ASTM D5806-95(2017)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5806 − 95 (Reapproved 2017)
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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers a potentiometric titration pro-
D459Terminology Relating to Soaps and Other Detergents
cedure for determining active matter in disinfectant quaternary
D1193Specification for Reagent Water
ammonium salts. This test method is intended for the analysis
D1681Test Method for SyntheticAnionicActive Ingredient
of quaternary ammonium salts used as disinfectants, and only
in Detergents by Cationic Titration Procedure
appliestothefollowingcommonlyusedquaternaryammonium
D3049Test Method for Synthetic Anionic Ingredient by
salts: n-alkyldimethylbenzylammonium chloride (see Fig. 1),
Cationic Titration
cetyltrimethylammoniumchloride,andablendof n-octyldecyl
E180Practice for Determining the Precision of ASTM
dimethylammonium chloride, di-n-octyl dimethylammonium
Methods for Analysis and Testing of Industrial and Spe-
chloride,anddi-n-decyldimethylammoniumchloride(seeFig. 3
cialty Chemicals (Withdrawn 2009)
2). Also, this test method can be applied to the analysis of
disinfectant type products where the formula ingredients are
3. Terminology
known and the quaternary ammonium salt is one of the above.
3.1 Definitions—See Terminology D459.
Interferences such as amines oxides and betaines present in
disinfectant formulations were not tested.
4. Summary of Test Method
1.2 This disinfectant quaternary ammonium salt conforms 4.1 Disinfectant type quaternary ammonium compounds
to the structures in Fig. 1 and Fig. 2. present,astheactivematerialsindisinfectanttypeproductsare
titrated potentiometrically in an aqueous medium with a
1.3 The values stated in SI units are to be regarded as
standard solution of sodium lauryl sulphate using a nitrate
standard. No other units of measurement are included in this
ion-selective electrode or a surfactant electrode (see also Test
standard.
Method D1681). In this potentiometric titration, the reaction
involves the formation of a complex between the disinfectant
1.4 This standard does not purport to address all of the
quaternary ammonium compound and the anionic surfactant
safety concerns, if any, associated with its use. It is the
which then precipitates. At the end point, the nitrate ion
responsibility of the user of this standard to establish appro-
electrode or surfactant electrode appears to respond to an
priate safety and health practices and determine the applica-
excess of titrant with a potential change large enough to give a
bility of regulatory limitations prior to use. For specific
well defined inflection in the titration curve.
precautionary information, see Section 8.
5. Significance and Use
5.1 Thistestmethodisusedtodeterminethepercentactives
in each type of the disinfectant quaternary ammonium salts,
1 2
This test method is under the jurisdiction ofASTM Committee D12 on Soaps For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
AnalysisandSpecificationsofSoaps,Synthetics,DetergentsandtheirComponents. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Jan. 1, 2017. Published February 2017. Originally the ASTM website.
approvedin1995.Lastpreviouseditionapprovedin2009asD5806-95(2009).DOI: The last approved version of this historical standard is referenced on
10.1520/D5806-95R17. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5806 − 95 (2017)
where:
−
X = chloride, and
R = aliphatic, normal C −C .
8 22
FIG. 1n-alkyldimethylbenzylammonium chloride and n-alkyldimethylethylbenzylammonium chloride
NOTE 2—Other electrodes (for example, calomel electrodes) are suit-
able 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 is suggested.
7. Reagents
where: 13
7.1 Sodium Lauryl Sulfate, primary standard (see Note 3).
−
X = chloride, and
7.2 Standardize with Hyamine 1622, dried previously at
R = aliphatic, normal C −C .
8 22
105°C for 1 h.
FIG. 2 Dialkyldimethyl quaternaries
NOTE 3—Sodium lauryl sulfate must be analyzed for purity according
to the Reagent section of Test Method D3049 before using as a primary
standard.
and also in the disinfectant products. Quaternary ammonium
7.3 Water, Type III, reagent water conforming to Specifica-
compounds being the active ingredients in disinfectant-type
tion D1193.
products require accurate determination to assess the cost and
7.4 Isopropanol, reagent grade. (Warning—Highly flam-
antimicrobial performance of such products.
mable.)
6. Apparatus
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
agent grade.
5 6
20-mL buret capacity, magnetic stirrer, evaluating ruler,
7 7.6 Boric Acid, (H BO ), reagent grade. (Warning—
3 3
titroprocessor with 10-mL buret capacity or equivalent auto-
Causes irritation.)
titration system.
8 9 7.7 Sodium Hydroxide, (NaOH), reagent grade.
6.2 Nitrate Specific Ion Electrode, or surfactant electrode,
10 (Warning—Causes severe burns on contact with skin.)
or equivalent. Silver/silver chloride reference electrode.
7.8 Sodium Hydroxide, 2N Solution—Dissolve 40 g of
6.3 Metrohm Coaxial Adaptor, required for indicator elec-
11 sodiumhydroxideinapproximately300mLofdeionizedwater
trode. Banana plug adaptor, required for reference electrode.
with stirring. Transfer to a 500-mL volumetric flask, dilute to
NOTE 1—To ensure electrical continuity (after assembly), shake down
volume with deionized water, and mix well.
electrode in the manner of a clinical thermometer.Also, the conditioning
of the electrode is essential for obtaining a good break in the titration 7.9 Borate Buffer Solution—Dissolve 1.5 g Na B O ·10
2 4 7
curve. Conditioning new electrodes in 0.004 M sodium lauryl sulfate,
H O and 1.0 g H BO in approximately 200 mL deionized
2 3 3
aqueous solution for 60 min (or more) prior to use is recommended.Also
water, with stirring; adjust pH to 9.5 with 2N HaOH, transfer
applies to the nitrate or surfactant electrode.
to a 1000-mL volumetric flask, mix and dilute to volume with
deionized water.
Metrohm-Brinkmann E-536, or equivalent, has been found satisfactory.Avail-
7.10 Octoxynol-9 Nonionic Surfactant.
able from Brinkmann Instruments Inc., Cantiague Rd., Westbury, NY 11590.
Potentiograph/E-535 and Dosimat/E-459, or equivalent, have been found
7.11 Triton Solution, 1%—Pipet 1 mL of the octoxynol-9
satisfactory. Available from Brinkmann Instruments Inc.
nonionic surfactant and transfer to a 100-mL volumetric flask
Evaluating Ruler EA-893, or equivalent, has been found satisfactory.Available
diluted to volume with deionized water.
from Brinkmann Instruments Inc.
Metrohm-BrinkmannTitrop
...