the contents ofthe container. The inspector shall thoroughly mix the grosssample, place 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 f
20、or 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 %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
21、each lot ofcontainers totaling not more than 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 (
22、9.1 kg), reducethe percentage of packages sampled so that the amount drawnshall not exceed 20 lb (9.1 kg). The samples shall be wrapped,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 t
23、han 1 %of the sellers shipping containers, provided each packagecontains not less than 50 lb (22.7 kg). In the case of smallercontainers, 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
24、sample shall inall cases consist of not less than three 0.5-lb (227-g) samples,each taken at random from separate containers. With very 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
25、 10 lb (4.5 kg). Theinspector shall promptly place the gross sample in a clean, dry,airtight and watertight container, which shall be 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 cyl
26、inder12 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 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 Powder
27、s and FlakesMinimizing exposure to air, rap-idly disintegrate and mix the sample of powdered, flake, orchip product. If desired, quarter 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
28、of the sample of liquid, otherthan a thorough mixing, is necessary unless it is receivedduring very cold weather, when it should be allowed 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 pr
29、eferably in glass. If crystals separate,melt on water bath.NOTE 2If pastes or liquids are known to be acidic, and decompositionof sample can result from heating, the samples shall be adequately labeledfor precautionary treatment and warmed to room temperature or othermaximum temperature as agreed up
30、on for mixing and sampling.D 1570 95 (2003)2TEST METHODS OF CHEMICAL ANALYSIS9. Purity of Reagents9.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the Ameri
31、can Chemical Society, where suchspecifications are available.5Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.9.2 Unless otherwise indicated, references to water shall beun
32、derstood to mean reagent water conforming to SpecificationD 1193.10. Duplicate Tests10.1 When a determination shows nonconformity with thespecifications, a duplicate test shall be made.MOISTURE BY THE DISTILLATION TEST METHOD11. Apparatus11.1 The apparatus shall consist of a glass flask heated bysui
33、table means and provided with a reflux condenser discharg-ing into a trap and connected to the flask. The connectionsbetween the trap and 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.
34、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 the 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
35、 heat control.11.1.3 CondenserA water-cooled glass reflux condenser(Fig. 1), having a jacket approximately 1534 in. (400 mm) inlength, with 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 inse
36、rtedin 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 condenser 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
37、sealed-intype of condenser, but any other condenser fulfilling thedetailed requirements of this paragraph may be used.11.1.4 TrapFor greatest accuracy several trap sizes areallowable, depending upon the percentage of moisture ex-pected:Moisture Expected, % Size of Trap, mL0 to 5, incl 5Over 5 to 17,
38、 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, constructed 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-mL d
39、ivisions 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 TrapSubdivided 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 2
40、5 mL in 0.2-mL divisions.NOTE 3The condenser and trap should be thoroughly cleaned beforeuse.12. Solvent12.1 Xylene (or Toluene)Saturate xylene (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
41、-mL flask, equipped with the sizeof trap specified in 11.1.4, an amount of sample according tothe percentage of moisture expected, as follows: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
42、 70, incl 30 6 3Over 70 to 85, incl 25 6 2AWeighed to the nearest 0.25 g.5Reagent 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 LaboratoryC
43、hemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.FIG. 1 Assembly of Distillation ApparatusD 1570 95 (2003)3Add immediately about 100 mL of xylene or toluene. Placea small, thin sheet of long-f
44、iber, chemical-resistant glass 3286on the surface of the toluene. The glass wool should bethoroughly dried in the oven and held in the desiccator beforeuse.13.2 Connect the flask and receiver to the condenser andpour sufficient xylene or toluene down the condenser tube tocause a slight overflow thro
45、ugh the side tube. Wrap the flaskand tube leading to the receiver with asbestos cloth, so thatrefluxing will be under better control.13.3 Heat 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 s
46、hould be approximately100 drops/min. When the greater part of the water has distilledover, increase the distillation rate to 200 drops/min until nomore water is collected. Purge the reflux condenser during thedistillation with 5-mL portions of xylene (or toluene) to washdown any moisture adhering to
47、 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 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
48、 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 distillate 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 = vol
49、ume of water, mL at 20C, andW = weight of the sample, g.pH15. Procedure15.1 Determine pH in accordance with Test Method D 1172,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 acid. Hydrochlo-ric acid is preferable. Standard acid weaker than 1 N may beused and titrations calculated to the equivalent in terms of 1 Nsolution.17.2 Indi
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