1、Designation: D501 03 (Reapproved 2016)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 U.S. Department of Defense.1. Scope1.1 These test methods cover proc
3、edures 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) 68Sodium Hydroxide (NaOH) 911Carbonate as Sodium Carbonate (Na2CO3) 12Carbon Dioxide (CO2) by the Evol
4、ution Method 1316Soda Ash:Sampling 17Matter Volatile at 150 to 155C 18 and 19Total Alkalinity as Sodium Carbonate (Na2CO3) 2022Sodium Bicarbonate (NaHCO3) 2325Sodium Bicarbonate (NaHCO3) by Potentiometric Titration 2628Matter Insoluble in Water 29 and 30Apparent Density 31 and 32Modified Soda (Sequi
5、carbonate Type):Sampling 33Total Alkalinity as Sodium Oxide (Na2O) 3436Sodium Bicarbonate (NaHCO3) and Sodium Carbonate (Na2CO3) 3739Matter Insoluble in Water 40Sodium Bicarbonate:Sampling 41Sodium Bicarbonate, Sodium Carbonate, and Free Moisture 4245Matter Insoluble in Water 46Sodium Metasilicate,
6、Sodium Sesquisilicate and Sodium Orthosil-icate:Sampling 47Total Alkalinity as Sodium Oxide (Na2O) 4850Total Silica as SiO25153Sodium Metasilicate (Na2SiO35H2O) 54Sodium Sesquisilicate (3Na2O2SiO211H2O) 55Matter Insoluble in Water 56 and 57Loss on Ignition of Sodium Sesquisilicate (3Na2O2SiO211H2O)
7、58 and 59Sodium Orthosilicate (Na4SiO4) 60Trisodium Phosphate:Sampling 61Trisodium Phosphate (Na3PO4) Content and PhosphorusPentoxide (P2O5) 6264Trisodium Phosphate Calculated as Na3PO412H2O, Na3PO4H2O, Na3PO4, and as P2O56568Total Alkalinity as Sodium Oxide (Na2O) 6971SectionsMatter Insoluble in Wa
8、ter 72 and 73Tetrasodium Pyrophosphate:Sampling 74Tetrasodium Pyrophosphate(Na4P2O7) 7579Matter Insoluble in Water 80 and 81Loss on Ignition 82 and 83Borax:Sampling 84Total Borate and Excess Alkalinity or Acidity 8587Matter Insoluble in Water 88 and 89Sodium Triphosphate:Sampling 90Tritratable Na2O
9、9194Total P2O5:Preferred Method 9597Alternative 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 129Temperature Ri
10、se 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 address all of th
11、esafety 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 and materials.
12、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 SubcommitteeD12.12 on Analysi
13、s and Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved July 1, 2016. Published August 2016. Originallyapproved in 1938. Last previous edition approved in 2009 as D501 03 (2009).DOI: 10.1520/D0501-03R16.2For referenced ASTM standards, visit the ASTM website
14、, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D
15、1193 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 inor-ganic alkali or alkaline salt having detergent properties,
16、 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 testmethods is defined in accordance with Terminology D459.4. Purit
17、y 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 Chemical Society,where such specifications are available.3Oth
18、er 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 beunderstood to mean reagent water conforming to SpecificationD1193.CAU
19、STIC 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 contentsof the drum in several places. The tube shall be dried byhe
20、ating 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 occur in thedrum.5.4 PrecautionsCaustic soda shall not be samp
21、led 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 transferred to athoroughly dried weighing bottle immediately after it
22、 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 1.0 Nacid solution.6.2 Methyl Red Indicator Solution.7. Procedure7.1 Weigh 10 g of the sample, dissolve in carbon dioxide(CO2)-free water, was
23、h 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 against 1.0 N acid, using methyl red as theindicator.8. Calculatio
24、n8.1 Calculate the total alkalinity as sodium oxide (Na2O) asfollows:Total alkalinity as Na2O,%5 A 35 33.1!/W (1)where:A = millilitres of acid required for titration of the Na2Ointhe sample, andW = grams of sample used.SODIUM HYDROXIDE (NaOH)9. Reagents9.1 Acid, Standard (1.0 N)Prepare and standardi
25、ze a 1.0 Nacid 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)Dissolve1 g of phenolphthalein in 50 mL of ethyl alcohol and then
