1、Designation: D501 03 (Reapproved 2009)Standard Test Methods ofSampling and Chemical Analysis of Alkaline Detergents1This standard is issued under the fixed designation D501; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods cover procedure
3、s for the samplingand chemical analysis of inorganic alkaline detergents.1.2 The procedures appear in the following order:SectionsCaustic Soda:Sampling 5Total Alkalinity as Sodium Oxide (Na2O) 6-8Sodium Hydroxide (NaOH) 9-11Carbonate as Sodium Carbonate (Na2CO3) 12Carbon Dioxide (CO2) by the Evoluti
4、on Method 13-16Soda Ash:Sampling 17Matter Volatile at 150 to 155C 18 and 19Total Alkalinity as Sodium Carbonate (Na2CO3) 20-22Sodium Bicarbonate (NaHCO3) 23-25Sodium Bicarbonate (NaHCO3) by Potentiometric Titration 26-28Matter Insoluble in Water 29 and 30Apparent Density 31 and 32Modified Soda (Sequ
5、icarbonate Type):Sampling 33Total Alkalinity as Sodium Oxide (Na2O) 34-36Sodium Bicarbonate (NaHCO3) and Sodium Carbonate (Na2CO3) 37-39Matter Insoluble in Water 40Sodium Bicarbonate:Sampling 41Sodium Bicarbonate, Sodium Carbonate, and Free Moisture 42-45Matter Insoluble in Water 46Sodium Metasilica
6、te, Sodium Sesquisilicate and Sodium Orthosil-icate:Sampling 47Total Alkalinity as Sodium Oxide (Na2O) 48-50Total Silica as SiO251-53Sodium Metasilicate (Na2SiO35H2O) 54Sodium Sesquisilicate (3Na2O2SiO211H2O) 55Matter Insoluble in Water 56 and 57Loss on Ignition of Sodium Sesquisilicate (3Na2O2SiO21
7、1H2O) 58 and 59Sodium Orthosilicate (Na4SiO4) 60Trisodium Phosphate:Sampling 61Trisodium Phosphate (Na3PO4) Content and PhosphorusPentoxide (P2O5) 62-64Trisodium Phosphate Calculated as Na3PO412H2O, Na3PO4H2O, Na3PO4, and as P2O565-68Total Alkalinity as Sodium Oxide (Na2O) 69-71Matter Insoluble in W
8、ater 72 and 73SectionsTetrasodium Pyrophosphate:Sampling 74Tetrasodium Pyrophosphate(Na4P2O7) 75-79Matter Insoluble in Water 80 and 81Loss on Ignition 82 and 83Borax:Sampling 84Total Borate and Excess Alkalinity or Acidity 85-87Matter Insoluble in Water 88 and 89Sodium Triphosphate:Sampling 90Tritra
9、table Na2O 91-94Total P2O5:Preferred Method 95-97Alternative Method 98-101pH Titration 102-107Quantitative Separation and Measurement of Various Phosphates:Reverse-Flow Ion-Exchange Chromatography (PreferredMethod) 108-119Paper Chromatographic Method 120-127pH of 1 percent Solution 128Turbidity 129T
10、emperature Rise 130-134Sulfate 135-137Ignition Loss 140 and141Matter Insoluble in Water 142-144Particle Size 145Orthophosphate 146-1511.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to addr
11、ess 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 determine the applica-bility of regulatory limitations prior to use. Material SafetyData Sheets are available for reagents an
12、d materials. Reviewthem for hazards prior to usage.2. Referenced Documents2.1 ASTM Standards:2D459 Terminology Relating to Soaps and Other Detergents1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD12.
