ASTM D5070-90(1997)

Standard Test Method for Synthetic Quaternary Ammonium Salts in Fabric Softeners by Potentiometric Titrations

SCOPE
1.1 This test method describes a potentiometric titration procedure for the determination of quaternary ammonium salts in fabric softeners. This test method is intended for the analysis of known quaternary ammonium salts such as the dialkyl dimethyl quaternary ammonium compound type and the diamidoamine based quaternary ammonium compound type.
1.2 The quaternary ammonium salts conform to the structures shown in Figs. 1 and 2.
1.3 The analytical procedure appears in the following order: Section Apparatus 5 Reagents 6 Preparation of standard reagents 7 Standardization of hyamine solution 8 Safety precautions 9 Procedure for determination of dialkyl dimethyl quaternaries 10 Procedure for determination of diamidoamine based quaternaries 11
1.4 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Mar-1997
• ICS: 71.060.50 - Salts
• Technical Committee: D12 - Soaps and Other Detergents
• Drafting Committee: D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components

Relations

• Replaced By: ASTM D5070-90(2005) - Standard Test Method for Synthetic Quaternary Ammonium Salts in Fabric Softeners by Potentiometric Titrations
• Effective Date: 01-May-2005

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5070–90(Reapproved 1997)
Standard Test Method for
Synthetic Quaternary Ammonium Salts in Fabric Softeners
by Potentiometric Titrations
This standard is issued under the fixed designation D5070; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope Methods forAnalysis andTesting of Industrial Chemicals
1.1 This test method describes a potentiometric titration
3. Summary of Test Method
procedureforthedeterminationofquaternaryammoniumsalts
3.1 Quaternary ammonium compounds present in fabric
infabricsofteners.Thistestmethodisintendedfortheanalysis
softeners,astheactivematerials,aretitratedpotentiometrically
of known quaternary ammonium salts such as the dialkyl
in an aqueous medium with a standard solution of sodium
dimethyl quaternary ammonium compound type and the dia-
lauryl sulfate using a nitrate ion-selective electrode. In this
midoamine based quaternary ammonium compound type.
potentiometric titration, the reaction involves the formation of
1.2 The quaternary ammonium salts conform to the struc-
a complex between the quaternary ammonium compound and
tures shown in Fig. 1 and Fig. 2.
theanionicsurfactantwhichthenprecipitates.Attheendpoint,
1.3 Theanalyticalprocedureappearsinthefollowingorder:
the nitrate ion electrode appears to respond to an excess of
Section
titrant with a potential change large enough to give a well
Apparatus 5
Reagents 6
defined inflection in the titration curve. Alternatively the
Preparation of standard reagents 7
quaternary ammonium compound can be first complexed with
Standardization of hyamine solution 9
an excess of standard sodium lauryl sulfate; the excess sodium
Safety precautions 8
Procedure for determination of dialkyl dimethyl quaternaries 10
lauryl sulfate is titrated potentiometrically with standard
Procedure for determination of diamidoamine based quaternaries 11 5
Hyamine 1622.
1.4 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.1 This test method is used to determine the quaternary
ammonium salts commonly found in fabric softeners. Quater-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. nary ammonium compounds being the active ingredients in
fabric softeners requires accurate determination to assess the
2. Referenced Documents
cost and performance of such compounds.
2.1 ASTM Standards:
5. Apparatus
D459 Terminology Relating to Soaps and Other Deter-
2 6
gents 5.1 AutotitrationSystem—buretwith10or20mLcapacity;
3 7 8
magnetic stirrer; evaluating ruler.
D1193 Specification for Reagent Water
D1681 Test Method for Synthetic Anionic Active Ingredi-
ent in Detergents by Cationic Titration Procedure
D3049 Test Method for Synthetic Anionic Ingredient by 4
Annual Book of ASTM Standards, Vol 15.05.
Cationic Titration The sole source of supply of Hyamine 1622 known to the committee at this
time is Gallard Schlesinger Manufacturing Corp., 584 Mineola Ave., Carle Place,
E180 Practice for Determining the Precision of ASTM
NY11514.Ifyouareawareofalternativesuppliers,pleaseprovidethisinformation
to ASTM Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee, which you may attend.
Metrohm-Brinkman E-536, or equivalent, has been found satisfactory. Avail-
This test method is under the jurisdiction ofASTM Committee D-12 on Soaps able from Brinkman Instruments Inc., Cantiague Rd., Westbury, NY 11590.
