CEN/TC 276 - Surface active agents

This document sets requirements for bio-based surfactants in terms of properties, limits, application classes and test methods. It lays down the characteristics and details for assessment of bio-based surfactants as to whether they:
-   are fit for purpose in terms of performance related properties;
-   comply with the requirements regarding the health, safety and environment which apply to general surfactants;
-   are derived from a certain minimum percentage of biomass;
-   comply with at least similar sustainability criteria as comparable (non-bio-based) surfactants.
The criteria of the regulation on Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) [13] also apply to bio-based surfactants.
NOTE   EN 16575 defines the term "bio-based" as derived from biomass and clarifies that "bio-based" does not imply "biodegradable". In addition, "biodegradable" does not necessarily imply the use of "bio-based" material.

The aim of this document is to summarize the actual situation regarding many aspects regarding bio-based surfactants and their relation to any other surfactant regardless of its origin. It will describe existing raw material sources with regard to their current usage in surface active agents, their source identification and conformation, and the options for communication same.
It also includes the current work on surfactants regarding their performances, their sustainability, the LCA approaches and end of life options.

This European Standard specifies a method of preparing water of known calcium and magnesium hardness for use in testing surface active agents and products containing them.

ISO 2871-1:2010 specifies a method for the determination of high-molecular-mass cationic-active materials such as quaternary ammonium compounds in which two of the alkyl groups each contain 10 or more carbon atoms, e.g. distearyl-dimethyl-ammonium chlorides, or salts of imidazoline or 3-methylimidazoline in which long-chain acylaminoethyl and alkyl groups are substituted in the 1- and 2-positions, respectively.
The method is applicable to solids or to aqueous solutions of the active material. The method is not applicable if anionic surface active agents are present.

ISO 2871-2:2010 specifies a method for the determination of low-molecular-mass cationic-active materials such as monoamines, amine oxides, quaternary ammonium compounds and alkyl-pyridinium salts which have a main chain of 10 to 22 carbon atoms and not more than 6 other carbon atoms in the cation. The method is also suitable for other cationic-active materials.
The method is applicable to solids or to aqueous solutions of the active material. The method is not applicable if anionic and/or amphoteric surface active agents are present.

ISO 8799:2009 specifies a method for the determination of the content of unsulfated matter present in ordinary commercial neutralized products of sulfation of ethoxylated alcohols or alkylphenols [alkyl oxyethylene sulfates (ethoxylated alcohol sulfates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates)] containing an average of not more than 20 oxyethylene groups per molecule.

ISO 2870:2009 specifies a method for the determination, in detergents, of anionic-active matter hydrolyzable and non-hydrolyzable under acid conditions.
This active matter includes alkyl sulfates and hydroxysulfates and alkylphenol and fatty alcohol ethoxysulfates.

This European Standard specifies a method for the determination of the effectiveness of surface active agents to create and to stabilize a dispersion of pigment powder in water. It is applicable to all classes of surface active agents and formulations of surface active agents. The method can also be applied analogously to other powders.

This European Standard specifies a procedure for the determination of the content of free fatty acid, FFA, in alkylamidopropylbetaines, which is defined as being the amount of fatty acid expressed in grams per 100 g of product.
This method has been validated for the determination of fatty acids from C6 to C20 in a total concentration range from 0,02  g to more than 3,0 g fatty acid per 100 g of product.

This European Standard specifies a method for the determination of hydroxyl value of aliphatic and cyclic hydroxyl compounds with hydroxyl groups attached to primary and secondary carbon atoms.
This European Standard is applicable to polyacetals, temperature sensitive materials, high solids polymer polyols and rigid polyols and phenols.
This European Standard is not suitable for determination of hydroxyl groups attached to tertiary carbon atoms.
NOTE   This method is currently recommended for neutral refined products. However for products that contain an excess of acidic species a validation should be carried out to show that the acidic species either does not interfere or that the acidic species interference has been obviated.

This European Standard specifies a method for the determination of the active matter content of alkylamidobetaines in commercial surface active agents.

This European Standard specifies a method for the identifying and quantifying of high boiling point solvents in finished liquid detergents and raw materials.

This document specifies methods for the determination of the cloud point of solutions of non-ionic surface active agents obtained by the reaction of ethylene oxide with a hydrophobic base molecule.
This document primarily applies to surfactants obtained by reaction of ethylene oxide with hydrophobic base molecules, such as fatty alcohols, fatty acids, long-chain alkylphenols, fatty amines, fatty acid esters of sugar derivatives among other ethoxylated non-ionic surfactants, which are by far the most commonly used.
NOTE   Other non-ionic surfactants containing other structural units, such as propylene oxide-ethylene oxide block copolymers, have distinctive behaviours that make the determination of the cloud point more difficult. This leads sometimes to a gradual turbidity over a temperature range of several degrees or even to the occurrence of two cloud points at significantly different temperatures.

