1、Designation: D 501 03Standard Test Methods ofSampling and Chemical Analysis of Alkaline Detergents1This standard is issued under the fixed designation D 501; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 procedures for the sampl
3、ingand 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 Evolution Method 13-16S
4、oda 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 (Sequicarbonate Type)
5、: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 Metasilicate, Sodium Sesqu
6、isilicate 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 (3Na2O2SiO211H2O) 58 and 59S
7、odium 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 Water 72 and 73Sec
8、tionsTetrasodium 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 90Tritratable Na2O 91-94T
9、otal 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 129Temperature Rise 1
10、30-134Sulfate 135-137Ignition Loss 140 and141Matter Insoluble in Water 142-144Particle Size 145Orthophosphate 146-1511.3 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-priat
11、e 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:2D 459 Terminology Relating to Soaps and Other D
12、etergentsD 1193 Specification for Reagent WaterE 1 Specification for ASTM ThermometersE 70 Test Method for pH of Aqueous Solutions with theGlass Electrode1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of Subcommitte
13、eD12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved Oct. 1, 2003. Published December 2003. Originallyapproved in 1938. Discontinued August 2001 and reinstated as D 501 03. Lastprevious edition approved in 1989 as D 501 89 (1998).2For r
14、eferenced 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, PO Box C700,
15、West Conshohocken, PA 19428-2959, United States.3. Terminology3.1 Definitions:3.1.1 inorganic alkaline detergenta water soluble inor-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
16、 Terminology D 459.3.2 Definitions of Terms Specific to This Standard:3.2.1 The term “inorganic alkaline detergent” in these testmethods is defined in accordance with Terminology D 459.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indi
17、cated, 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.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to pe
18、rmit its use without lessening theaccuracy of the determination.4.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD 1193.CAUSTIC SODA5. Sampling5.1 Flake Caustic SodaFlake caustic soda shall besampled by removing portions from var
19、ious 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 byheating just before use.5.3 Fused Caustic SodaFused caustic soda shall besampled by taking chipped samples f
20、rom 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 sampled in amoist atmosphere. In the case of fused caustic soda the portiontaken for analysis shall have the s
21、urface 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 is taken;the bottle shall be tightly stoppered at once.TOTAL ALKALINITY AS SODIUM OXIDE (Na2O)6. Reagents
22、6.1 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 of 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 ai
23、r 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. Calculation8.1 Calculate the total alkalinity as sodium oxide (Na2O) asfollows:Total alkalinity as Na2O,%5 A 3 5 3 3
24、.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 standardize a 1.0N acid solution.9.2 Barium Chloride, Neutral Solution (100 g/L)Dissolve100 g of barium chloride
25、(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 mixwith 50 mL of water.10. Procedure10.1 Determine the NaOH on a second one-fifth aliquotpipetted into
26、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 hydroxide (NaOH)as follows:NaOH, % 5 B 3 5 3 4.0!/C (2)where:B = millilitres of acid necessary for titration
27、of the NaOH inthe sample, andC = grams of sample used.CARBONATE AS SODIUM CARBONATE (Na2CO3)12. Calculation12.1 Calculate the carbonate as sodium carbonate (Na2CO3)as follows:3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on th
28、e testing of reagents notlisted by the American Chemical 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.D501032Na2CO3,%5 A 2 B! 3 5 3 5.3#/W (3)wh
29、ere: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 accurate results are desired, the evolution methodfor carbon dioxide as described in Sections 13-16 should b
30、e 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 stopper, one opening to carry a 25-cm refluxcondenser, the second to carry a thistle tube with a twowaysto
31、pcock 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 the thistle and air supply tubes to a small point, andplace them in the stopper so that the points are very
32、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 Absorption TrainAttach to the top ofthe reflux condenser a train consisting of the following:13.2.1 A U-tube cont
33、aining 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-tube containing soda-asbestos in thefirst half and the same drying agent in the second half as usedin 13.2.2
34、, 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)Dissolve0.1 g of methyl orange in water and dilute to 100 mL.14.2 Sulfuric Acid (2 + 9)Mix 2 volumes of concentrate
35、dsulfuric 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/min until the train isfree from CO2as determined by no further change in weightgreater than 0.3 mg in the
36、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 theapparatus with the train in place. Start the aspiration at a rate of20 to 30 mL/min, and slowly add through the t
37、histle 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 tubeas an air seal. Heat gently and continue until the contents of theflask have boiled for 5 min; remov
38、e 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 increase inweight represents CO2.16. Calculation16.1 From the increase in weight of the tube calculate thep
39、ercentage of carbon dioxide (CO2) as sodium carbonate(Na2CO3) as follows:Na2CO3,%5 C 3 2.409!/W# 3 100 (4)where:C = grams of CO2, 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
40、is required.D501033SODA 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 where caking is noticeable dueto the absorption of moisture and carbon dioxide through thecontainer. If the sod
41、a 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 approximately2gofthesample in a taredweighing bottle and weigh to the nearest 0.1 mg. Remove thestopper and dry in an oven at 150 to
42、 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 follows:Volatile matter, % 5 L/W! 3 100 (5)where:L = grams loss in weight, andW = grams of sample used.TOTAL A
43、LKALINITY 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 (0.5 N)Prepare andstandardize 0.5 N hydrochloric acid (HCl).21. Procedure21.1 Transfer approximately 1.2 g of sa
44、mple 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 50 mL ofwater in a 400-mL beaker and add 2 drops of methyl orangeindicator solution. Run in, while stirring, 0.
45、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 titration to thefirst appearance of a pink color in the solution.22. Calculation22.1 Calculate the total alkalinity
46、 as sodium carbonate(Na2CO3) as follows:Total alkalinity, % 5 AN 3 5.3!/W (6)where:A = millilitres of HCl required for 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 ni
47、trate (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.24. Procedure24.1 Weigh 8.4 g of the sample to the nearest 0.05 g andtransfer to a 250-mL beaker. Dissolve i
48、n 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 Calculate the percentage of sodium bicarbonate(NaHCO3) as follows:NaHCO3,%5 mL of 1.0 N NaOH solution (7)Calculate
49、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 TITRATION26. Reagents26.1 Barium Chloride, Neutral Solution (122 g/L)Dissolve 122 g of barium chloride (BaCl22H2O) in water anddilute to 1 L. Make the solution neutral to phenolphthalein.
