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Designation: D 1439 – 97AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr., West Conshohocken, PA 19428Reprinted from the Annual Book of ASTM Standards. Copyright ASTMStandard Test Methods forSodium Carboxymethylcellulose1This standard is issued under the fixed designation D 1439; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.3.2 Unless otherwise indicated, references to water shall beunderstood to mean distilled water.1. Scope1.1 These test methods cover the testing of sodiumcarboxymethylcellulose.1.2 The test procedures appear in the following order:SectionsMoistureDegree of Etherification:Test Method A—Acid WashTest Method B—Nonaqueous TitrationViscosityPuritySodium GlycolateSodium ChlorideDensity4-9MOISTURE10-1710, 11, 18-2324-3031-3839-4748-5556-624. Scope4.1 This test method covers the determination of the volatilecontent of sodium carboxymethylcellulose.4.2 The results of this test are used for calculating the totalsolids in the sample; and, by common usage, all materialsvolatile at this test temperature are designated as moisture.1.3 The values stated in inch-pound units are to be regardedas the standard. The values given in parentheses are forinformation only.1.4 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 establishappropriate safety and health practices and determine theapplicability of regulatory limitations prior to use. For specifichazard statements, see Note 1 and Note 2.5. Significance and Use5.1 Moisture analysis (along with purity) is used to calculatethe amount of active polymer in the material and must beconsidered when determining the amount of sodiumcarboxymethylcellulose to use in various formulations.6. Apparatus6.1 Oven—Gravity convection oven, capable ofmaintaining a temperature of 105 6 3 C.6.2 Weighing Bottles, low-form, 50-mm inside diameter by30-mm height, or equivalent.6.3 Analytical Balance.2. Referenced Documents2.1 ASTM Standards:D 1347 Test Methods for Methylcellulose2E 1 Specification for ASTM Thermometers33. Purity of Reagents3.1 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 Society4, where suchspecifications are available. Other grades may be used,7. Procedure7.1 Weigh 3 to 5 g of the sample to the nearest 0.001 g in atared and covered weighing bottle.7.2 Place the bottle in an oven at 105 C for 2 h with thecover removed. Cool the bottle in a desiccator, replace thecover, and weigh.7.3 Replace the sample in the oven for 30 min, cool, andreweigh.7.4 Continue this procedure to a mass loss of not more than5 mg for 30 min drying time.1These test methods are under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings, Materials, and Applications and are the direct responsibilityof Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved Nov. 10, 1997. Published July 1998. Originallypublished as D 1439 – 56 T. Last previous edition D 1439 – 94.2Annual Book of ASTM Standards, Vol 06.03.3Annual Book of ASTM Standards, Vol 14.03.4Reagent 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 Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.8. Calculation8.1 Calculate the percent moisture, M, as follows:M 5 A/B! 3 100where:A 5 mass loss on heating, g, and1(1)

