1、Designation: D 1568 05Standard Test Methods forSampling and Chemical Analysis of AlkylbenzeneSulfonates1This standard is issued under the fixed designation D 1568; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. 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 alkylbenzenesulfonates.1.2
3、The procedures for sampling and analysis appear in thefollowing order:SectionsSampling:Powders and Flakes Packed in Cans or Cartons 3Powders and Flakes in Bulk 4Liquids 6Pastes 7Hazards 8Preparation of Sample 9Moisture:Distillation Method 11-14Karl Fischer Method 15-20Total Matter Insoluble in Alcoh
4、ol 21-23Neutral Oil 24-27Chlorides Calculated as Sodium Chloride (NaCl) 28-31pH 321.3 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 appro-priate safety and health practices and d
5、etermine the applica-bility of regulatory limitations prior to use. For a specifichazards statement, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D 1172 Test Method for pH of Aqueous Solutions of Soapsand DetergentsD 1193 Specification for Reagent WaterSAMPLING3. General Requirements3.1
6、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 and Flakes Packed in Cans or Cartons4.1 One can or carton shall be taken at random from not lessthan 1 % of the sellers shipping containers, provi
7、ded 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 shall in allcases consist of not less than three cans or cartons
8、 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 will not exceed 20 lb (9.1kg). The individual cans or cartons shall be tightly w
9、rapped atonce in paraffined paper and sealed by rubbing the edges witha heated iron. The inspector shall accurately weigh eachwrapped can or carton and record its weight and the date ofweighing on the wrapper. The wrapped cans or cartons shall beplaced in an airtight container which should be nearly
10、 filled,and which shall then be sealed, marked, and sent to thelaboratory for test. Samples shall be kept cool until tested.5. Powders and Flakes in Bulk5.1 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 p
11、ackage contains not less than 100 lb(45.4 kg). In the case of smaller containers, a grab sample ofnot less than 0.5 lb (227 g) shall be taken at random from eachlot of containers totaling not more than 10,000 lb (4536 kg) orfraction thereof. The gross sample shall in all cases consist ofnot less tha
12、n three grab samples of 0.5 lb (227 g) each taken atrandom from separate containers. In the case of very large lotsthe sample drawn as above will amount to more than 20 lb (9.1kg), the percentage of packages sampled shall be reduced so1These test methods are under the jurisdiction of ASTM Committee
13、D12 onSoaps and Other Detergents and is the direct responsibility of D12.12 on Analysisof Soaps and Synthetic Detergents.Current edition approved May 1, 2005. Published June 2005. Originallyapproved in 1958. Last previous edition approved in 1997 as D 1568 97.2For referenced ASTM standards, visit th
14、e ASTM website, www.astm.org, orcontact 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,
15、United States.that the 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 la
16、boratory for test.Samples shall be kept cool until tested.6. Liquids6.1 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 smaller containers, a samp
17、le of not lessthan 0.5 pt (236.6 mL) shall be taken at random from each lotof containers 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
18、drawing the samplefrom the container selected, the contents of the container shallbe thoroughly agitated. The inspector shall thoroughly mix thegross sample, place it in clean, dry cans or bottles, which shallbe completely filled and securely stoppered with clean corks orcaps, then sealed, marked, a
19、nd sent to the laboratory for test.7. Pastes7.1 Pastes 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 containers,
20、 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 the sample
21、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 (9.1kg). The samples shall be wrapped, sealed, marked, and sent tothe laboratory for test.7.2 Pastes Packed in BulkA“trier” sample (Note 1)ofnotle
22、ss than 0.5 lb (227 g) 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 containers, a “trier” sample of not less than 0.5 lb (227g) shall be taken at random from each lot of container
23、s totalingnot more than 5000 lb (2268 kg) or fraction thereof. The grosssample shall in all cases consist of not less than three 0.5-lb(227-g) samples, each taken at random from separate contain-ers. With very large lots where the sample drawn as above willamount to more than 10 lb (4.5 kg), the per
