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ASTM D5806-95(2003)

(Test Method)

Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration

Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration

SIGNIFICANCE AND USE
This test method is used to determine the percent actives 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 products require accurate determination to assess the cost and antimicrobial performance of such products.
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: n-alkyldimethylbenzylammonium chloride (see Fig. 1), cetyltrimethylammonium chloride, and a blend of n-octyldecyl dimethylammonium chloride, di-n-octyl dimethylammonium chloride, and di-n-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 Fig. 1 and Fig. 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
09-Oct-1995
ICS
71.100.35 - Chemicals for industrial and domestic disinfection purposes
Technical Committee
D12 - Soaps and Other Detergents
Drafting Committee
D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components
Current Stage
Ref Project

Relations

Replaces
ASTM D5806-95 - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration
Effective Date
10-Oct-1995
Replaced By
ASTM D5806-95(2009) - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration
Effective Date
01-Oct-2009

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ASTM D5806-95(2003) - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric TitrationASTM D5806-95(2003) - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration
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ASTM D5806-95(2003) - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration
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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:D5806–95(Reapproved 2003)
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 Methods for Analysis and Testing of Industrial and Spe-
cialty Chemicals
1.1 This test method covers a potentiometric titration pro-
cedure for determining active matter in disinfectant quaternary
3. Terminology
ammonium salts. This test method is intended for the analysis
3.1 Definitions—See Terminology D459.
of quaternary ammonium salts used as disinfectants, and only
appliestothefollowingcommonlyusedquaternaryammonium
4. Summary of Test Method
salts: n-alkyldimethylbenzylammonium chloride (see Fig. 1),
4.1 Disinfectant type quaternary ammonium compounds
cetyltrimethylammoniumchloride,andablendof n-octyldecyl
present,astheactivematerialsindisinfectanttypeproductsare
dimethylammonium chloride, di-n-octyl dimethylammonium
titrated potentiometrically in an aqueous medium with a
chloride,anddi-n-decyldimethylammoniumchloride(seeFig.
standard solution of sodium lauryl sulphate using a nitrate
2). Also, this test method can be applied to the analysis of
ion-selective electrode or a surfactant electrode (see also Test
disinfectant type products where the formula ingredients are
Method D1681). In this potentiometric titration, the reaction
known and the quaternary ammonium salt is one of the above.
involves the formation of a complex between the disinfectant
Interferences such as amines oxides and betaines present in
quaternary ammonium compound and the anionic surfactant
disinfectant formulations were not tested.
which then precipitates. At the end point, the nitrate ion
1.2 This disinfectant quaternary ammonium salt conforms
electrode or surfactant electrode appears to respond to an
to the structures in Fig. 1 and Fig. 2.
excess of titrant with a potential change large enough to give a
1.3 This standard does not purport to address all of the
well defined inflection in the titration curve.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety and health practices and determine the applica-
5.1 Thistestmethodisusedtodeterminethepercentactives
bility of regulatory limitations prior to use. For specific
in each type of the disinfectant quaternary ammonium salts,
precautionary information, see Section 8.
and also in the disinfectant products. Quaternary ammonium
compounds being the active ingredients in disinfectant-type
2. Referenced Documents
products require accurate determination to assess the cost and
2.1 ASTM Standards:
antimicrobial performance of such products.
D459 Terminology Relating to Soaps and Other Detergents
D1193 Specification for Reagent Water
6. Apparatus
D1681 TestMethodforSyntheticAnionicActiveIngredient
6.1 Autotitration System, with 10-mL buret capacity, or
in Detergents by Cationic Titration Procedure
5 6
20-mL buret capacity, magnetic stirrer, evaluating ruler,
D3049 Test Method for Synthetic Anionic Ingredient by
titroprocessor with 10-mLburet capacity or equivalent autoti-
Cationic Titration
tration system.
E180 Practice for Determining the Precision of ASTM
Withdrawn. The last approved version of this historical standard is referenced
This test method is under the jurisdiction ofASTM Committee D12 on Soaps on www.astm.org.
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Metrohm-Brinkmann E-536, or equivalent, has been found satisfactory.Avail-
Analysis of Soaps and Synthetic Detergents. able from Brinkmann Instruments Inc., Cantiague Rd., Westbury, NY 11590.
Current edition approved Oct. 10, 1995. Published December 1995. DOI: Potentiograph/E-535 and Dosimat/E-459, or equivalent, have been found
10.1520/D5806-95R03. satisfactory. Available from Brinkmann Instruments Inc.
2 6
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Evaluating Ruler EA-893, or equivalent, has been found satisfactory.Available
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM from Brinkmann Instruments Inc.
Standards volume information, refer to the standard’s Document Summary page on Metrohm-BrinkmannTitroprocessor670hasbeenfoundsatisfactory.Available
the ASTM website. from Brinkmann Instruments Inc.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5806–95 (2003)
where:
−
X = chloride, and
R = aliphatic, normal C −C .
8 22
FIG. 1 n-alkyldimethylbenzylammonium chloride and n-alkyldimethylethylbenzylammonium chloride
7.3 Water, Type III, reagent water conforming to Specifica-
tion D1193.
7.4 Isopropanol, reagent grade. (Warning—Highly flam-
mable.)
7.5 Sodium Borate Decahydrate, (Na B O 10H O), re-
2 4 7 2
agent grade.
where:
7.6 Boric Acid,(H BO ), reagent grade. (Warning—
3 3
−
X = chloride, and
Causes irritation.)
R = aliphatic, normal C −C .
8 22
7.7 Sodium Hydroxide, (NaOH), reagent grade.
FIG. 2 Dialkyldimethyl quaternaries
(Warning—Causes severe burns on contact with skin.)
7.8 Sodium Hydroxide, 2N Solution—Dissolve 40 g of
6.2 Nitrate Specific Ion Electrode, or surfactant elec-
sodiumhydroxideinapproximately300mLofdeionizedwater
trode, or equivalent. Silver/silver chloride reference elec- with stirring. Transfer to a 500-mL volumetric flask, dilute to
trode.
volume with deionized water, and mix well.
6.3 Metrohm Coaxial Adaptor, required for indicator elec-
7.9 Borate Buffer Solution—Dissolve 1.5 g Na B O·10
2 4 7
trode. Banana plug adaptor, required for reference electrode.
H O and 1.0 g H BO in approximately 200 mL deionized
2 3 3
water, with stirring; adjust pH to 9.5 with 2N HaOH, transfer
NOTE 1—To ensure electrical continuity (after assembly), shake down
to a 1000-mLvolumetric flask, mix and dilute to volume with
electrode in the manner of a clinical thermometer.Also, the conditioning
deionized water.
of the electrode is essential for obtaining a good break in the titration
curve. Conditioning new electrodes in 0.004 M sodium lauryl sulfate,
7.10 Octoxynol-9 Nonionic Surfactant.
aqueous solution for 60 min (or more) prior to use is recommended.Also
7.11 Triton Solution, 1 %—Pipet 1 mL of the octoxynol-9
applies to the nitrate or surfactant electrode.
nonionic surfactant and transfer to a 100-mL volumetric flask
NOTE 2—Other electrodes (for example, calomel electrodes) are suit-
diluted to volume with deionized water.
able as the reference electrode provided they give a stable reference
−3
potential during the titration. Reference electrodes having a ceramic or an
7.12 Sodium Lauryl Sulfate Solution, 8 3 10 N—Weigh
asbestos junction tend to clog with use. Therefore, a ground-glass sleeve
accurately2.42 60.01gofsodiumlaurylsulfatetonearest0.1
electrode is suggested.
mg; dissolve in water and dilute to a final volume of 1 L.
Determine the normality of the solution with the following
7. Reagents
equation:
7.1 Sodium Lauryl Sulfate, primary standard (see Note
W 3 P
3).
Normalityofsodiumlaurylsulfate 5 (1)
~288.38! ~100!
7.2 St
...