D 1439B 5 sample used, g.14.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid(HNO3).14.7 Sodium Hydroxide, Standard Solution (0.3 to 0.5 N)—Prepare and standardize a 0.3 to 0.5 N solution of sodiumhydroxide (NaOH).14.8 Sulfuric Acid (9 2)—Carefully mix 9 volumes H2SO4with 2 volumes of water.9. Precision and Bias9.1 Precision—Statistical analysis of interlaboratoryreproducibility test results on samples containing 2 to 10 %moisture indicates a precision of 60.2 % absolute at the 95 %confidence level.9.2 Bias—No justifiable statement can be made on the biasof the procedure for measuring moisture because no suitablereference material exists.15. Procedure15.1 Weigh approximately 4 g of the sample into a 250-mLbeaker and add 75 mL of ethyl alcohol (95 %). Stir the mixturewith an air–driven stirrer until a good slurry is obtained. Add 5mL of HNO3, while agitating, and continue agitation for 1 to 2min. Heat the slurry and boil for 5 min. (Warning—See Note1.) Remove the heat and continue agitation for 10 to 15 min.DEGREE OF ETHERIFICATION10. Scope10.1 These test methods cover the determination of ylcellulose.10.2 Two test methods are included as follows:10.2.1 Test Method A (Acid Wash), for crude grades ofsodium carboxymethylcellulose with degrees of etherificationup to 0.85. Above 0.85 degree of etherification, slightly lowresults may be obtained.10.2.2 Test Method B (Nonaqueous Titration), for purifiedgrades of sodium carboxymethylcellulose of all degrees ofetherification. It is not applicable to the crude grades.Test Method A—Acid WashNOTE 1—Warning: Exercise care to avoid fire.15.2 Decant the supernatant liquid through the filter andtransfer the precipitate to the filter with 50 to 100 mL of ethylalcohol (95 %). Wash the precipitate with ethyl alcohol (80 %)that has been heated to 60 C, until all of the acid has beenremoved.15.3 Test for the removal of acid and salts (ash) by mixinga drop of the acid carboxymethylcellulose slurry from the filterwith a drop of diphenylamine reagent on a white spot plate. Ablue color indicates the presence of nitrate and the necessity forfurther washing. If the first drop of reagent does not produce ablue color, further drops should be added until an excess ofreagent is known to be present, noting the color after each drop.Four to six washings will usually suffice to give a negative testfor nitrate.15.4 Finally, wash the precipitate with a small amount ofanhydrous methanol and draw air through it until the alcohol iscompletely removed. Transfer the precipitate to a glass oraluminum weighing dish provided with a cover. Heat theuncovered dish on a steam bath until the odor of alcohol can nolonger be detected (in order to avoid fires due to methanolfumes in the oven), then dry the dish and contents, uncoveredfor 3 h at 105 C. Place the cover on the dish and cool to roomtemperature in a desiccator.15.5 The sulfate ash content of the sample at this pointshould be less than 0.5 % when determined on 0.5 g of thesample by the procedure given in the Ash as Sulfate section ofTest Methods D 1347. If the ash content is greater than 0.5 %,rewash the sample with ethyl alcohol (80 %). If necessary,repeat the procedure described in 13.1-13.3 to Weigh, to the nearest 0.01 g, about 1 to 1.5 g of thedried acid carboxymethylcellulose (depending on thenormality of the acid and base to be used) into a 500-mLErlenmeyer flask. Add 100 mL of water and 25.00 mL of 0.3 to0.5 N NaOH solution, while stirring. Heat the solution toboiling, and boil for 15 to 30 min.15.7 Titrate the excess NaOH, while the solution is hot, withthe 0.3 to 0.5 N HCl to a phenolphthalein end point.11. Summary of Test Method11.1 The water-soluble sodium carboxymethylcellulose isconverted to the insoluble acid form, purified by washing,dried, and then a weighed sample is reconverted to the sodiumsalt with a measured excess of sodium hydroxide.12. Significance and Use12.1 These test methods determine the amount ofsubstituent groups added to the cellulose backbone. The levelcan greatly affect solution properties, rheology, viscosity,hygroscopicity, salt tolerance, and many other properties of thepolymer.13. Apparatus13.1 Stirrer, air-driven.13.2 Buchner Funnel, 75-mm, fitted with a 70-mm finetexture, heavy-duty filter paper. A60-mm medium-porosity,fritted glass funnel may also be used.13.3 Drying Oven, maintained at 105 C.14. Reagents14.1 Diphenylamine Reagent—Dissolve 0.5 g ofdiphenylamine in 120 mL of sulfuric acid (H2SO4, 9 2). Thereagent should be essentially water-white. It will give a deepblue coloration with traces of nitrate or other oxidizing agents.14.2 Ethyl Alcohol (95 volume %)—Denatured ethylalcohol conforming to either Formula 2B, 3A, or 30 of the U.S. Bureau of Internal Revenue.14.3 Ethyl Alcohol (80 % by volume)—Dilute 840 mL ofFormula 2B, 3A, or 30 denatured alcohol to 1 L with water.14.4 Hydrochloric Acid, Standard (HCl, 0.3 to 0.5 N).14.5 Methanol, anhydrous.16. Calculation16.1 Calculate the degree of etherification, G, as follows:2A 5 BC – DE!/F(2)G 5 0.162A/ 1– 0.0584A!(3)

