ISO/TC 91 - Surface active agents

This document specifies a method for the determination of static electricity elimination (antistatic) performance. This document is applicable to fabric conditioners and antistatic agents. NOTE The differences between this document and some International Standards related to static electricity on textiles are listed in Annex B.

This document specifies a method for the simultaneous determination of the total alkali content and the total fatty matter content of soaps (including liquid soaps), excluding compounded products.

This document provides a method for the determination of alkylphenol ethoxylates (APEOs) in surfactants using high performance liquid chromatography (HPLC) and detected with diode array detector (DAD) or fluorescence detector (FLD). This method is appropriate for the detection and quantification of APEOs in surfactants.

This document provides microbiological test methods for enumeration and detection of aerobic mesophilic bacteria, detection of Escherichia coli and Pseudomonas aeruginosa in liquid hand dishwashing.

This document specifies a potentiometric method for the determination of the chloride content of soaps, containing or not containing other surface active agents, and also of compounded products.

ISO 19619:2018 specifies an analytical procedure for the determination of free propylene oxide in surfactants which are synthesized from propylene oxide copolymers. The method is appropriate for the qualitative and quantitative determination of propylene oxide groups in propylene oxide adducts, polyethers and polyglycol esters by headspace gas chromatography (HS-GC) with a flame ionization detector (FID) based on external procedure. Gas chromatography-mass spectrometry (GC-MS) is used for the confirmatory purposes.

ISO 17280:2015 provides a method for the determination of 1,4-dioxane residues in surfactants which are synthesized from epoxyethane, such as alkyl ether sulfates and alcohol ethoxylates. The method is applicable for samples containing 1,4-dioxane more than 5 mg/kg. For samples containing 1,4-dioxane more than 100 mg/kg, the sample solutions should be diluted to appropriate concentration.

ISO 16560:2015 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) n OH; where n 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 %. This International Standard is not applicable to PEG whose molar mass is lower than 400 g/mol. Monomeric ethylene glycol, diethylene glycol, triethylene glycol, and glycerol are not detected.

ISO 17283-1:2014 specifies a method for the determination of monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate) in surfactants by HPLC method. The method applies for anionic surfactants such as alkyl (phenyl) ethoxylated carboxylate (AEC) or amphoteric surfactants such as alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine. The limit of detection (LOD) is ≤0,3 µg/ml for monochloroacetic acid and ≤0,2 µg/ml for dichloroacetic acid; the limit of quantification (LOQ) is ≤1,0 µg/ml for monochloroacetic acid and ≤0,75 µg/ml for dichloroacetic acid (using a standard solution). The LOD, at 5 g of sample weight, is ≤6 mg/kg for monochloroacetic acid and ≤4 mg/kg for dichloroacetic acid; and the LOQ is ≤20 mg/kg for monochloroacetic acid and ≤15 mg/kg for dichloroacetic acid.

ISO 17293-2:2014 specifies a method for the determination of monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate) in surfactants by ion chromatographic method. The method applies for anionic surfactants such as alkyl (phenyl) ethoxylated carboxylate (AEC) or amphoteric surfactants such as alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine. The limit of detection (LOD) is ≤0,01 µg/ml for monochloroacetic acid and ≤0,05 µg/ml for dichloroacetic acid; and the limit of quantification (LOQ) is ≤0,1 µg/ml for each standard (using a standard solution). The LOD, at 1 g of sample weight, is ≤1 mg/kg for monochloroacetic acid and ≤5 mg/kg for dichloroacetic acid; and the LOQ is ≤10 mg/kg for each acid.

ISO 4317:2011 specifies two titration methods (volumetric and coulometric) using Karl Fischer reagent for the determination of the water content of surface active agents and detergents. These methods are applicable to products in the form of powders, pastes and solutions. They are applicable only if so indicated in the specific standard for each product. As alkaline compounds react with Karl Fischer reagent, the methods give values which are too high in the case of samples containing alkali metal silicates, carbonates, hydroxides or borates. Therefore, samples need to be analysed for the presence of such alkali metal salts prior to the determination of the water content.

