1、Designation: D 2363 79 (Reapproved 2006)Standard Test Methods forHydroxypropyl Methylcellulose1This standard is issued under the fixed designation D 2363; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、 number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the testing of hydroxypropylmethylcellulose.1.2 The test procedures appear in the following order:SectionsMo
3、isture 4 to 6Ash (as Sulfate) 7 to 10Chlorides (as NaCl) 11 to 14Alkalinity (as Na2CO3) 15 to 18Iron 19 to 24Heavy Metals 25 to 29Methoxyl Content 30 to 35Hydroxypropoxyl Content 36 to 41Viscosity 42 to 46pH 47Solids 48 to 51Density 52 to 561.3 The values stated in SI units are to be regarded as the
4、standard. The values given in parentheses are for informationonly.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 establish appro-priate safety and health practices and determine the app
5、lica-bility of regulatory limitations prior to use. For a specifichazard statement, see 33.5.1.2. Referenced Documents2.1 ASTM Standards:2D96 Test Method for Water and Sediment in Crude Oil byCentrifuge Method (Field Procedure)3E70 Test Method for pH of Aqueous Solutions With theGlass Electrode3. Pu
6、rity 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 Society, where suchspecifications are available.4Other grades may be
7、used, pro-vided 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.MOISTURE4. Scope4.1 This test method covers the d
8、etermination of the volatilecontent of hydroxypropyl methylcellulose and, by commonusage, designated moisture.5. Procedure5.1 Transfer 2 to5gofthesample weighed to the nearest0.01 g to a tared dish (fitted with a lid) and dry for2hinanoven at 100 to 105C with lid removed. Remove the dish fromthe ove
9、n, cover with a lid, cool in a desiccator, and weigh.6. Calculation6.1 Calculate the percent of moisture as follows:Moisture, % 5 A/B! 3 100 (1)where:1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directrespo
10、nsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 1965. Last previous edition approved in 2000 as D 2363 79 (2000)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orconta
11、ct ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the
12、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.1Copyright ASTM International, 100 Barr Harb
13、or Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.A = mass loss on heating, andB = sample used, g.ASHAS SULFATE7. Scope7.1 This test method covers the determination of the amountof residue left from igniting a sample of hydroxypropylmethylcellulose after being moistened with sul
14、furic acid.8. Reagents8.1 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).8.2 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid(H2SO4).9. Procedure9.1 Weigh to the nearest 0.01 g about2gofthesample(previously dried for12 h at 105C) into a tared Coors No. 1,high-form, porcelain crucible. Ad
15、d 5 drops of H2SO4aroundthe inside surface of the crucible. Place the crucible inside of aloosely fitting aluminum ring (approximately 32 mm (114 in.)high, with 6.4-mm (14-in.) sidewall, and 44-mm (134-in.)inside diameter, cut from a piece of aluminum pipe) on a hotplate. Loosely cover with a crucib
16、le cover. Carefully char thehydroxypropyl methylcellulose until all the volatiles are re-moved.9.2 Cool the crucible, add 1 ml of H2SO4and2mlofHNO3so that it completely wets the charred residue. Cautiously heatto dense white fumes on a hot plate. Place the uncoveredcrucible in a muffle furnace at 60
17、0C and ignite until all thecarbon is gone (for about 1 h). Transfer to a dessicator untilcool, then weigh. (Save the residue for the Heavy Metalsdetermination.)10. Calculation10.1 Calculate the percent of ash, C, as follows:C 5 A/B! 3 100 (2)where:A = sulfated ash, g, andB = sample used, g.CHLORIDES
18、AS SODIUM CHLORIDE11. Scope11.1 This test method covers the determination of the totalpercent of chloride (bromide included if present) calculated assodium chloride (NaCl) in hydroxypropyl methylcellulose. Thesample is dispersed and the chloride titrated volumetricallywith 0.100 N silver nitrate sol
19、ution.12. Reagents12.1 Ferric Alum Indicator Solution Add 100 g of ferricammonium sulfate FeNH4(SO4)212H2O to 250 mL of water.Heat to boiling and add NHO3(sp gr 1.42) slowly until the redcolor is removed. This will usually require about 6 to 15 mL ofHNO3. Filter the solution and store in a glass bot
20、tle.12.2 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).12.3 Potassium Thiocyanate Standard Solution (0.1 N)Dissolve 10 g of potassium thiocyanate (KCNS) in 1 L ofwater. By means of a pipet, measure 25 mL of 0.100 N silvernitrate (AgNO3) solution into a 400-mL beaker.Add 100 mL ofwater, 10 m
