1、Designation: D5564 95 (Reapproved 2011)Standard Test Method forDetermination of the Total Ammonia Contained inSulfonated or Sulfated Oils1This standard is issued under the fixed designation D5564; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 of revision, the year 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.1. Scope1.1 This test method covers determination of the totalammonia contained in sulfonated or sulfate
3、d oils.1.2 The values stated in SI units are to be regarded as thestandard.1.3 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-priate safety and health practices and determin
4、e the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D5350 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Titration, Test Method A3. Significance and Use3.1 This test method of analysis is intended to determine thetotal
5、ammonia in a sample of sulfonated or sulfated oil, or both,by boiling a water solution of the sample with excess alkali anddetermining by titration the loss in alkali after the boiling.4. Apparatus4.1 The apparatus required consists of a glass flask providedwith a glass stopper and an air condenser.
6、 The connectionbetween the flask and the condenser shall be a ground joint.Perforated glass beads shall be used to prevent bumping.4.1.1 FlaskAn Erlenmeyer flask (Fig. 1) made of aborosilicate glass, having a capacity of approximately 300 mLand provided with a glass stopper.4.1.2 Condenser, consisti
7、ng of a glass tube, 915 mm (36 in.)in length and 8 mm (516 in.) in outside diameter. The lower endof the tube shall be flared and ground to fit the mouth of theErlenmeyer flask.4.1.3 Glass BeadsPerforated glass beads, made of chemi-cally resistant glass, approximately 4 mm (532 in.) in diameter.Befo
8、re using, the glass beads shall be boiled thoroughly inseveral portions of water or until the wash water reacts neutralto a methyl orange indicator.5. Reagents5.1 Ethyl Ether.5.2 Methyl Orange Indicator Solution (1 g/L)Dissolve 0.1g of methyl orange in 100 mL of water.5.3 Sodium Chloride (NaCl), sol
9、id.5.4 Sodium Hydroxide, Standard Solution (1 N)Accurately prepare and standardize a 1 N sodium hydroxide(NaOH) solution. Express the strength or concentration of thesolution as mg of KOH per mL; 1 mL of 1 N NaOH solutionis equivalent to 56.1 mg of KOH.1This test method is under the jurisdiction of
10、ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 49-1957).Current edition approved Jan. 1, 2011. Published March 2011. Originallyapproved in 1994. Last
11、 previous edition approved in 2006 as D5564 95(2006).DOI: 10.1520/D5564-95R11.2For 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 on
12、the ASTM website.FIG. 1 Apparatus for Determination of Organically CombinedSulfuric Anhydride, Method A1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.5 Sodium Hydroxide, Standard Solution (0.5 N) Accu-rately prepare and standardiz
13、e a 0.5 N NaOH solution. Expressthe strength of the solution as mg of KOH per mL; 1 mL of 0.5N NaOH solution is equivalent to 28.05 mg of KOH.5.6 Sulfuric Acid, Standard (0.5 N)Accurately prepareand standardize a 0.5 N sulfuric acid (H2SO4) solution. Expressthe strength of the solution as mg of KOH
14、per mL; 1 mL of 0.5N H2SO4is equivalent to 28.05 mg of KOH.5.7 Sulfuric Acid (1+19)Carefully mix 1 volume of con-centrated sulfuric acid (H2SO4, sp gr 1.84) into 19 volumes ofwater while stirring.6. Procedure6.1 The procedure consists of two determinations: namely,(1) the total alkalinity, and (2) t
15、he loss in alkalinity after boilingwith excess NaOH.6.1.1 Total AlkalinityDetermine the total alkalinity asdescribed in the determination of organically combined sulfu-ric anhydride, Test Method D5350; Procedure.6.1.2 Alkalinity After BoilingDissolve 10 g of the samplein 100 mL of water in a 500-mL
16、beaker, add 25 mL of 0.5 NNaOH solution, and boil the mixture for 30 min or until all theammonia is expelled as indicated by moistened red litmuspaper. Cool the contents of the beaker, add methyl orangeindicator solution (0.1 %), and titrate to an approximate endpoint. Transfer the mixture to a 250-
17、mL glass-stoppered flaskand complete the titration (with the addition of salt and ether)as described in the determination of organically combinedsulfuric anhydride, Test Method D5350; Procedure.7. Calculation7.1 Calculate the total ammonia, %, as follows:T 5 A 1 $B 3 D! 2 C 3 E!#/W% (1)ortotal ammon
18、ia 5 0.0303 T (2)where:T = total ammonia, mg of KOH/g,A = total alkalinity, mg of KOH/g,B = mL of NaOH solution added,C =mLofH2SO4required for titration of the sample,D = strength of NaOH solution, mg of KOH/mL,E = strength of H2SO4, mg of KOH/mL, andW = weight of sample, g.8. Precision and Bias8.1
19、This test method is adopted from the procedures of theAmerican Leather Chemists Association, where it has longbeen in use and was approved for publication before theinclusion of precision and bias statements was mandated. Theoriginal interlaboratory test data are no longer available. Theuser is caut
20、ioned to verify by the use of reference materials, ifavailable, that the precision and bias (or reproducibility) of thistest method is adequate for the contemplated use.9. Keywords9.1 leather; sulfated; sulfonated; total ammoniaASTM International takes no position respecting the validity of any pate
21、nt rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision
22、at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comme
23、nts will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted
24、 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5564 95 (2011)2