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.

Specifies five methods of measurement. Methods A, B and C are applicable to agents derived by condensation with a lipophilic compound without oxypropylene groups. Methods D and E should be used only after agreement between the parties concerned. This second edition cancels and replaces the first edition (1975).

A cotton disc of known nature and characteristics, held in a grip, is immersed in a solution of surface active agent of known concentration. After displacement of air an penetration of the solution into the cloth, the cotton disc starts to sink. The wetting time is determined by measurement the interval between the moment of immersion of the cotton disc and the moment when it begins to sink. The wetting time is determined of two standard solutions and for each of five different concentrations and then of the surface active agent solution under test for five different concentrations. The three curves "wetting time / concentration" are plotted and compared.

A test portion of the sample is dissolved in water, the pH of the solution adjusted to 4.65 and the solution titrated against standard copper(II) sulphate solution using 1-(2-pyridylazo)-2-naphthol as indicator. Principally the method has been designed principally for determining ethylenediaminetetraacetic acid (EDTA) and it salts. Before determining other chelating agents, or determining ethylenediaminetetraacetic acid in the presence of other chelating agents, the applicability of the method should be confirmed.

A stock solution is prepared by dissolving an appropriate quantity of calcium chloride in water. The calcium content of this stock solution is determined by complexometric titration with the disodium salt of (ethylenedinitrilo)tetraacetic acid (EDTA) using a mixture of Mordant Black 11 (C.I. 14645) and methyl red as indicator. Dilute solutions of the hardness required are prepared by dilution of appropriate volumes of the stock solution.

Flow properties of a newtonian or non-newtonian test portion are determined by means of a specified rotational viscometer, which will allow, for the newtonian products, the simultaneous measurements of the shear rate at which the determination is carried out, but for the non-newtonian products, possible measurement of various apparent rates of shear used for the determination.

Specifies the following methods of analysis for the substance to be tested: measurement of pH, determination of water content, determination of free alkalinity or free acidity, determination of matter extractable by light petroleum, determination of sodium alkane sulphonates content, determination of alkane monosulphonates content, determination of sodium sulphite content, determination of sodium sulphate content, determination of sodium chloride content. In annexes a general scheme of analysis and a method for the determination of total salts content is given.

The substance is determined in a medium consisting of an aqueous and a chloroform phase by titration with a standard volumetric cationic-active solution (benzethonium- chloride) in the presence of an indicator which consists of a mixture of cationic dye (dimidium bromide) and an anionic dye (acid blue 1). The method is applicable to solids or to aqueous solutions of the active material. The relative molecular mass of the anionic active matter has to be known. The method is not applicable if cationic surface active agents are present.

A test portion is boiled under reflux with ethanol in the presence of sodium sulphate. The solution is filtrated, the filtrate evaporated, and the residue weighed. Any sodium chloride present is determined by dissolution of the residue in aqueous acetone and titration with a standard volumetric silver nitrate solution. The mass of the residue is corrected for the sodium chloride content.

Methods for the determination of the following characteristics of the test pieces after washing are specified: intrinsic greying, intrinsic yellowing, increase in organic deposit content, increase in incineration residue, overall decrease in breaking strength, decrease in breaking strength resulting from chemical degradation of cellulose due to laundering and from mechanical factors in laundering. Annexes contain the determination of increase (or decrease) in degree of whiteness and of chemical wear and further a grey scale and the measurement of reflection.

The sample is hydrolyzed by nascent hydroiodic acid. The iodine liberated is titrated with a standard volumetric sodium thiosulfate solution. The method is applicable to the analysis of polyethoxylated derivatives of primary saturated fatty alcohols, oleyl alcohol, satureted fatty acids, straight and branched chain alkylphenols. It is not applicable in the present of compounds containing sulfur or nitrogen, compounds containing oxypropylene group, aldehydes or acetals, sterols and derivatives.