21、L of HNO3(sp gr 1.42), and 5 mL of ferric alumindicator solution. Titrate with the KCNS solution, whilestirring, until a faint persistent red color is produced. Calculatethe normality, N, of the KCNS solution as follows:N 5 A/B!3 0.1 (3)where:A = 0.100 N AgNO3solution added, mL, andB = KCNS solution
22、 required for the titration, mL.12.4 Silver Nitrate-Standard Solution (0.100 N)Grindsilver nitrate (AgNO3) crystals fine enough to pass through aNo. 20 (850-m) sieve and then dry for2hat110C. Preparea 0.100 N solution by dissolving 16.989 g of dry AgNO3inchloride-free water and diluting to 1 L in a
23、volumetric flask.13. Procedure13.1 Weigh to the nearest 0.01 g about 1.0 g of the sample(previously dried for12 h at 100 to 105C) and transfer to a500-mL, wide-mouth Erlenmeyer flask. Add 250 mL of hotwater and swirl for a few minutes; then cool to dissolve.13.2 Add 5 mL of 0.100 N AgNO3solution and
24、 5 mL offerric alum indicator solution, and back-titrate with 0.1 NKCNS solution to the first appearance of a faint pink color.14. Calculation14.1 Calculate the percent of chlorides as NaCl as follows:Chlorides, % 5 AB 2 CD! 3 0.0585/E! 3 100 (4)where:A = AgNO3solution added, mL,B = normality of the
25、 AgNO3solution,C = KCNS solution required to back-titrate the excessAgNO3, mL,D = normality of the KCNS solution, andE = sample used, g.ALKALINITYAS SODIUM CARBONATE15. Scope15.1 This test method covers the determination of the totalalkalinity of hydroxypropyl methylcellulose expressed as so-dium ca
26、rbonate (Na2CO3).16. Reagents16.1 Methyl Purple Indicator Solution.16.2 Sulfuric Acid, Standard (0.01 N) Prepare and stan-dardize a 0.01 N solution of sulfuric acid (H2SO4).17. Procedure17.1 Weigh to the nearest 0.01 g about 1.0 g of the sample(previously dried for12 h at 100 to 105C) and transfer t
27、o a500-ml, widemouth Erlenmeyer flask. Add 250 mL of hotwater and swirl for a few minutes; then cool to dissolve.D 2363 79 (2006)217.2 Add 4 drops of methyl purple indicator solution andtitrate to the first faint pink color with 0.01 N H2SO4.18. Calculation18.1 Calculate the percent alkalinity as Na
28、2CO3, S,asfollows:S 5 AB 3 0.053!/C 3 100 (5)where:A =H2SO4required for titration of the sample, mL,B = normality of the H2SO4, andC = sample used, g.IRON19. Scope19.1 This test method covers the determination of total ironcontent in samples of hydroxypropyl methylcellulose. The ironis converted to
29、ferric sulfate which reacts with the indicator toform a pink color that can be quantitatively measured.20. Apparatus20.1 PhotometerAny photoelectric filter photometer orspectrophotometer suitable for measurements at 430 nm.20.2 Kjeldahl FlasksCalibrated to contain 50 mL, andmade of heat- and chemica
30、l-resistant glass.21. Reagents21.1 Ammonium Hydroxide (sp gr 0.90)Concentrated am-monium hydroxide (NH4OH).21.2 Buffer SolutionDissolve 20 g of sodium bicarbonate(NaHCO3) and 10 g of sodium carbonate (Na2CO3) in waterand dilute to 1 L.21.3 Disodium-1,2-Dihydroxybenzene-3,5-DisulfonateSolutionPrepare
31、 an aqueous solution containing 25 g/L.21.4 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl).21.5 Hydrogen Peroxide (30 %)Concentrated hydrogenperoxide (H2O2).21.6 Iron Standard Solution (0.0001 g Fe/ml)Dissolve0.01 g of iron powder containing not less than 99.9 % iron inHCl (sp g
32、r 1.19). Oxidize the solution with bromine water andexpel the excess by boiling. Dilute to 1 L in a volumetric flask.21.7 Phenolphthalein Indicator Solution (1 g/100 mL)Dissolve1gofphenolphthalein in 100 mL of ethanol (95 %).21.8 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid(H2SO4).21.9 Sulfu
33、ric Acid (1+4)Carefully mix 1 volume ofH2SO4(sp gr 1.84) with 4 volumes of water, adding the H2SO4gradually while mixing.22. Preparation of Calibration Curve22.1 Following the procedure given in Section 23, and usingvaried amounts of the standard iron solution prepared inaccordance with 21.6, prepar
34、e a calibration curve showing ironcontent in parts per million and the corresponding photometerreadings.23. Procedure23.1 Weigh to the nearest 0.01 g about2gofthesample(previously dried for12 h at 100 to 105C). Transfer by meansof a funnel to a Kjeldahl flask. Place the flask at a 20 angle inthe fur
35、nace at 500C and heat until some charring of the samplehas taken place. (Care must be taken not to char too much.)Remove and allow to cool.23.2 Add 3 mL of H2SO4to the flask. Place on the digestionrack and digest. Cool and add H2O2dropwise until the solutionis clear. Heat over a Meker burner to a vo
