1、Designation: D1568 05 (Reapproved 2014)Standard Test Methods forSampling and Chemical Analysis of AlkylbenzeneSulfonates1This standard is issued under the fixed designation D1568; 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 () 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 alkylbenzene
3、sulfonates.1.2 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 1114Karl Fischer Method 1520Total Matter Insol
4、uble in Alcohol 2123Neutral Oil 2427Chlorides Calculated as Sodium Chloride (NaCl) 2831pH 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 pract
5、ices and determine the applica-bility of regulatory limitations prior to use. For a specifichazards statement, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D1172 Guide for pH of Aqueous Solutions of Soaps andDetergentsD1193 Specification for Reagent WaterSAMPLING3. General Requirements3.
6、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 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, pro
7、vided 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 carto
8、ns 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
9、 wrapped 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 near
10、ly 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
11、 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 (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 t
12、han 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 sothat the amount drawn shall not exceed 20 lb (9.1 kg). Theinspe
13、ctor shall rapidly mix the gross sample and place it in an1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergentsand is the direct responsibility of D12.12 on Analysisand Specifications of Soaps, Synthetics, Detergents and their Components.Current edition ap
14、proved Jan. 1, 2014. Published February 2014. Originallyapproved in 1958. Last previous edition approved in 2005 as D1568 05. DOI:10.1520/D1568-05R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStand
15、ards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1airtight container which shall be filled, sealed, marked, accu-rately weighed, with its weight an
16、d 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 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
17、 less than 10 gal(37.9 L). In the case of smaller containers, a sample 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
18、 pt (236.6 mL) each taken atrandom from separate containers. Before 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 an
19、d 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) orLessOne can or carton shall be taken at random from not lessthan 1 % of the sellers shipping containers, provided eachpackage conta
20、ins 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 taken atrandom from
21、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 exceed 20 lb (9.1kg). The samples shall be wrapped, sealed, marked, and sent tothe laborato
22、ry for test.7.2 Pastes Packed in BulkA“trier” sample (Note 1)ofnotless 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 th
23、an 0.5 lb (227g) shall be taken at random from each lot of containers 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 s
24、ample drawn as above willamount to more than 10 lb (4.5 kg), the percentage 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
25、, marked, and sent to the laboratoryfor test.NOTE 1A trier sample is 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. Afte
26、r insertion, the trier is turnedtwo or three times, and upon removal 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
27、MSDS(Material Safety Data Sheet).9. Preparation of Sample9.1 Powders 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
28、in an airtight container in a cool place.9.2 LiquidsNo preparation of the sample of liquid, otherthan a thorough mixing, is necessary unless it is receivedduring very cold weather, when it should be allowed to standat least 1 h after it has warmed to room temperature (20 to30C) before it is tested,
29、particularly for its lathering qualities.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 upon for mixing and
30、sampling.9.3 PastesStore preferably in glass. If crystals separate,melt 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
31、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 reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.10.2 Unless ot
32、herwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD1193.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 condenserdi
33、scharging into a trap and connected to the flask. Theconnections between the trap and the condenser and flask shallbe interchangeable 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
34、 Fig.1.3Reagent 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 Pha
35、rmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D1568 05 (2014)211.1.1 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 provid
36、ed 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, with an inner tube38 to12 in. (9.5 to 12.7 mm) inoutside diameter, and not less than14 in. (6.35 mm) in insidediameter, sh
37、all 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 condenser shall be about14 in. (7 mm) above thesurface of the liquid in the trap after the distillation conditionshav
38、e 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 greatest accuracy several trap sizes areallowable, depending upon the percentage of moisture ex-pected:Moisture Expecte
39、d, percent 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, constructed essentiallyas shown in Fig. 1, and graduated to contain one of thefollowing specified volumes at 20C shall
40、 be used:11.1.4.1 5-mL TrapSubdivided into 0.1-mL divisions 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 mLin 0.1-mLdivisions and from 1 to 10 mL in 0.2-mL divisions.11.1.4.3 25-mL TrapSubdivid
41、ed from 0 to 1 mLin 0.1-mLdivisions 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 xylene (or toluene) withwater by shaking with a small quantity of water and distill. Usethe distillate for the d
42、etermination.13. Procedure13.1 Transfer to the 1000-mL flask, equipped with 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, gA0to5,incl 505Over 5 to 17, incl 50 5Over 17 to 30,
43、incl 40 4Over 30 to 50, incl 30 3Over 50 to 70, incl 30 3Over 70 to 85, incl 25 2AWeighed 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 dr
44、ied 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 through the side tube. Wrap the flaskand tube leading to the receiver with an insulating cloth, so thatrefl
45、uxing 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 should be approximately100 drops/min. When the greater part of the water has distilledover, increas
46、e 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 the walls of the condenser. Thewater in the receiver may be made to separate from the xylene(or t
47、oluene) 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 off the heat at the end of this period.13.4 Wash down condenser with 1 mL of absolute ethanol(CH3
48、CH2OH). Adjust the temperature of the distillate to 20Cand read the volume of water.14. Calculations14.1 Calculate the percentage of moisture as follows:Moisture, % 5 V 30.998!/W# 3100 (1)where:V = volume of water, mL at 20C, and4Borosilicate glass has been found satisfactory for this purpose.FIG. 1
49、 Assembly of Distillation ApparatusD1568 05 (2014)3W = weight of the 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
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