Standard ICS number:Chemical Technology>>Chemical Products>>71.100.40 Surfactants and other additives
Standard Classification Number:Chemical Industry>>Chemical Additives, Surfactants, Catalysts, Water Treatment Agents>>G72 Basic Standards and General Methods for Surfactants
Drafting unit:China Daily Chemical Industry Research Institute
Focal point unit:National Technical Committee on Standardization of Surfactants and Detergents
Proposing unit:China Light Industry Federation
Publishing department:General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China Standardization Administration of China
competent authority:China Light Industry Federation
This standard specifies the determination method of cationic active substances in surfactants and detergents. This standard is applicable to the determination of cationic active substances such as: a) mono-, di-, tri-fatty alkyl tertiary amine quaternary ammonium salts, methyl sulfate quaternary ammonium salts; b) long-chain amide ethyl and alkyl imidazolinium salts or 3-methyl imidazolinium salts; c) amine oxides and alkyl pyridinium salts. This standard is applicable to solid active substances or aqueous solutions of active substances. If the content is expressed as mass fraction, the average relative molecular mass of the cationic active substance must be known or determined in advance. This standard is not applicable to the determination in the presence of anionic or amphoteric surfactants. GB/T 5174-2004 Determination of the content of cationic active substances in surfactant detergents GB/T5174-2004 Standard download decompression password: www.bzxz.net
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ICS 71. 100. 40 National Standard of the People's Republic of China GB/T5174—2004 Replaces GB/T5174-1985 Surfactants Detergents Determination of cationic-active matter content Surface active agents--Detergents-Determination of cationic-active matter content[ISO 2871.1:1988 Surface active agents—Detergents-Determination of cationic-active matter contentPart 1: High-molecular-mass cationic-active matter, MODISO 2871.2:1990 Surface active agentsDetergents-Determination of cationic-active matter contentPart 2:Cationic-active matter of low molecular mass(between 200 and 500),MODJ 2004-03-15 Issued General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China Standardization Administration of China 2004-09-01 Implementation GB/T5174—2004 This standard is modified to adopt ISO2871.1:1988 "Determination of cationic active matter content of surfactant detergents (high molecular weight cationic active matter)" (English version) and ISO2871.2:1990 "Determination of cationic active matter content of surfactant detergents (low molecular weight (200-500) cationic active matter)" (English version). This standard replaces GB/T5174-1985 "Determination of cationic active matter in detergents by direct two-phase titration". ISO2871.1:1988 and ISO2871.2:1990 are both standards for the determination of surfactant-detergent-cationic active content, based on the same direct two-phase titration principle, using the same reagents, instruments and calculation formulas. This standard combines the two and serves as the basis for the revision of the national standard GB/T5174-1985. This standard is redrafted based on ISO2871.1:1988 and ISO2871.2:1990. According to my country's national conditions and laboratory verification, this standard has made the following technical modifications when adopting ISO2871.1:1988: the standard titration solution is placed in a burette and titrated with the cationic surfactant sample solution placed in a stoppered measuring cylinder, instead of placing the surfactant sample solution in a burette and titrating the anionic surfactant standard solution placed in a stoppered measuring cylinder in ISO2871.1:1988. The high molecular weight (700) sample is dissolved in a 1:1 isopropanol aqueous solution. This standard was revised to adopt ISO2871.1:1988 and ISO2871.2:1990. The following editorial changes were made for ease of use: a) "this international standard" was changed to "this standard"; b) the decimal point "," was replaced by the comma ","; c) the foreword of the international standard was deleted; d) 4.2.1, 4.2.2 and 4.3.1, 4.3.2 in ISO2871.2:1990 were deleted. This standard was proposed by China National Light Industry Council. This standard was approved by the General Administration of Quality Supervision, Inspection and Quarantine. This standard is under the jurisdiction of the National Surfactant Detergent Standardization Center. The drafting units of this standard are China Daily Chemical Industry Research Institute and Jiangsu Feixiang Chemical Co., Ltd. The main drafters of this standard are Zhang Baolian, Gao Xinhua and Ma Lin. This standard was first published in May 1985, and this revision is the first revision. 1 Scope Surfactants and detergents Determination of cationic active matter content This standard specifies the determination method of cationic active matter in surfactants and detergents. This standard is applicable to the determination of cationic active matter such as: a) quaternary ammonium salts of mono-, di- and tri-fatty alkyl tertiary amines, quaternary ammonium salts of methyl sulfate; b) imidazolinium salts or 3-methylimidazolinium salts of long-chain amide ethyl and alkyl; c) amine oxides and alkyl pyridinium salts. GB/T5174—2004 This standard is applicable to solid active matter or aqueous solution of active matter. If its content is expressed as mass fraction, the average relative molecular mass of the cationic active matter must be known or determined in advance. This standard is not applicable to the determination in the presence of anionic or amphoteric surfactants. Note: Relatively low molecular weight toluene sulfonates and xylene sulfonates present as cosolvents do not cause interference when their concentration (mass fraction) relative to the active matter is less than or equal to 15%. If the concentration is higher, its influence needs to be considered. Nonionic surfactants, soap, urea and ethylenediaminetetraacetate do not interfere. Typical inorganic components of detergent formulations, such as sodium chloride, sodium sulfate, sodium tripolyphosphate, sodium borate, sodium perborate, sodium silicate, etc., do not interfere. However, other bleaching agents other than perborate should be pre-destroyed before analysis. 