13、12 on Analysis and Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved Oct. 1, 2009. Published December 2009. Originallyapproved in 1938. Discontinued August 2001 and reinstated as D501 03. Lastprevious edition approved in 2003 as D501 03. DOI: 10.1520/D0501-
14、03R09.2For referenced ASTM standards, visit the 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, P
15、O Box C700, West Conshohocken, PA 19428-2959, United States.D1193 Specification for Reagent WaterE1 Specification for ASTM Liquid-in-Glass ThermometersE70 Test Method for pH of Aqueous Solutions With theGlass Electrode3. Terminology3.1 Definitions:3.1.1 inorganic alkaline detergenta water soluble in
16、or-ganic alkali or alkaline salt having detergent properties, butcontaining no soap or synthetics.3.1.2 For definitions of other terms used in these testmethods, refer to Terminology D459.3.2 Definitions of Terms Specific to This Standard:3.2.1 The term “inorganic alkaline detergent” in these testme
17、thods is defined in accordance with Terminology D459.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American
18、Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Unless otherwise indicated, references to water shall beundersto
19、od to mean reagent water conforming to SpecificationD1193.CAUSTIC SODA5. Sampling5.1 Flake Caustic SodaFlake caustic soda shall besampled by removing portions from various parts of the drum.5.2 Powdered Caustic SodaPowdered caustic soda shallbe sampled by inserting a sampling tube through the conten
20、tsof the drum in several places. The tube shall be dried byheating just before use.5.3 Fused Caustic SodaFused caustic soda shall besampled by taking chipped samples from the center and bottomof the drum and then mixing the gross sample in the approxi-mate proportions in which the tops and bottoms o
21、ccur in thedrum.5.4 PrecautionsCaustic soda shall not be sampled in amoist atmosphere. In the case of fused caustic soda the portiontaken for analysis shall have the surface layer of carbonatescraped off immediately before transferring to the weighingbottle. In all cases the sample shall be transfer
22、red to athoroughly dried weighing bottle immediately after it is taken;the bottle shall be tightly stoppered at once.TOTAL ALKALINITY AS SODIUM OXIDE (Na2O)6. Reagents6.1 Acid, Standard (1.0 N)Prepare and standardize a 1.0N acid solution.6.2 Methyl Red Indicator Solution.7. Procedure7.1 Weigh 10 g o
23、f the sample, dissolve in carbon dioxide(CO2)-free water, wash into a 500-mL volumetric flask, anddilute to volume with CO2-free water. Protect the solution fromthe air as much as possible. Pipet a one-fifth aliquot into a400-mL beaker and determine sodium oxide (Na2O) by titrat-ing the sample again
24、st 1.0 N acid, using methyl red as theindicator.8. Calculation8.1 Calculate the total alkalinity as sodium oxide (Na2O) asfollows:Total alkalinity as Na2O,%5 A 3 5 3 3.1!/W (1)where:A = millilitres of acid required for titration of the Na2Ointhe sample, andW = grams of sample used.SODIUM HYDROXIDE (
25、NaOH)9. Reagents9.1 Acid, Standard (1.0 N)Prepare and standardize a 1.0N acid solution.9.2 Barium Chloride, Neutral Solution (100 g/L)Dissolve100 g of barium chloride (BaCl22H2O) in water and dilute to1 L. Make the solution neutral to phenolphthalein.9.3 Phenolphthalein Indicator Solution (10 g/L)Di
26、ssolve1 g of phenolphthalein in 50 mL of ethyl alcohol and then mixwith 50 mL of water.10. Procedure10.1 Determine the NaOH on a second one-fifth aliquotpipetted into a 250-mL Erlenmeyer flask. Add about 25 mL ofBaCl2solution and titrate the sample with 1.0 N acid usingphenolphthalein as the indicat
27、or.11. Calculation11.1 Calculate the percentage of sodium hydroxide (NaOH)as follows:NaOH, % 5 B 3 5 3 4.0!/C (2)where:3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemica
28、l 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), Rockville,MD.D501 03 (2009)2B = millilitres of acid necessary for titration of the NaOH inthe sample, andC = g
29、rams of sample used.CARBONATE AS SODIUM CARBONATE (Na2CO3)12. Calculation12.1 Calculate the carbonate as sodium carbonate (Na2CO3)as follows:Na2CO3,%5 A 2 B! 3 5 3 5.3/W (3)where:A = millilitres of acid required for titration of the Na2Ointhe sample,B = millilitres of acid required for titration of
30、the NaOH inthe sample, andW = grams of sample used.NOTE 1When more accurate results are desired, the evolution methodfor carbon dioxide as described in Sections 13-16 should be used.CARBON DIOXIDE (CO2) BY THE EVOLUTION METHOD13. Apparatus13.1 Apparatus AssemblyPlace a 150-mL wide-neck ex-traction f
31、lask on a gauze over a burner. Fit the flask with athree-hole rubber stopper, one opening to carry a 25-cm refluxcondenser, the second to carry a thistle tube with a twowaystopcock for the introduction of acid into the flask, and thethird to carry a tube for the introduction of a continuous streamof
32、 carbon dioxide (CO2)-free air into the flask. Draw out theends of the thistle and air supply tubes to a small point, andplace them in the stopper so that the points are very close to thebottom of the flask. Attach to the air supply tube, a U-tubecontaining soda-asbestos (Ascarite) so that the air a
