ASTM D5806-95

Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration

SCOPE
1.1 This test method covers a potentiometric titration procedure for determining active matter in disinfectant quaternary ammonium salts. This test method is intended for the analysis of quaternary ammonium salts used as disinfectants, and only applies to the following commonly used quaternary ammonium salts: -alkyldimethylbenzylammonium chloride (see Fig. 1), cetyltrimethylammonium chloride, and a blend of -octyldecyl dimethylammonium chloride, di- -octyl dimethylammonium chloride, and di -decyldimethyl ammonium chloride (see Fig. 2). Also, this test method can be applied to the analysis of disinfectant type products where the formula ingredients are known and the quaternary ammonium salt is one of the above. Interferences such as amines oxides and betaines present in disinfectant formulations were not tested.  
1.2 This disinfectant quaternary ammonium salt conforms to the structures in Figs. 1 and 2.  
1.3 This standard does not purport to address all of the safety concerns, if any, 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. For specific precautionary information, see Section 8.

General Information

• Status: Historical
• Publication Date: 31-Dec-1994
• 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 D5806-95(2003) - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration
• Effective Date: 10-Oct-1995

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation:D5806–95
Standard Test Method for
Disinfectant Quaternary Ammonium Salts by Potentiometric
Titration
This standard is issued under the fixed designation D5806; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D1193 Specification for Reagent Water
D1681 Test Method for Synthetic Anionic Active Ingredi-
1.1 This test method covers a potentiometric titration pro-
ent in Detergents by Cationic Titration Procedure
cedure for determining active matter in disinfectant quaternary
D3049 Test Method for Synthetic Anionic Ingredient by
ammonium salts. This test method is intended for the analysis
Cationic Titration
of quaternary ammonium salts used as disinfectants, and only
E180 Practice for Determining the Precision Data of
appliestothefollowingcommonlyusedquaternaryammonium
ASTM Methods for Analysis and Testing of Industrial
salts: n-alkyldimethylbenzylammonium chloride (see Fig. 1),
Chemicals
cetyltrimethylammoniumchloride,andablendof n-octyldecyl
dimethylammonium chloride, di-n-octyl dimethylammonium
3. Terminology
chloride,anddi-n-decyldimethylammoniumchloride(seeFig.
3.1 Definitions—See Terminology D459D459.
2). Also, this test method can be applied to the analysis of
disinfectant type products where the formula ingredients are
4. Summary of Test Method
known and the quaternary ammonium salt is one of the above.
4.1 Disinfectant type quaternary ammonium compounds
Interferences such as amines oxides and betaines present in
present,astheactivematerialsindisinfectanttypeproductsare
disinfectant formulations were not tested.
titrated potentiometrically in an aqueous medium with a
1.2 This disinfectant quaternary ammonium salt conforms
standard solution of sodium lauryl sulphate using a nitrate
to the structures in Fig. 1 and Fig. 2.
ion-selective electrode or a surfactant electrode (see also Test
1.3 This standard does not purport to address all of the
Method D1681D1681). In this potentiometric titration, the
safety concerns, if any, associated with its use. It is the
reaction involves the formation of a complex between the
responsibility of the user of this standard to establish appro-
disinfectant quaternary ammonium compound and the anionic
priate safety and health practices and determine the applica-
surfactant which then precipitates.At the end point, the nitrate
bility of regulatory limitations prior to use. For specific
ion electrode or surfactant electrode appears to respond to an
precautionary information, see Section 8.
excess of titrant with a potential change large enough to give a
well defined inflection in the titration curve.
2. Referenced Documents
2.1 ASTM Standards:
5. Significance and Use
D459 Terminology Relating to Soaps and Other Deter-
5.1 Thistestmethodisusedtodeterminethepercentactives
