4.1 This test method determines anionic detergents commonly found in laundry, dishwashing, and other cleaning materials. Accurate determination of the anionic active substance is highly important in assessing the cost and effectiveness of such cleaning substances.1.1 Direct titration of an anionic surfactant with a standardized cationic reagent is a simple and convenient method for the quantitative determination of the content of active ingredient. The end point is detffected by the transfer of a colored complex from an organic solvent phase to an aqueous phase. The relationship between anionic and cationic agents is not always stoichiometric, and for maximum accuracy the anionic type of interest should first be characterized and then used to standardize the cationic reagent. In most cases, however, the different anionic surfactants likely to be encountered react in the same proportions. That is, a cationic titrating solution standardized against a characterized anionic agent can be used to analyze other anionics of known molecular weights.1.2 This test method is applicable to alkylaryl sulfonates and fatty alkyl sulfates. Low results are obtained with alkylbenzene sulfonates having the alkyl chain length less than eight carbon atoms. Low results are also obtained for alkyl sulfates with the alkyl chain length of less than twelve carbon atoms. The anionic surfactants characterized in accordance with Sections 17 – 23 should be the sodium salt and not amine, ammonium, or potassium salts. In case only amine or ammonium salts are available, they should be first converted to the sodium salt before proceeding with this analysis.1.3 The analytical procedures appear in the following order:  SectionsSeparation of Alcohol-Soluble Matter 8 and 9Separation of Oil-Free Sulfonate 10 and 11Determination of Sodium Chloride (NaCl) Content 12 – 17Characterization of Anionic Surfactant Standard:   Part I. Determination of Surfactant, SO3 Content, and Solution  Molarity 18 – 20 Part II. Determination of Surfactant, SO3 and Active Ingredient  Contents Combining Weight, and Solution Molarity 21 – 24Standardization of Cationic Reagent 25 – 29Quantitative Determination of Anionic Surfactant by Cationic   Titration 30 – 331.4 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 and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazards statement, see Section 7.

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5.1 In the power-generation industry, high-purity water is used to reduce corrosion from anions, such as sulfate, chloride, and fluoride. These anions are known to be detrimental to materials of construction used in steam generators, reactor vessel internals and recirculation piping, heat exchangers, connective piping, and turbines. Most electric generating plants try to control these anions to <1.0 μg/L in the steam generator feed water. Some nuclear power plants have been able to control anion contaminants at less than 0.02 μg/L.5.2 These anions and others cause low product yields in semiconductor manufacturing. They are also monitored and controlled at similarly low levels as in the electric power industry.5.3 Low molecular weight organic acids (acetate, formate, propionate) have been detected in steam generator feed water. These low molecular weight organic materials are believed to be high-temperature degradation products of chemicals used to control cycle water pH and organic contaminants in cycle makeup water.5.4 In the semiconductor industry, anion contaminants may come from the breakdown of low molecular weight organic materials by ultraviolet light radiation, which is frequently used to produce bacteria-free water. These organic compounds may also contribute to low product yield.5.5 The production of high-purity water for process makeup and use frequently employs the use of demineralizers to remove unwanted anion contaminants. Also in the electric power industry, demineralizers are used in the process stream to maintain low levels of these contaminants. As such, it is important to monitor this process to ensure that water quality standards are being met. These processes can be monitored for the above-mentioned anions.5.6 On-line measurements of these contaminants provide a greater degree of protection of the processes by allowing for frequent on-line measurement of these species. Early detection of contaminant ingress allows for quicker corrective action to locate, reduce, or eliminate, or combination thereof, the source. Grab samples will not provide the same level of protection because of their intermittent nature and the longer time required to obtain and then analyze the sample.5.7 Additionally, on-line monitoring significantly reduces the potential for contamination of high-purity water samples, a significant problem when sampling and testing high-purity water.1.1 This test method covers on-line analysis of high-purity water by the ion chromatography technique. This test method is applicable for measuring various anionic contaminants in high-purity water, typically in the range of 0.01 to 100 μg/L. This test method is used to determine the concentration of acetate, formate, chloride, fluoride, phosphate, nitrate, and sulfate in a continuously flowing sample. The range of the test method is only as good as the reagent water available for preparing standards. At extremely low concentrations, <1.0 μg/L, preparing standards is difficult, and extra care must be taken in their preparation. The sample may have to be conditioned from higher pressures and temperatures to conditions that are suitable for use by on-line instruments.1.2 Online sample analysis of flowing streams does not lend itself to collaborative studies due to the nature of the sample and the possibility of contamination that may result from handling the sample as part of the collaborative study. Therefore this standard test method is not based on the results of a collaborative study but is intended to provide the best possible guidance for doing this type of analysis.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 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.

