1、Designation: D 5564 95 (Reapproved 2006)Standard Test Method forDetermination of the Total Ammonia Contained inSulfonated or Sulfated Oils1This standard is issued under the fixed designation D 5564; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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.1. Scope1.1 This test method covers determination of the totalammonia contained in sulfonated or sulf
3、ated 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 deter
4、mine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 5350 Test Method for Determination of OrganicallyCombined Sulfuric Anhydride by Titration, Test Method A3. Significance and Use3.1 This test method of analysis is intended to determine thetota
5、l 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 condense
6、r. 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, consis
7、ting 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.Be
8、fore 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), s
9、olid.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.5.5 Sodium Hydroxide, Standard Solution (0.5
10、N) Accu-rately prepare and standardize 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. Express1This
11、 test method is under the jurisdiction of 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 April 1, 2006. Published A
12、pril 2006. Originallyapproved in 1994. Last previous edition approved in 2001 as D 5564 95(2001).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 Docum
13、ent Summary page onthe 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.the strength of the solution as mg of KOH per mL; 1 mL of 0.5N
14、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) the loss in alkalinity
15、 after boilingwith excess NaOH.6.1.1 Total AlkalinityDetermine the total alkalinity asdescribed in the determination of organically combined sulfu-ric anhydride, Test Method D 5350; Procedure.6.1.2 Alkalinity After BoilingDissolve 10 g of the samplein 100 mL of water in a 500-mL beaker, add 25 mL of
16、 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-mL glass-stoppered f
17、laskand complete the titration (with the addition of salt and ether)as described in the determination of organically combinedsulfuric anhydride, Test Method D 5350; Procedure.7. Calculation7.1 Calculate the total ammonia, %, as follows:T 5 A 1 $B 3 D! 2 C 3 E!#/W% (1)ortotal ammonia 5 0.0303 T (2)wh
18、ere: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 This test method is
19、 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 cautioned to verify by
20、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 patent rights asserted
21、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 at any time by the
22、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 comments will receive ca
23、reful 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 by ASTM Internatio
24、nal, 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).D 5564 95 (2006)2