24、centage of packagessampled shall be reduced so that the amount drawn shall notexceed 10 lb (4.5 kg). The inspector shall promptly place thegross sample in a clean, dry, airtight and watertight container,which shall be filled, sealed, marked, and sent to the laboratoryfor test.NOTE 1A trier sample is
25、 obtained by inserting a “trier” into thematerial. A trier is a halfround 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 other end. After insertion, the trier is turnedtwo or three times, and upon removal
26、 a core of the material being sampledis obtained.8. Hazards8.1 All reagents and chemicals should be handled with care.Before using any chemical, read and follow all safety precau-tions and instructions on the manufacturers label or MSDS(Material Safety Data Sheet).9. Preparation of Sample9.1 Powders
27、 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.9.2 LiquidsNo preparation o
28、f 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 2If pastes or liquids
29、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 upon for mixing and sampling.9.3 PastesStore preferably in glass. If crystals separate,m
30、elt on water bath (Note 1).METHODS OF CHEMICAL ANALYSIS10. Purity of Reagents10.1 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 American Chemical Society
31、, where suchspecifications are available.3Other 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.10.2 Unless otherwise indicated, references to water shall beunderstood to mean re
32、agent water conforming to SpecificationD 1193.MOISTURE BY THE DISTILLATION METHOD(Preferred Method)11. Apparatus11.1 The apparatus required shall consist of a glass flaskheated by suitable means and provided with a reflux condenserdischarging into a trap and connected to the flask. Theconnections be
33、tween the trap and the condenser and flask shallbe interchangeable ground joints. The trap serves to collect and3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Societ
34、y, 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.D1568052measure the condensed water and to return the solvent to theflask. A suitable assembly of the app
35、aratus 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 SourceEither 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
36、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. (6.35 mm) in insidediameter, shall be used. The end of the condenser to be insertedin the trap may be grou
37、nd 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. (7 mm) above thesurface of the liquid in the trap after the distillation conditionshave been established. Fig. 1 shows a conventional sealed-intype of condenser,
38、 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, percent Size of Trap, mL0to5,incl 5Over 5 to 17, incl 10Over 17 to 30, i
39、ncl 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-mLdivisions witheach 1 mL li
40、ne 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 in0.1-mL divisions and from 1 to 10 mL in 0.2-mL divisions.11.1.4.3 25-mL TrapSubdivided from 0 to 1 mL in0.1-mL divisions and from 1 to 25 mL in 0.2-mL division
41、s.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-mL flask, equipped wit
42、h the sizeof the trap specified in 11.1.4, an amount of sample accordingto the 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 406 4Over 30 to 50, incl 30 6 3Over 50 to 70, incl 30 6 3Over
43、 70 to 85, incl 25 6 2_AWeighed to the nearest 0.25 g.Add immediately about 100 mL of xylene or toluene. Placea small, thin sheet of long-fiber, chemical-resistant glass4woolon the surface of the toluene. The glass wool should bethoroughly dried in the oven and held in the desiccator beforeuse.13.2
44、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 an insulating cloth, so thatrefluxing will be under better control.13.3 Heat the oil bath
45、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 until nomore wate
46、r 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 wire. Movethe
47、 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 distillate to 20Cand
48、 read the volume of water.14. Calculations14.1 Calculate the percentage of moisture as follows:Moisture, % 5 V3 0.998!/W 3 100 (1)where:4Borosilicate glass has been found satisfactory for this purpose.FIG. 1 Assembly of Distillation ApparatusD1568053V = volume of water, mL at 20C, andW = weight of t
49、he sample, g.WATER BY THE KARL FISCHER TITRATIONMETHOD(Alternative Method)15. Application15.1 This method is intended to be used where the amountof moisture is low.16. Apparatus16.1 Automatic Buret (Machlett Type), 50-mL capacity,1000-mL reservoir of amber glass with a straight tip. The buretshould also be equipped with a drying tube containing asuitable drying agent such as anhydrous calcium sulfate(Drierite)5to protect the Karl Fischer reagent from moisture inthe air. Calcium chloride also is satisfactory. Magnesiumperchlorate (Deh
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