TC - Modification to 4.10

TC - Modification to 4.8
German translation received on 2006-06-07 NOT circulated as the corrigendum concerns the English text ONLY.

This European Standard specifies a method for the determination of the content of free N-(3-dimethylaminopropyl)-alkylamides (amidoamine) in alkylamidopropylbetaines, expressed in grams per 100 g of product.
This method is applicable in the range between 0,02 g and 1,0 g of amidoamine per 100 g of product.

This European Standard specifies a method for the determination of the content of inorganic sulphate in anionic surface active agents. It can be applied to a-olefin sulphonates and n-olefin sulphonates, alcohol sulphates, alcohol ether sulphates, alkyl benzene sulphonates and other alkyl sulphonates. This method is used also for the determination of inorganic sulphate in alkyl benzene sulphonates or other alkyl sulphonates in their acid form. This method also applies to deep-coloured samples.
NOTE   Sulphate can be present as sulphuric acid, ionic salts of this acid or mixture of these.

This European Standard specifies a method for the determination of the content of quaternary ammonium surface active agents in raw materials and formulated products, defined as being the amount of quaternary ammonium surface active agents expressed in millimoles per 100 g of product.
NOTE 1   The applicability in products different than those tested should be checked in each particular case.
NOTE 2   In comparison to usual laboratory two-phase titration with visual endpoint determination (see ISO 2871-1 and ISO 2871-2) potentiometric titration offers the advantage of automation, operator-dependent differences in recognising the equivalence point can be neglected, and a non-critical solvent replaces the toxicologically critical chloroform.

This European Standard specifies a method for the determination of tetraacetyl ethylene diamine (TAED) content greater than or equal to 25 g/100 g in granules.

This European Standard specifies a method for the determination of the active content and molar mass of sodium dodecyl sulphate used as original titre for the titre determination of standard solutions for surface active agents titration.
NOTE   These are used in the mixed indicator two-phase titration (e. g. ISO 2271) and in the potentiometric titration using a surface active agent sensitive electrode (e.g. EN 14480).

This European Standard specifies a method for the determination of the content of anionic surface active agents and soaps in detergents and cleansers, defined as being the amount of anionic surface active agents expressed in millimoles per 100 g of product.
NOTE 1   The applicability in products different that those tested should be checked in each particular case.
NOTE 2   In comparison to usual laboratory two-phase titration with visual endpoint determination (see ISO 2271), potentiometric titration offers the advantage of automation; operator-dependent differences in recognising the equivalence point can be neglected, and a non-critical solvent replaces the toxicologically critical chloroform.

This European standard specifies a method for the determination of the content of low boiling solvents, e. g. methanol, ethanol propan-1-ol and propan-2-ol in liquid detergents.
The method is applicable to liquid detergents containing low boiling solvents in the range from 0,5 g/100 g to 10 g/100 g.

This European Standard specifies a method for the determination of physical stability of surface active agents in alkaline and acid solutions. It is applicable to all classes of surface active agents and also to other substances or mixtures such as polymers, complexing agents and formulations of surface active agents.

This document specifies a method for the determination of foamability and degree of foamability of surface active agents by means of a circulation equipment, whereby the solution of the surface active agent is under fast circulation.
The method is applicable to many surface active agents, especially for low and medium foaming surface active agents and products containing surface active agents.

This document specifies a method for the determination of the content of anionic surface active agents in raw materials, defined as being the amount of anionic surface active agents expressed in millimoles per 100 g of product.
NOTE 1   The applicability in products different than those tested should be checked in each particular case.
NOTE 2   In comparison to usual laboratory two-phase titration with visual endpoint determination (see ISO 2271) potentiometric titration offers the advantage of automation, operator-dependent differences in recognising the equivalence point can be neglected, and a non-critical solvent replaces the toxicologically critical chloroform.

This document specifies test methods for the determination of surface tension of liquids, particularly surface active agent solutions.
The methods are suitable for determining the static surface tension of liquids, for example inorganic and organic liquids and solutions.

This European Standard specifies test methods for the determination of interfacial tension in the range from 4 mN/m to 50 mN/m between two immiscible liquids which can also be free from surface active agents.
It is particularly suitable for determining the interfacial tension between water or aqueous solutions and organic liquids which are immiscible with water.

This European Standard specifies a method for the determination of pH value of solutions or dispersions of surface active agents and gives a method for their preparation.
The method is applicable to aqueous solutions containing anionic, cationic and non-ionic surface active agents, ampholytic surface active agents and products in solution containing surface active agents.

This draft European Standard specifies a method for the determination of hydroxyl value of aliphatic and alicyclic hydroxyl compounds such as polyols, sorbitan esters, plasticisers and surface active agent alcohols and ethoxylates with hydroxyl values greater than 20 mg/g KOH.