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.

The determination is carried out in the following way: Decomposition of the soap by sulfuric acid and extraction of the fatty acida with light petroleum. Oxidation of the free glycerol remaining in the aqueous phase by periodic acid to formic acid and formaldehyde. On reaction with chromotropic acid, the aldehyde formed gives an absorbing compound whose absorbance is propotional to the free glycerol content. Spectrometric measurement of the absorbance at a wavelength about 571 mm.

The water in a test portion is removed by azeotropic destillation with boiling xylene or petroleum. The volume of the water collected is measured. The method is applicable to products in the form of powders having water contents greater than 5 % (m/m), and in the form of pastes ans solutions. It is not applicable to samples containing water-soluble volatile compounds, for example ethanol.

The determination is carried out in a consisting of an aqueous phase and a chloroform phase, in the presence of sodium sulfate, by titration against a standard volumetric cationic-active solution (benzethonium chloride), in the presence of an indicator consisting of a mixture of a cationic dye (dimidium bromide) and an anionic dye (acid blue 1).

By successive extraction, separation, evaporation, redissolution, and filtration through an ion-exchange resin the contents of sodium chloride, anionic-active matter, polyglycol, and polyglycol sulfate are determined. From the content of anionic surface active agent (alkylether sulfate) and the anionic surface active matter content determined by two-phase titration, the mean relative molecular mass is estimated.

A test portion is desulfonated in concentrated phosphoric acid medium and the liberated alkylbenzene is extracted with light petroleum. The mean relative molecular mass of the extracted alkylbenzene is determined chromatograhically. The mean relative molecular mass of the alkylbenzenesulfonate is calculated.

The volume of a drop of an aqueous phase formed at the end of a vertical capillary tube is measured when it detaches from the tube in contact with the organic phase. The interfacial tension between two liquid phases is obtained by balancing the weight of the drop with the interfacial tension force supporting it and applying a correction factor. Then the interfacial tension is calculated from the volume of the falling drop, the outer capillary radius, the density difference between the two liquid phases and the acceleration due to gravity.

The following requirements are specified: residue after evaporation, electrical conductivity, oxidizable matter expressed in oxygen content, absorbance at 254 nm and 1 cm cell optical path length: 0.01 units max., reactive silica content, surface tension. The corresponding methods of test are specified in an annex.

A certain number of increments is taken from the batch to be sampled. The increments are mixed to form a representative sample (bulk sample). From the representative sample a final sample is prepared by means of replicate reductions.

A given number of test pieces of control cloth and machine loads of normally soiled articles are together subjected to a given number of consecutive laundering processes. After these processes characteristic properties of the test pieces of control cloth are measured and compared with their initial values. The changes in these properties during washing should enable the causes of damage in household textile articles in the laundering process to be detected.

The determination is carried out in the following way: Measurement of the maximum force which can be exerted before the film breaks, the force being exerted vertically on a stirrup or ring, in contact with he interfacial liquid film between two immiscible liquid phases placed in a measuring cup, in order to draw up the interfacial film. The force must pass through a maximum, otherwise the measurement is not valid.

The maximum force is measured which is necessary to act vertically on a stirrup or a ring, in contact with the surface of the liquid being examined placed in a measuring cup, in order to separate it from this surface, or on a plate with an edge in contact with the surface, in order to draw up the film that has formed. The surface tension of pure liquids or other solutions can also be measured by this method.

From a test portion all ethanol-soluble matter is removed by extraction with ethanol. The solution of the ethanol-insoluble residue is treated with hydrochloric acid and evaporated to dryness. The residue is dissolved in water and the operations are repeated twice. From the solution obtained after this operations the precipitate is filtered, washed, heated to 900 °C and weighed.