2 Normative references The clauses in the following documents become clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties to an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version applies to this standard. GB/T5173--1995 Determination of anionic active substances in surfactants and detergents Direct two-phase titration method (eqvISO2271:1989) GB/T13173.1 Detergent sample splitting method (eqvISO607:1980)3 Principle In a two-phase (water-chloroform) system with a mixed indicator of cationic dye and anionic dye, a standard anionic surfactant solution is used to titrate the cationic active substances in the sample. The cationic surfactant in the sample initially reacts with the anionic dye to form a salt and dissolves in the chloroform layer, making it blue. During the titration, the anionic surfactant replaces the anionic dye and forms a salt with the cationic dye at the end point, making the chloroform layer light gray-pink. 4 Reagents Unless otherwise specified, only reagents confirmed as analytically pure and distilled water or deionized water or water of equivalent purity are used in the analysis. 4.1 Chloroform (GB/T682); 4.2 Isosorbide-5-Nitrae-Glycol HG/T2892—1997; 4.3 Sodium lauryl sulfate c(Ci2H2sSO,Na)=0.004mol/L standard titration solution, prepared according to 4.5 of GB/T5173--1995; 4.4 Mixed indicator solution, prepared according to 4.8 of GB/T5173--1995. 5 Instruments Ordinary laboratory instruments and GB/T5174—2004 Stopper, 100mL; 5.2 Stoppered burette, 25mL; 5.3 Single-scale volumetric flask, 1000mL; Pipette, 25mL. 6 Sample preparation Laboratory samples of detergents should be prepared and stored in accordance with the provisions of GB/T13173.1. 7 Analysis steps 7.1 Test portion Weigh the laboratory sample containing 0.002mol~0.004mol of cationic active substances to the nearest 0.001g. The sample concentration should be prepared based on the volume of 10mL~20mL of the standard titration solution consumed. Table 1 calculated based on the relative molecular mass of 360 is for reference. Table 1 Test portion mass guide Expected cationic active substance content (mass fraction)/%10 7.2 Determination Test portion mass/g 7.2.1 For low molecular weight (200~~500) samples, dissolve the test portion (7.1) in water and make up to 1000mL (test solution A). 7.2.2 For high molecular weight (500-700) samples, dissolve the test portion (7.1) in 20 mL of isopropanol (4.2), heating if necessary. Add about 50 mL of water and stir to dissolve. Transfer to a 1000 mL single-scale volumetric flask (5.3), dilute to the mark with water, and mix well (test solution A). 7.2.3 For high molecular weight (>700) samples, dissolve the test portion (7.1) Dissolve with 1:1 isopropanol aqueous solution, heat to dissolve if necessary, transfer to a 1000mL single-scale volumetric flask (5.3), dilute to scale with 1:1 isopropanol aqueous solution, and mix well (test solution A). Use a pipette (5.4) to transfer 25.0mL of test solution A to a 100mL stoppered measuring cylinder (5.1). Add 10mL of water, 15mL of chloroform (4.1), and 10mL of mixed indicator solution (4.4) to the measuring cylinder respectively, and mix well. Fill the burette (5.2) with sodium lauryl sulfate standard titration solution (4.3) and start titration. After each drop, add a stopper and shake thoroughly. When approaching the endpoint, the emulsion formed by shaking is very easy to break. Continue to titrate drop by drop and shake vigorously repeatedly until the blue color fades and the chloroform layer is light gray-pink, which means the endpoint has been reached. Record the volume of sodium lauryl sulfate standard titration solution (4.3) consumed in the titration. 8 Result expression Cationic active matter content, expressed as mass fraction X, calculated according to formula (1). X(%) = VXcXM, × 100 mo×25×1000 Wherein: 4×V×c×M, V-~-volume of sodium lauryl sulfate standard titration solution (4.3) consumed, mL; concentration of sodium lauryl sulfate standard titration solution (4.3), mol/L; M, average relative molecular mass of cationic active matter; mo-mass of test portion (7.1), g. ·(1) The arithmetic mean of the results of two parallel determinations is expressed to one decimal place as the determination result. 9 Precisionwww.bzxz.net 9. 1 Repeatability GB/T5174—2004 The absolute difference between two independent test results obtained under repeatability conditions shall not exceed 1.5% of the arithmetic mean of the two measured values, provided that the difference does not exceed 5% when it exceeds 1.5%. 9.2 Reproducibility The absolute difference between two independent test results obtained under reproducibility conditions shall not exceed 3% of the arithmetic mean of the two measured values, provided that the difference does not exceed 5% when it exceeds 3%. 10 Test report The test report shall include the following: a) All information required to fully identify the sample, b) The method used; The results and the expression method used; Any abnormal phenomena occurring during the measurement process; All operating details not included in this standard or optional; Test date. 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