A test portion is dissolved in ethanol and the solution is acidified. The alkane monosulfonic acids are separated from the alkane disulfonates and sulfate ions by extraction with light petroleum. The light petroleum phase is evaporated and the residue is solved in ethanol. Traces of alkali are removed by means of a cation-exchange column. The eluate is neutralized with carbonate-free sodium hydroxide solution. The sodium alkane monosulfonates so formed are dried and weighed. The mean relative molecular mass of the alkanemonosulfonates and the alkanemonosulfonate content are calculated.

This European Standard specifies a method for the determination of the solubility of ionic surface active agents in water as a function of concentration and temperature and for the determination of the Krafft point by graphical evaluation of the measurement results.
In the temperature range from 0 °C to 90 °C, the solubility is determined without any limitations if the viscosity of the solution does not exceed about 700 mPas.
At temperatures below 0 °C, determination is only possible if the solvent does not freeze.
The method is applicable both to pure surface active agents and to technical products optically clear and not unduly coloured solutions.
The solubility both of solid and liquid surface active agents and of aqueous solutions of surface active agents is determined by the method specified.

This European Standard specifies a method for the determination of dialkyl-tetralins (DAT), being 1,4-dialkyl-2,3-dihydro-naphthalene in linear alkylbenzene (LAB) in the range of the mass fraction of 0,5 % to 10 %.

This European Standard specifies the methods for the determination of primary, secondary and tertiary amino nitrogen content in surface active agents by potentiometric titration.

This European Standard specifies a method for measuring the foaming power of a surface active agent and the antifoaming power of a defoamer with regard to a foaming solution.
The method is applicable to all surface active agents and particularly to low foaming products and antifoaming surface active agents.
However, measurement of the foaming power of solutions of readily hydrolyzable agents does not give valid results, as the hydrolysis products gather in the films of liquid and affect the persistence of the foam.

TC - Modification in 4.4

This European Standard specifies the determination of the water number of ethoxylated products up to about 70 % ethylene oxide. EO/PO block polymers with water numbers higher than about 23 become hard to interpret.
NOTE   The values obtained by this method are not completely identical with the water number obtained in dioxane, in particular water numbers higher than 23.

This European Standard specifies a test method for the determination of the content of free ethylene oxide in the range from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols and in fatty acid polyglycol esters.

TC - Modification in 5.3 and Clause 8

TC - Modification in 10.2

This European Standard specifies a method for the determination of total base nitrogen content in surface-active agents by potentiometric titration.

This European Standard specifies a method for the determination of amide nitrogen content in surface active agents by potentiometric titration. It is not applicable to other basic substances.

This European Standard specifies a method for the determination of 0,02 mmol to 1 mmol of free amine in alkyl dimethyl betaines. Monochloroacetic acid, glycolic acid and strong acids do not interfere the determination.

This European Standard specifies a method for the qualitative and quantitative determination of ethylene oxide and propylene oxide groups in ethylene oxide (EO) and propylene oxide (PO) adducts, polyethers and polyglycol esters.
NOTE   If a suitable calibration is performed, methoxy groups can also be determined.

This European Standard specifies a method for the determination of the contents of non-ionic substances in anionic surface active agents (sulfates, sulfonates and ethoxysulfates) by high performance liquid chromatography (HPLC).

This European Standard specifies a test method for the determination of up to 1 milliequivalent of alkyldimethyl betaine. Monochloroacetic acid, glycolic acid, strong acids and amines do not intefere.

This European Standard specifies the Karl Fischer method using electrometric end point detection for the determination of the water content of surface active agents. The method is applicable to products in form of powders, pastes and solutions.

This European Standard specifies a gas-liquid chromatography (GLC)/head space method for the determination of 1,4-dioxane in alkyl-ethoxy-sulfate products. The method is applicable to samples containing 1,4-dioxane in the range from 5 mg/kg to 100 mg/kg.

This European Standard specifies a test method for the determination of foaming power of surface active agents diluted in water with different degree of calcium hardness and a content of surface active agent less than or equal to 1 % (m/m).

This European Standard specifies a method for determining the wetting power of a surface active agent in solution by immersion of a disc of raw cotton cloth in the solution. The method is applicable to all surface active agents, whatever their ionic character, used as wetting agents in neutral, slightly acid or slightly basic baths for textile applications. The method is not applicable to mercerizing agents (baths highly basic) or to carbonizing assistants (baths highly acid).

This European standard specifies a method for the determination of the polyethylene glycol (PEG) content in aromatic and aliphatic non-ionic surface active agents of the type R - (O - C2H4) p OH; where p is the mean ethylene oxide (EO) value. It is applicable to all ethoxylated products soluble in methanol or methanol/water mixture. This method applies to PEG concentrations as mass fraction greater than or equal to 0,1 %.