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Potentiograph/E-535 and Dosimat/E-459, or equivalent, have been found
Analysis of Soaps and Synthetic Detergents. satisfactory. Available from Brinkman Instruments Inc., Cantiague Rd., Westbury,
Current edition approved May 25, 1990. Published July 1990. NY 11590.
2 8
Annual Book of ASTM Standards, Vol 15.04. Evaluating Ruler EA-893, or equivalent, has been found satisfactory.Available
Annual Book of ASTM Standards, Vol 11.01. from Brinkman Instruments Inc., Cantiague Rd., Westbury, NY 11590.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5070
5.2 Electrodes—(1) nitrate specific ion electrode; (2) sur-
10 11
factant electrode; (3) Ag/AgCl reference electrode.
5.3 Adaptors—(1) coaxial adaptor, required for indicator
electrode, (2) banana plug adaptor, required for reference
electrode.
NOTE 1—To insure electrical continuity (after assembly) shake down
electrode in the manner of a clinical thermometer.Also, the conditioning
−
X 5 chloride or methyl sulfate
of the electrode is essential for obtaining a good break in the titration
R 5 fatty alkyl groups saturated or unsaturated, normal or branched C −C
8 22
curve.Conditioningnewelectrodesin0.01MKNO ,aqueoussolutionfor
FIG. 1 Dialkyl Dimethyl Quaternaries
60 min (or more) prior to use is recommended.
NOTE 2—Other electrodes (for example, a calomel electrode) are
suitable as the reference electrode provided they give a stable reference
potential during the titration. Reference electrodes having a ceramic or an
asbestos junction tend to clog with use. Therefore, a ground-glass sleeve
electrode (such as the Metrohm EA 440 or equivalent) is suggested.
6. Reagents
6.1 Hyamine 1622, diisobutylphenoxyethoxyethyl dim-
ethyl benzyl ammonium chloride monohydrate.
6.2 Sodium Lauryl Sulfate, primary standard (Note 3).
NOTE 3—Sodium lauryl sulfate must be analyzed for purity according
to the Reagent section ofTest Method D3049, before its use as a primary
standard.
−
X 5 usually methyl sulfate
6.3 Water, type III reagent water conforming to Specifica-
R 5 fatty alkyl groups, saturated or unsaturated, normal or branched C −C
12 18
R 5 2-hydroxyethyl,
tion D1193.
2-hydroxypropyl
6.4 Isopropanol, reagent grade.
FIG. 2 Diamidoamine Based Quarternaries
NOTE 4—Warning:HIGHLY FLAMMABLE.
6.5 Sodium Borate Decahydrate—(Na B O 10H O), re-
2 4 7 2
7. Preparation of Standard Reagents
agent grade.
−3
7.1 Sodium Lauryl Sulfate Solution,4 310 N—Weigh
6.6 Boric Acid (H BO ), reagent grade.
3 3
accurately 1.15 6 0.01 g of sodium lauryl sulfate to 0.1 mg;
NOTE 5—Warning:CAUSES IRRITATION.
dissolve in water and dilute to a final volume of 1 L. Calculate
the normality of the solution with the following equation:
6.7 Sulfuric Acid (H SO ), reagent grade.
2 4
W 3 P
NOTE 6—Warning: CAUSES SEVERE BURNS ON CONTACT
Normalityofsodiumlaurylsulfate 5 (1)
~288.38! ~100!
WITH SKIN. See Section 8.
6.8 Five percent (V/V) Sulfuric Acid Solution—Using a
where:
graduated cylinder, transfer 80 mL of deionized water to a P 5 purity of the sodium lauryl sulfate, weight %
100-mL volumetric flask. Slowly, carefully, and with stirring, W 5 weight of sodium lauryl sulfate, g
7.2 Keepthesolutionnolongerthan1monthbeforemaking
add5mLofconcentratedsulfuricacid.Cooltoroomtempera-
ture and dilute to the mark with water. a fresh solution.
−3
7.3 Hyamine 1622 Solution,4 310 N—Dissolve 1.85 6
6.9 Borate Buffer Solution pH 6.00—In a 500 mL beaker,
dissolve 5.0 g 6 0.02 g of sodium borate decahydrate and 7.0 0.5 g of Hyamine 1622 in deionized water. Transfer toa1L
volumetric flask, and dilute to volume with water.
g 6 0.02 g of boric acid in approximately 300 mLwater, with
stirring; adjust pH to 6.00 with 5% sulfuric acid solution.
8. Hazards
Transfer to a 500-mL volumetric flask, mix, and dilute to
volume with water.
8.1 ALL REAGENTS AND CHEMICALS SHOULD BE
HANDLED WITH CARE. BEFORE USING ANY CHEMI-
CAL,READANDFOLLOWALLSAFETYPRECAUTIONS
Orion Model 93.07, or equivalent, has been found satisfactory.Available from
AND INSTRUCTIONS ON THE MANUFACTURER’S LA-
Orion Research Inc., 529 Main St., Boston, MA 02129.
10 BEL OR MSDS (MATERIAL SAFETY DATA SHEET).
OrionModel93.42,orequivalent,hasbeenfoundsatisfactory.Availablefrom
Orion Research Inc., 529 Main St., Boston, MA 02129.
MetrohmModelEA-440,orequivalent,hasbeenfoundsatisfactory.Available 9. Standardization of Hyamine 1622 Solution
from Brinkman Instruments Inc., Cantiague Rd., Westbury, NY 11590.
12 9.1 Thisdeterminationmustbedoneintriplicate.Pipet5.00
The Metrohm coaxial adaptor, or equivalent, has been found satisfactory fo
...