From a test portion all ethanol-soluble matter is removed by extraction with ethanol. In the presence of silicates the solution of the residue is treated with hydrochloric acid and evaporated to dryness. The residue is dissolved in water and the operations are repeated twice. The last solution is filtered and in the filtrate or in the silicatefree solution of the first step the sulfates are precipitated with barium chloride. The precipitate is filtered, washed, heated at 900 degree Celsius and weighed.

Defines terms frequently used in this field. Gives, in particular, specific terms for textiles applications, dry cleaning, etc., but terms for other applications may be introduced. Annex A contains scientific terms directly related to surface phenomena and to the preparation of surface active agents and Annex B general terms non-specific to the field of surface active agents.

Covers the principal considerations for assessing products for hand dishwashing: a) the performance characteristics relevant to the successive stages of washing; b) the soiled articles required for assessing these characteristics; c) the washing processes to be employed. In dealing with the load of articles and the washing processes, a number of primary and secondary variables is listed. Methods of assessment of performance characteristics and the way in which results of tests shall be reported and interpreted are also covered.

Covers the following principal considerations for assessing products for machine dishwashing: a) the performance characteristics; b) the soiled articles required for assessing these characteristics; c) the washing processes. In dealing with the load of soiled articles and washing process, a number of primary and secondary variables is listed.

The determination is carried out by argentometric titration after decomposition of a test and separation of fatty acids by filtration. The method is applicable to soaps having a chloride content, expressed as sodium chloride, equal to or greater than 0,1 % (m/m). It cannot be applied to componounded products.

The test is carried out in the following way: Immersion in the liquor containing the agent being studied of a hank of smooth cotton held by a hook and with a load fixed on the end of it. determination of the shrinkage of the hank at different intervals of time using one of the tow pieces of apparatus described.

A 0,5 % (m/m) aqueous soap solution is prepared, and after maintaining this at testing temperature for 24 h, an aliquot portion of this solution is taken. This aliquot portion is mixed with a dilute solution of the dispersing agent (surface active agent) and subsequently with a specified volume of water of known calcium hardness. The mixture is maintained for 1 h at the testing temperature and then the calcium soap present in a aliquot portion of the lower layer is titrated with a standard volumetric solution of hydrochloric acid in the presence of bromcresol green as indicator.

A buffered acetonic solution of a test portion is titrated with a standard volumetric lead(II) nitrate solution in the presence of dithizone as indicator. The method is applicable to anionic surface active agents, containing sodium, ammonium and alkanolamine sulphates. It is not applicable to products containing other compounds such as phosphates or large amounts of chloride nor is it applicable in the presence of large amounts of salts of weak acids (for example, soaps or monoesters of sulphosuccinic acid).

From premixes containing different amounts of water and relatively constant amounts of the detergent and solvent dry cleaning solutions with the desired final concentration of detergent are prepared. The water solubilizing power of the detergent is determined by visula assesment of the optical density of the solutions, and, after adding water to those solutions that are still clear, the solubilized water content for a given concentration of detergent is determined. The water emulsifying power of the detergent is determined by observation of phase separation in the solutions, and, after adding water to those solutions in which the phases are considered not to have separated, the emulsified water content for a given concentration of the detergent is determined.

Preliminary the temperatures are determined at which solutions of known concentration change on heating from being cloudy to clear and on cooling from being clear to cloudy. Two solutions of the same concentration, one being colder and cloudy and the other being warmer and clear, are placed in a bath, controlled at a preliminary determined temperature and their appearance at temperature equilibrium is noted. The test is repeated at varying temperatures until the clear solution remains clear and cloudy solution cloudy.

The determination is carried out as follows: Potentiometric determination of the chloride or bromide ion activity of a series of solutions of cationic surface active agents the concentration of which cover the expected micellization concentration. Plotting the graph of potential as a function of the logarithm of the concentration; the c.m.c. corresponds to the singularity on this curve. The method is applicable to purified cationic surface active agents (hydrochlorides and/or hydrobromides), which are soluble in water and which have a Krafft temperature below 60 degree Celsius.