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5.1 Anionic surfactants are the most widely used of the synthetic detergents. ASTM methods in current use for their determination involve two-phase aqueous/chloroform titrations with the organic dyes methylene blue (Test Method D1681) or disulphine blue/dimidium bromide (Test Method D3049) as indicators. One advantage of the potentiometric method is that it eliminates the use of chloroform whose use is restricted for environmental and toxicological reasons.5.2 This test method is intended for use as described in 1.1.1.1 This test method describes a potentiometric titration procedure for determining the anionic active matter in detergents. It is intended for the analysis of anionic surfactants such as detergent range alkylbenzenesulfonates, α-olefin sulfonates, alcohol sulfates, and alcohol ethosulfates. It has not been tested for surfactant formulations.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 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. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.(A) Methylene blue method.(B) Mixed indicator method.

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4.1 This test method offers a means of determining anionic detergents commonly found in laundry, dishwashing, and other cleaning materials. Accurate determination of the anionic active substance is highly important in assessing the cost and effectiveness of such cleaning substances.4.2 This test method is not affected by low molecular weight sulfonates, such as those of toluene and xylene commonly found in detergent formulations, when these substances are present up to 15 weight % of active material.1.1 This test method covers the determination of the amount of synthetic anionic ingredient in a surfactant by direct titration with a standardized cationic reagent. The test method is a simple and convenient means for the quantitative estimation of the anionic material. The end point is detected by the transfer of a colored complex from an organic solvent phase to an aqueous phase. The colored complex is formed by the addition of a solution of dye to a solution of the anionic surfactant. This complex is soluble in the organic-solvent phase and insoluble in the aqueous phase. When this solution is titrated with a standardized solution of a cationic reagent, the dye is displaced from the colored complex and, being water-soluble, migrates to the aqueous phase. Therefore, a cationic titrating solution that has been standardized against a characterized anionic agent can be used to analyze for other anionics of known molecular mass.1.2 This test method is applicable to alkylaryl sulfonates, alkyl sulfonates, alkyl sulfates and hydroxy-sulfates, alkylphenol- and fatty alcohol ethoxy-sulfates and dialkylsulfosuccinates. It applies to active materials containing one hydrophilic group per molecule.1.3 The analytical procedures appear in the following order:  SectionsReagents 6 Primary Standard 8  Purity 8.2 Alcohols 8.3 Free Acid or Alkali 8.4Preparation of Mixed Indicator Solution 9 Preparation of Hyamine Solution 10 Standardization of Hyamine Solution 11 General Procedure for Anionic-Active Material 12 1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.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 and health practices and determine the applicability of regulatory limitations prior to use. A precautionary statement appears in Section 7. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.

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5.1 The most common anionic surfactants presented in this test method are used widely in synthetic detergents and other household cleaners. Current analysis of the active matter in these anionic surfactants involves the two-phase aqueous/chloroform titration with a mixed indicator, organic dyes such as disulphine blue/dimidium bromide (see Test Method D3049), and methylene blue (see Test Method D1681). This test method eliminates the use of hazardous chloroform, the use of which is restricted for environmental and toxicological reasons.5.2 This test method also describes the titration of various ratio blends of sodium alkylbenzene sulfonate and sodium xylene sulfonate. Active matter content in these blends is attributable directly to sodium alkylbenzene sulfonate. Therefore, the presence of various amounts of sodium xylene sulfonate in these blends does not interfere with the determination of percent actives.1.1 This test method is based on a potentiometric titration of common anionic surfactants and blends of anionic surfactant with a hydrotrope. This test method solely is intended for the analysis of active matter in the following surfactants: alcohol ether sulfate, alpha olefin sulfonate, alkylbenzene sulfonic acid, alcohol sulfate, sodium alkylbenzene sulfonate/sodium xylene sulfonate blend (5:1), sodium alkylbenzene sulfonate/sodium xylene sulfonate blend (16:1), and sodium alkylbenzene sulfonate/sodium xylene sulfonate blend (22:1). It has not been tested for surfactant formulations.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 does not purport to address all 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. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.

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