gents
in each type of the disinfectant quaternary ammonium salts,
and also in the disinfectant products. Quaternary ammonium
compounds being the active ingredients in disinfectant-type
This test method is under the jurisdiction ofASTM Committee D-12 on Soaps
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on
Analysis of Soaps and Synthetic Detergents.
Current edition approved Oct. 10, 1995. Published December 1995. Annual Book of ASTM Standards, Vol 11.01.
2 4
Annual Book of ASTM Standards, Vol 15.04. Annual Book of ASTM Standards, Vol 15.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
D5806–95
where:
−
X = chloride, and
R = aliphatic, normal C −C .
8 22
FIG. 1 n-alkyldimethylbenzylammonium chloride and n-alkyldimethylethylbenzylammonium chloride
potential during the titration. Reference electrodes having a ceramic or an
asbestos junction tend to clog with use. Therefore, a ground-glass sleeve
electrode is suggested.
7. Reagents
7.1 Sodium Lauryl Sulfate, primary standard (see Note
3).
where:
7.2 Standardize with Hyamine 1622, dried previously at
−
X = chloride, and
105°C for 1 h.
R = aliphatic, normal C −C .
8 22
NOTE 3—Sodium lauryl sulfate must be analyzed for purity according
FIG. 2 Dialkyldimethyl quaternaries
to the Reagent section of Test Method D3049D3049 before using as a
primary standard.
7.3 Water, Type III, reagent water conforming to Specifica-
products require accurate determination to assess the cost and
tion D1193D1193.
antimicrobial performance of such products.
7.4 Isopropanol, reagent grade. Caution: Highly flam-
6. Apparatus mable.
5 7.5 Sodium Borate Decahydrate, (Na B O 10H O), re-
2 4 7 2
6.1 Autotitration System, with 10-mL buret capacity, or
6 7 agent grade.
20-mL buret capacity, magnetic stirrer, evaluating ruler,
8 7.6 Boric Acid,(H BO ), reagent grade. Caution: Causes
3 3
titroprocessor with 10-mL buret capacity or equivalent auto-
irritation.
titration system.
9 7.7 Sodium Hydroxide, (NaOH), reagent grade. Caution:
6.2 Nitrate Specific Ion Electrode, or surfactant elec-
Causes severe burns on contact with skin.
trode, or equivalent. Silver/silver chloride reference elec-
11 7.8 Sodium Hydroxide, 2N Solution—Dissolve 40 g of
trode.
sodiumhydroxideinapproximately300mLofdeionizedwater
6.3 Metrohm Coaxial Adaptor, required for indicator elec-
12 with stirring. Transfer to a 500-mL volumetric flask, dilute to
trode. Banana plug adaptor, required for reference electrode.
volume with deionized water, and mix well.
NOTE 1—To ensure electrical continuity (after assembly), shake down
7.9 Borate Buffer Solution—Dissolve 1.5 g Na B O·10
2 4 7
electrode in the manner of a clinical thermometer.Also, the conditioning
H O and 1.0 g H BO in approximately 200 mL deionized
2 3 3
of the electrode is essential for obtaining a good break in the titration
water, with stirring; adjust pH to 9.5 with 2N HaOH, transfer
curve. Conditioning new electrodes in 0.004 M sodium lauryl sulfate,
to a 1000-mLvolumetric flask, mix and dilute to volume with
aqueous solution for 60 min (or more) prior to use is recommended.Also
deionized water.
applies to the nitrate or surfactant electrode.
NOTE 2—Other electrodes (for example, calomel electrodes) are suit-
7.10 Octoxynol-9 Nonionic Surfactant.
able as the reference electrode provided they give a stable reference
7.11 Triton Solution, 1 %—Pipet 1 mL of the octoxynol-9
nonionic surfactant and transfer to a 100-mL volumetric flask
diluted to volume with deionized water.
−3
Metrohm-Brinkmann E-536, or equivalent, has been found satisfactory.Avail-
7.12 Sodium Lauryl Sulfate Solution, 8 3 10 N—Weigh
able from Brinkmann Instruments Inc., Cantiague Rd., Westbury, NY 11590.
accurately2.42 60.01gofsodiumlaurylsulfatetonearest0.1
Potentiograph/E-535 and Dosimat/E-459, or equivalent, have been found
mg; dissolve in water and dilute to a final volume of 1 L.
satisfactory. Available from Brinkmann Instruments Inc.
Determine the normality of the solution with the following
Evaluating Ruler EA-893, or equivalent, has been found satisfactory.Available
from Brinkmann Instruments Inc.
equation:
Metrohm-BrinkmannTitroprocessor670hasbeenfoundsatisfactory.Available
from Brinkmann Instruments Inc.
Orion Model 93.07, or equivalent, has b
...