1、Designation:D 4224-89 AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race St.,Philadelphia,Pa.19103 Reprinled from the Annual Book of ASTM Standards.Copyrighl ASTM If not listed in the currenl combined index,will appear in the nexl edilion.Standard Test Method for Anionic Detergent by Pam-foluidine
2、 Hydrochloride This standard is issued under the fixed designation D 4224;the number immediately following the designation indicates the year of origjnal adoption or,in the case of revision,the year of last revision.A numberin parentheses indicates the year of last reapproval.A superscript epsilon(6
3、)indicates an editorial change since the last revision or reapproval.1.Scope I.1 This test method covers the determination of the equiv-alent weight and the amount of total anionic ingredient in a surfactant.It is applicable to single organic sulfates and sulfonates of specified molecular weights,an
4、d in general wherever an aliphatic chain longer than six carbons is present.1.2 This test method includes the use of carbon tetrachlo-ride,a hazardous solvent,that,while not flammable,is very harmful to the human body,particularly the liver.Breathing of vapors and repeated or prolonged contact with
5、the skin is to be avoided.It is the responsibility of the user of this standard to establish appropriate safety practices and to determine the applicability of regulatory limitations prior to use.Material Safety Data Sheets are available for reagents and materials.Review them for hazards prior to us
6、age,1.3 The analytical procedures appear.in the following order:Equivalent Weight Percent Anionic Detergent 2.Referenced Documents Sections 5 to 10 II to 16.2.1 ASTM Standards:D 1193.Specification for Reagent Wate?E 200 Practice for Preparation,Standardization,and Storage of Standard Solutions for C
7、hemical Analysis 3.Significance and Use 3.1 Other direct titration methods for making this deter-mination require prior knowledge of the equivaletit weight of the material.Different methods,while riot contingent on knowledge of equivalent weight,depend on time-consuming and often imprecise determina
8、tions of many individual components.3.2 The procedures described in this test method offer a relatively rapid and simple approach to determining both the equivalent weight and the amount of anionic surfactant preserit in a surfactant formulation.4.Interferences 4.1 Soaps,fatty acids and fatty amides
9、 may interfere.4.2 Low molecular weight sulfonates,such as those of toluene and xylene,do not interfere when present tip to 15%of active material,nor do normal inorganic components of I This test method is under the jurisdiction of-ASTM Committee D-12 on Soaps and Other Detergents and is the direct
10、resoonsibiitv of Subcommittee Dli.12 on Analysis of Soaps and Synthetic Detergents.-Current edition approved May 26,1989.Published July 1989.Originally published as D4224-83.Last previous edition D4224-83.2 Annual Book of ASTM Standards,Vol 11.O 1.detergent formulations such as chloride,sulfate,bora
11、te,phosphates,perborate,and silicates.EQUIVALENT WEIGHT 5.Summary of Test Method 5.1 Carbon tetrachloride extractable materials are re-moved from an alcohol-water solution of the sample which is then treated with para-toluidine hydrochloride.This reagent reacts with high molecular weight anionic sur
12、factants to form amine salts that are soluble in and can be extracted quantitatively by carbon tetrachloride.5.2 The carbon tetrachloride extract is dried and weighed to give the weight of the amine salt formed.The residue is dissolved in alcohol and titrated against standard base and standard silve
13、r nitrate.The equivalent weight is calculated from the weight of the amine salt and the two titrations.6.Apparatus 6;1 Analytical Balance,6.2 Vacuum Oven.6.3 Vacuum Pump or Aspirator,6.4 Desiccator.6.5 Steam Bath.6.6-Automatic TitratorS3(Alternative:D 820:39-41 man-ual titration.)6.7 ing.4 Combinati
14、on Electrode,silver with silver chloride coat-6.8 Beaker,tall form,.180 mL.5 7.Reagents and Materials 7.1 Purity of Reagents-Reagent grade chemicals shall be used in all tests.Unl&s otherwise indicated,it is intended that all reagents conform to the specifications of the Com-mittee on Analytical Rea
15、gents of the American Chemical Society where such specifications are available.”Other grades may be used,provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessen-ing the accuracy of the determination.7.2 Purity of Water-Unless otherwise indica
16、ted,refer-ences to water shall be understood to mean water as defined by Type II of Specification D 1193.3 The Metrohm E436 has been found satisfactory for this purpose.4 The Metrohm E246 has been found satisfactory for this 5 The Pyrex beaker,No.114,or its equivalent,has been found satisfactory for this purpose.6“Reagent Chemicals,American Chemical Society Specifications,”Am.Chem-ical Sot.,Washington,D.C.For suggestions on the testing of reagents not listed by The American Chemical Society,see“