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5.1 This test method is used to determine the percent actives 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 products require accurate determination to assess the cost and antimicrobial performance of such products.
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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: n-alkyldimethylbenzylammonium chloride (see Fig. 1), cetyltrimethylammonium chloride, and a blend of n-octyldecyl dimethylammonium chloride, di-n-octyl dimethylammonium chloride, and di-n-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.  X−  =  chloride, and    R  =  aliphatic, normal C8 − C22.    
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SIGNIFICANCE AND USE
5.1 Hand hygiene is considered one of the most important measures for preventing the spread of infectious microorganisms and is critical for reducing the incidence of food-borne disease. Food-handling settings are unique in that moderate to heavy soil load present on hands often can influence the ability of a product to remove or kill microorganisms (3, 4). Test methods are needed for assessing the efficacy of hand hygiene products under conditions representative of those encountered in a food-handling environment.  
5.2 This test method is specifically designed to evaluate the effectiveness of food-handler products to kill and remove bacteria from experimentally-contaminated hands under conditions of moderate to heavy organic soil load. The inclusion of soils typical of food service setting makes this a methodology more appropriate than Test Method E1174, which was designed to evaluate healthcare personnel hand washes and does not include an option to include soil (4).
SCOPE
1.1 This test method is designed to determine the activity of food-handler handwashes against transient bacterial flora on the hands.  
1.2 Performance of this procedure requires the knowledge of regulations pertaining to the protection of human subjects (1)2.  
1.3 This test method should be performed by persons with training in microbiology, in facilities designed and equipped for work with potentially infectious agents at biosafety level 2 (2).  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For more specific precautionary statements see 8.1.1.  
1.6 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.

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ASTM
ASTM E2011-21(Test Method)
Standard Test Method for Evaluation of Hygienic Handwash and Handrub Formulations for Virus-Eliminating Activity Using the Entire Hand

SIGNIFICANCE AND USE
5.1 This test method is designed to evaluate the virus-eliminating activity of hygienic handwash and handrub agents from experimentally-contaminated hands. Such formulations may be further assessed in a clinical trial for their effectiveness in the field. This test method incorporates whole-hand exposure and reflects actual use conditions such as friction during hand decontamination, and enables alternative product forms such as alcohol- or non-alcohol-based liquids, gels, and foams to be tested according to label directions. It is meant to extend, if required, the results of testing with Test Method E1838, which gives precise reductions in viral infectivity on a limited area of the hands. It may also serve as an alternative test method when product form is not amenable to testing by Test Method E1838.  
5.2 This test method is not meant for use with surgical hand scrubs or preoperative skin preparations.
Note 2: Application of viruses on the entire surface of both hands entails a greater risk to the subjects than using fingerpads only. Therefore, greater care is needed to ensure that the hands of the participants are free from any apparent damage. Also, virus preparations must be thoroughly screened for, or documented to be free from, extraneous or adventitious pathogens before use in such tests.
SCOPE
1.1 This test method is designed to evaluate handwash or handrub agents for their ability to reduce or eliminate viable viruses from the skin of human hands.
Note 1: A knowledge of virological techniques is required for this test method.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard may involve hazardous materials, operations and equipment. 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. The user should consult a reference for laboratory safety recommendations. (3-5)  
1.4 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.

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