36、lume of 2 mL. Cool,and wash the sides of the flask with water. Add 3 drops ofphenolphthalein indicator solution. Add NH4OH to a red endpoint. Wash the neck of the flask. The solution should be clearand not greater than 20 mL in volume.23.3 Add 2 mL of the color-forming solution described in21.3, and
37、 mix. Adjust pH to 7.0 and then dilute to mark withbuffer. Transfer a small portion to an absorption cell anddetermine the photometer reading at 480 nm.23.4 BlankMake a blank determination, using the sameamount of reagents and the same procedure as for the sample.24. Calculation24.1 Read the iron co
38、ntent, in parts per million, directlyfrom the calibration curve (Section 22). Subtract the parts permillion of iron due to iron in the blank.HEAVY METALS25. Scope25.1 This test method covers the determination of whetheror not the heavy metals content of hydroxypropyl methylcel-lulose is below a give
39、n level based on a lead standard.26. Summary of Test Method26.1 The ash residue from the sulfated ash test is digestedwith dilute hydrochloric acid. A standard containing a knownamount of lead is prepared, and the heavy metals content isdetermined qualitatively by comparing the sample to thestandard
40、.27. Apparatus27.1 Nessler Tubes, 50-mL.27.2 Volumetric Flasks, 50-mL.28. Reagents28.1 Acetic AcidGlacial acetic acid.28.2 Ammonium Hydroxide (sp gr 0.90)Concentrated am-monium hydroxide (NH4OH).28.3 Ammonium Hydroxide (2+3)Dilute 400 mL ofNH4OH (sp gr 0.90) with sufficient water to make 1000 mL.28.
41、4 Buffer SolutionDissolve 60 mL of acetic acid inabout 500 mL of water, add 10 mL of NH4OH, and dilute to 1L.28.5 Hydrochloric Acid (1+2)Dilute 1 volume of concen-trated hydrochloric acid (HCl, sp gr 1.19) with 2 volumes ofwater.28.6 Hydrogen Sulfide TSSaturate a convenient volume ofwater with hydro
42、gen sulfide (H2S) in a narrow-neck, glass-stoppered, amber bottle. This solution must be made fresh.D 2363 79 (2006)328.7 Hydroxylamine Hydrochloride Solution (200 g/L)Dissolve 20 g of hydroxylamine hydrochloride (NH2OHHCl)in 100 mL of water.28.8 Lead Nitrate Stock SolutionDissolve 159.8 mg oflead n
43、itrate (Pb(NO3)2) in 100 mL of water containing 1 mL ofHNO3(sp gr 1.42). Dilute with water to 1000.0 mL and mix.This solution should be prepared and stored in glass containersthat are free from lead salts.28.9 Lead Standard Solution (1 mL = 1 g Pb)Dilute 10mLof the lead nitrate stock solution, accur
44、ately measured, withwater to 100.0 mL. Each millilitre of the solution so preparedcontains 10 g of lead.29. Procedure29.1 Pipet into a 50-mL Nessler tube 0.15 mL of HCl (1+2),2 mL of the buffer solution, and a volume of the standard leadsolution containing the quantity of lead equivalent to thespeci
45、fied heavy metals limit. Add water to make 40 mL andlabel as Solution A. Make sure that the final pH of thesesolutions is between 3 and 4. This can be tested by pH indicatorpaper or pH meter. For visual comparison make sure that theoptimum lead content is between 20 and 40 g.29.2 To the crucible con
46、taining the sulfated ash residue add4 mL of HCl (1+2). Cover and carefully digest on a steam bathfor 10 min. Uncover and slowly evaporate to dryness. Moistenthe residue with 0.15 mL of HCl (1+2), 0.5 mL of hydroxy-lamine hydrochloride solution, and 10 mL of hot water.Carefully digest for 2 min. Add
47、2 mL of the buffer solution.Filter if necessary. Thoroughly wash the crucible and filter withwater into a 50-mL Nessler tube that matches the one used forSolution A. If necessary, adjust the pH to 3 to 4 with NH4OH(2+3) or HCl (1+2) using pH indicator paper. Dilute to 40 mLand label this Solution B.
48、29.3 Add 10 mL of H2S solution to each tube: Solution Aand Solution B. Mix and view downward over a white surface.The color of Solution B shall be no darker than that of SolutionA. Make the comparison within 10 min.METHOXYL CONTENT30. Scope30.1 This test method covers the determination of themethoxy
49、l content of hydroxypropyl methylcellulose. Totalalkoxyl is first determined and the methoxyl content found bysubtracting the hydroxypropyl content from the total alkoxylfigure.31. Summary of Test Method31.1 The hydroxypropyl methylcellulose is heated with astrong solution of hydriodic acid to form an alkyl iodide, whichby means of a carbon dioxide stream is swept through acondenser and finally absorbed in a mixture of bromine, aceticacid, and sodium acetate. The alkyl iodide absorbed in theaforementioned mixture is oxi