D 1439acid, shake to dissolve, and then make up to volume and mixthoroughly. Pipet 10 mL into a 100-mL beaker and add 50 mLof acetic acid. Place on a magnetic stirrer and insert theelectrodes of the pH meter. Add nearly the required amount ofHClO4 from a buret, then decrease the increments to 0.05 mLas the end point is approached. Record the millilitres of titrantversus millivolts, and continue the titration a few millilitresbeyond the end point. Plot the titration curve and read thevolume of titrant at the inflection point. Calculate thenormality, N, as follows:where:A5 milliequivalents of acid consumed per gram ofsample,B5 NaOH solution added, mL,C5 normality of the NaOH solution,D5 HCl required for titration of the excess NaOH, mL,E5 normality of the HCl,F5 acid carboxymethylcellulose used, g,162 5 gram molecular mass of the anhydroglucose unit ofcellulose, and58 5 net increase in molecular mass of anhydroglucoseunit for each carboxymethyl group substituted.N 5 A 3 10 3 1000!/ B 3 204.22 3 250!(4)where:A5 potassium acid phthalate used, g,B5 HClO4 added, mL,204.22 5 gram molecular mass of potassium acidphthalate,105 potassium acid phthalate solution added, mL,and2505 glacial acetic acid used to dissolve potassiumacid phthalate, mL.20.5 Potassium Acid Phthalate, primary standard, NationalInstitute of Standards and Technology Standard Sample No.84.17. Precision and Bias17.1 Precision—Statistical analysis of intralaboratory(repeatability) test results indicates a precision of 60.04 D.E.units at the 95 % confidence level.17.2 Bias—No justifiable statement can be made on the biasof the procedure for measuring degree of etherification becauseno suitable reference material exists.Test Method B—Nonaqueous Titration18. Summary of Test Methods18.1 This measurement is based upon a nonaqueous acidbase titration. The sample is refluxed with glacial acetic acid,and the resulting sodium acetate is titrated with a standardsolution of perchloric acid in dioxane, to a potentiometric endpoint. Impurities containing alkaline sodium will also betitrated under these conditions. Sodium chloride does notinterfere.21. Procedure21.1 Weigh 0.2 g of the sample, to the nearest 0.0001 g, intoa 250-mL Erlenmeyer flask with ground-glass joint. Add 75mL of acetic acid, connect to a water-cooled condenser, andreflux gently on a hot plate for 2 h.21.2 Cool, and transfer the solution to a 250-mL beaker withthe aid of 50 mL of acetic acid. Place on the magnetic stirrerand titrate to a potentiometric end point with 0.1 N HClO4 inaccordance with 20.4.19. Apparatus19.1 pH Meter, equipped with a standard glass electrode anda calomel electrode modified as follows:19.1.1 Discard the aqueous potassium chloride solution,then rinse and fill with the calomel electrode solution asdescribed in Add a few crystals of potassium chloride and silverchloride or silver oxide to the electrode.19.2 Buret, micro, 10-mL capacity.22. Calculation22.1 Calculate the degree of etherification, H, as follows(Note 3):M 5 AN 3 100!/ G 3 100 2 B!!(5)H 5 0.162 M/ 1.000– 0.080 M!!(6)where:M5 milliequivalents of acid consumed per gram ofsample,A5 HClO4 added, mL,N5 normality of HClO4,G5 sample used, g,B5 percent moisture, determined on a separate sample,in accordance with Sections 4-7,162 5 gram molecular mass of an anhydroglucose unit ofcellulose, and80 5 net increase in molecular mass of ananhydroglucoseunitforeachsodiumcarboxymethyl group added.20. Reagents20.1 Acetic Acid, glacial.20.2 Calomel Electrode Solution—Add 2 g of potassiumchloride (KCl) and 2 g of silver chloride (AgCl) or silver oxide(Ag2O) to 100 mL of methanol and shake thoroughly tosaturate. Use the supernatant liquid.20.3 1,4-Dioxane.20.4 Perchloric Acid (0.1 N)—Add 9 mL of concentratedperchloric acid (HClO4, 70 % to 1 L of dioxane, with stirring(Warning—See Note 2). Store in an amber glass bottle. Anyslight discoloration that appears on standing may bedisregarded.NOTE 3—The result calculated in accordance with Section 18 includesthe alkaline sodium from sodium glycolate; however, if the latter is lessthan 0.5 %, the interference is negligible.NOTE 2—Warning: The solution of perchloric acid in dioxane shouldnever be heated or allowed to evaporate.20.4.1 Standardize the solution as follows: Dry potassiumacid phthalate for 2 h at 120 C. Weigh 2.5 g to the nearest0.0001 g into a 250-mL volumetric flask. Add glacial acetic23. Precision and Bias23.1 Precision—Statistical analysis of interlaboratory test3

D 1439results indicates the precision of this test method as shownbelow:ApproximateD.E. Level0.400.801.35Precision, D.E. Units(95 % Confidence Level)60.01060.01260.03823.2 Bias—No justifiable statement can be ma

2 Annual Book of ASTM Standards, Vol 06.03. 3 Annual Book of ASTM Standards, Vol 14.03. 4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia .

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