26、 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 indicator.11. Calculation11.1 Calculate the percentage of sodium hydro
27、xide (NaOH)as follows:NaOH, % 5 B 35 34.0!/C (2)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
28、, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D501 03 (2016)2where:B = millilitres of acid necessary for titration of the NaOH inthe sample, andC = grams of sample used.CARBONATE AS SODIUM CARBONATE (Na2CO3)12. Calc
29、ulation12.1 Calculate the carbonate as sodium carbonate (Na2CO3)as follows:Na2CO3,%5 A 2 B! 35 35.3#/W (3)where:A = millilitres of acid required for titration of the Na2Ointhe sample,B = millilitres of acid required for titration of the NaOH inthe sample, andW = grams of sample used.NOTE 1When more
30、accurate results are desired, the evolution methodfor carbon dioxide as described in Sections 1316should be used.CARBON DIOXIDE (CO2) BY THE EVOLUTION METHOD13. Apparatus13.1 Apparatus AssemblyPlace a 150-mL wide-neck ex-traction flask on a gauze over a burner. Fit the flask with athree-hole rubber
31、stopper, one opening to carry a 25-cm refluxcondenser, the second to carry a thistle tube with a two-waystopcock for the introduction of acid into the flask, and thethird to carry a tube for the introduction of a continuous streamof carbon dioxide (CO2)-free air into the flask. Draw out theends of t
32、he 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 admitted tothe flask will be free from CO2.13.2 Preparation of Absorp
33、tion 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 sulfate (Drierite), or anhydrous calciumchloride,13.2.3 A weighed U-t
34、ube 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 aspirator.14. Reagents14.1 Methyl Orange Indicator Solution (1 g/L)Dissolve
35、0.1 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 carbon dioxide (CO2)-free airat a rate of approximately 20 to 30 mL/m
36、in 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 boiledwater, add 2 drops of methyl orange solution, and close theapparatu
37、s 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 as indicated bythe methyl orange. Always leave some acid in the thistle
38、 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 soda-asbestos andweigh using a tared U-tube as a counterpoise. The in
39、crease 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 32.409!/W# 3100 (4)where:C = grams of CO2, andW = grams of sample used.NOTE 2This test method for the determin
40、ation of Na2CO3as CO2isto be preferred when a procedure more accurate than that described inSection 12 is required.D501 03 (2016)3SODA ASH17. Sampling17.1 Soda ash shall be sampled by removing portions fromvarious parts of the container. Samples shall not be taken fromthose portions of the soda ash
41、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.MATTER VOLATILE AT 150 TO 155C18. Procedure18.1 Place approximately2gofthes
42、ample 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 reweigh.19. Calculation19.1 Calculate the percentage of volatile matter as
43、 follows:Volatile matter, % 5 L/W! 3100 (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 orange in water and dilute to 100 mL.20.2 Hydrochloric Acid, Standard (0
44、.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, from moisture in theair during weighing. Dissolve the sample in about 5
45、0 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 boiling, and boil for 1minto remove most of the CO2. Cool and finish the titra
46、tion 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 35.3!/W (6)where:A = millilitres of HCl required for titration of the sample,N = normality of the HCl, andW = grams of sample
47、 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 Solution (1.0 N)Prepare and standardize a 1.0 N sodium hydroxide (NaOH)solution
48、.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 AgNO3solution on a spot plategives a dark color instantly.25. Calculation25.1 Calcul
49、ate 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,%30.6309! (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 TITRATION26. Reagents26.1 Barium Chloride, Ne