33、dmitted tothe flask will be free from CO2.13.2 Preparation of Absorption TrainAttach to the top ofthe reflux condenser a train consisting of the following:13.2.1 A U-tube containing granulated zinc for the removalof acid gases,13.2.2 A drying tube containing magnesium perchlorate,anhydrous calcium s
34、ulfate (Drierite), or anhydrous calciumchloride,13.2.3 A weighed U-tube containing soda-asbestos in thefirst half and the same drying agent in the second half as usedin 13.2.2, and13.2.4 A protective U-tube containing any of the abovementioned drying agents.13.2.5 Attach the final tube to an aspirat
35、or.14. Reagents14.1 Methyl Orange Indicator Solution (1 g/L)Dissolve0.1 g of methyl orange in water and dilute to 100 mL.14.2 Sulfuric Acid (2 + 9)Mix 2 volumes of concentratedsulfuric acid (H2SO4, sp gr 1.84) carefully with stirring into 9volumes of water.15. Procedure15.1 Aspirate with a stream of
36、 carbon dioxide (CO2)-free airat a rate of approximately 20 to 30 mL/min until the train isfree from CO2as determined by no further change in weightgreater than 0.3 mg in the U-tube.15.2 Weigh 10 g of the sample to the nearest 0.01 g directlyinto the extraction flask, cover with 50 mL of freshly boi
37、ledwater, add 2 drops of methyl orange solution, and close theapparatus with the train in place. Start the aspiration at a rate of20 to 30 mL/min, and slowly add through the thistle tubesufficient H2SO4(2 + 9) to neutralize the NaOH and a sufficientexcess to ensure the final acidity of the mixture a
38、s indicated bythe methyl orange. Always leave some acid in the thistle tubeas an air seal. Heat gently and continue until the contents of theflask have boiled for 5 min; remove the source of heat, andcontinue aspirating until the flask has cooled, or for about 30min.15.3 Remove the U-tube containing
39、 soda-asbestos andweigh using a tared U-tube as a counterpoise. The increase inweight represents CO2.16. Calculation16.1 From the increase in weight of the tube calculate thepercentage of carbon dioxide (CO2) as sodium carbonate(Na2CO3) as follows:Na2CO3,%5 C 3 2.409!/W 3 100 (4)where:C = grams of C
40、O2, andW = grams of sample used.NOTE 2This test method for the determination of Na2CO3as CO2isto be preferred when a procedure more accurate than that described inSection 12 is required.D501 03 (2009)3SODA ASH17. Sampling17.1 Soda ash shall be sampled by removing portions fromvarious parts of the co
41、ntainer. Samples shall not be taken fromthose portions of the soda ash where caking is noticeable dueto the absorption of moisture and carbon dioxide through thecontainer. If the soda ash is caked, the sample shall be obtainedby thoroughly mixing and quartering the entire contents of thepackage.MATT
42、ER VOLATILE AT 150 TO 155C18. Procedure18.1 Place approximately2gofthesample in a taredweighing bottle and weigh to the nearest 0.1 mg. Remove thestopper and dry in an oven at 150 to 155C for 1 h. Replace thestopper and allow to cool to room temperature in a desiccatorcontaining no desiccant and rew
43、eigh.19. Calculation19.1 Calculate the percentage of volatile matter as follows:Volatile matter, % 5 L/W! 3 100 (5)where:L = grams loss in weight, andW = grams of sample used.TOTAL ALKALINITY AS SODIUM CARBONATE(Na2CO3)20. Reagents20.1 Methyl Orange Indicator Solution (1 g/L)Dissolve0.1 g of methyl
44、orange in water and dilute to 100 mL.20.2 Hydrochloric Acid, Standard (0.5 N)Prepare andstandardize 0.5 N hydrochloric acid (HCl).21. Procedure21.1 Transfer approximately 1.2 g of sample into a taredweighing bottle. Weigh to the nearest 0.1 mg, protecting thesample at all times, as much as possible,
45、 from moisture in theair during weighing. Dissolve the sample in about 50 mL ofwater in a 400-mL beaker and add 2 drops of methyl orangeindicator solution. Run in, while stirring, 0.5 N HCl until 1drop establishes the first appearance of a pink color in thesolution. Remove the beaker, heat to boilin
46、g, and boil for 1minto remove most of the CO2. Cool and finish the titration to thefirst appearance of a pink color in the solution.22. Calculation22.1 Calculate the total alkalinity as sodium carbonate(Na2CO3) as follows:Total alkalinity, % 5 AN 3 5.3!/W (6)where:A = millilitres of HCl required for
47、 titration of the sample,N = normality of the HCl, andW = grams of sample used.SODIUM BICARBONATE (NaHCO3)23. Reagents23.1 Silver Nitrate Solution (100 g/L)Dissolve 100 g ofsilver nitrate (AgNO3) in water and dilute to 1 L. Prepare thissolution fresh before use.23.2 Sodium Hydroxide, Standard Soluti
48、on (1.0 N)Prepare and standardize a 1.0 N sodium hydroxide (NaOH)solution.24. Procedure24.1 Weigh 8.4 g of the sample to the nearest 0.05 g andtransfer to a 250-mL beaker. Dissolve in 100 mL of water, andtitrate with 1.0 N NaOH solution until a drop of the testsolution added to a drop of AgNO3soluti
49、on on a spot plategives a dark color instantly.25. Calculation25.1 Calculate the percentage of sodium bicarbonate(NaHCO3) as follows:NaHCO3,%5 mL of 1.0 N NaOH solution (7)Calculate the percentage of sodium carbonate (Na2CO3)asfollows:Na2CO3,%5 A 2 NaHCO3,%3 0.6309! (8)where:A = total alkalinity as Na2CO3, in percent.NOTE 3For referee purposes, or when more accurate results arerequired than are yielded by the procedure described in Section 25, themethod described in Section 28 shall be used.SODIUM BICARBONATE (NaHCO3)BYPOTENTIOMETRIC TI
