GB/T 13173-2021Surface active agents - Test methods for detergents (English PDF)

Foreword

This standard is drafted in accordance with the rules given in GB/T 1.1-2009.

This standard replaces GB/T 13173-2008 Surface active agents - Detergents - Testing

methods. The following main technical changes have been made with respect to GB/T

13173-2008.

-- The sample reduction method of block sample is added (see 4.2.4);

-- The specimen treatment of phosphorus molybdenum blue colorimetry in the

determination of total phosphorus oxide content is modified (see 6.2.4.2; 6.2.4.2

of Edition 2008);

-- The extraction of ethanol solution in the determination of total active substance

content is modified (see 7.4.1.1; 7.5.1.1 of Edition 2008);

-- The procedure of determining sodium oxide in the determination of total active

substance content is modified (see 7.4.1.2; 7.5.1.2 of Edition 2008);

-- The application of mixed bed resin in the determination of non-ionic surface active

agent content is added (see 8.2.1.3 and 8.4.1.3);

-- The relative foaming power determination in the determination of foaming power is added (see 11.7);

-- The determination of relative enzyme activity or content of protease is deleted (see Clause 18 of Edition 2008);

-- The determination of alkylphenol ethoxylates content in detergents is added (see Clause 18);

-- The determination of free alkali content in detergents is added (see Clause 20);

-- The determination of dry sodium soap content in detergents is added (see Clause 21);

-- The determination of high and low temperature stability of detergents is added (see Clause 22);

-- The determination of odour is added (see Clause 23);

-- The determination of colour and appearance is added (see Clause 24);

-- The informative annex "Identification test of alkylphenol ethoxylates" is added (see Annex C).

This standard has been redrafted and modified in relation to ISO 607.1980 Surface

active agents and detergents -- Methods of sample division, ISO 697.1981 Surface

active agents -- Washing powders -- Determination of apparent density -- Method by

measuring the mass of a given volume, ISO 4313.1976 Washing powders --

Determination of total phosphorus oxide content -- Quinoline phosphomolybdate

gravimetric method, ISO 4321.1977 Washing powders -- Determination of active

oxygen content -- Titrimetric method, ISO 4325.1990 Soaps and detergents --

Determination of chelating agent content -- Titrimetric method, and ISO 21264.2019

Surface active agents -- Detergents -- Determination of alkylphenol ethoxylates.

This standard is changed largely in terms of structure due to the integration of several

international standards; the comparison between this standard and the international

standards in clause/subclause number is listed in Annex A.

Technical differences have been made in this standard with respect to the above

international standards, and relevant technical differences and their causes have been

listed in Annex B.

This standard was proposed by China National Light Industry Council.

This standard shall be under the jurisdiction of the National Technical Committee on

Surfactant and Detergent of Standardization Administration of China (SAC/TC 272).

The drafting organizations of this standard. China Daily Chemical Research Institute

Co., Ltd., Shanghai Kaimi Technology Co., Ltd., Blue Moon (China) Co., Ltd.,

Unilever (China) Co., Ltd., Shenzhen Bagmei Biotechnology Co., Ltd., Zhejiang Keli

Technology Co., Ltd., Xiamen Amber Daily Chemical Co., Ltd. Technology Co., Ltd.,

South China University of Technology.

1 Scope

This standard describes the test methods for indexes of surface active agents and

detergents, such as sample reduction, particle size, total phosphorus oxide content, total

active substance content, non-ionic surface active agent content, various phosphate

content, toluenesulfonate content, foaming power, chelating agent (EDTA) content,

apparent density, whiteness, moisture and volatile matter content, active oxygen content,

4A zeolite content, alkylphenol ethoxylates content, effective chlorine content, free

alkali content, dry sodium soap content, stability at high and low temperature, odour,

colour and appearance, etc.

2 Normative references

The following referenced documents are indispensable for the application of this

document. For dated references, only the edition cited applies. For undated references,

the latest edition of the referenced document (including any amendments) applies.

GB/T 6003.1 Test sieves -- Technical requirements and testing -- Part 1.Test

sieves of metal wire cloth (GB/T 6003.1-2012, ISO 3310-1.2000,

MOD)

GB/T 6682 Water for analytical laboratory use -- Specification and test

methods (GB/T 6682-2008, ISO 3696.1987, MOD)

JJG 512 Whiteness meters

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.

3.1

surface active agents

The surface-active compound that dissolves in liquids, especially in water, and has a

significant reduction in surface or interfacial tension due to preferential adsorption on

liquid/gas surfaces or other interfaces

3.2

detergent

The specially prepared product that is used for cleaning in the process of cleaning

4 Reduction of sample

Reduction of a bulk sample by a mechanical process until a reduced sample is obtained.

The sample reduction process may be required for the following reasons.

The procedure specified is applicable to powders, including spray-dried powders, and

particularly, those that contain additives that have been introduced after the drying

process.

5 Determination of particle size of powdered detergents

The specimen is sieved by a mechanical oscillator through a sieve with a specified pore

size, and the mass of the specimen left on the sieve and in the tray is weighed

respectively, expressed as a percentage of the specimen.

Test sieve, of sieve frame diameter D=200 mm, complying with the requirements of GB/T

6 Determination of total phosphorus oxide content in detergents

Hydrolysis of polyphosphates by nitric acid. Precipitation of phosphates in the form of

quinoline phosphomolybdate in acetone solution. Drying and weighing of the precipitate.

After the specimen solution is filtered out of water-insoluble substances such as

pyrophyllite, the remaining polyphosphate is hydrolyzed into orthophosphate in

inorganic acid, and phosphorus molybdenum blue is formed with ammonium

molybdate in the presence of reducing agent.

7 Determination of total active substance content in detergents

Extract the specimen with ethanol; filter and separate it; quantify the ethanol solute and

sodium chloride in it. The total active substance content in product is obtained by

subtracting the content of sodium chloride in ethanol solute from the content of ethanol

solute. When it is necessary to deduct water cosolvent from the total active substance,

it can be obtained by further extracting the quantified ethanol soluble substance with

chloroform and then deducting the chloroform insoluble substance.

8 Determination of non-ionic surface active agent content in detergents

Anion exchange resin and cation exchange resin are used to exchange ion with ionic

surface active agents, so that it remains on the ion exchange column, while non-ionic

surface active agent is not exchanged and flows out with solvent. After distilling the

solvent, the content of non-ionic surface active agent is determined by gravimetric

method.

9 Separation determination of various phosphates content in detergents

After injecting the specimen solution into anion exchange resin column, first elute the

cation and non-ionic surface active agents with water; then elute with potassium

chloride solution with increasing concentration in turn to separate orthophosphate,

pyrophosphate, tripolyphosphate, trimetaphosphate and polyphosphate, which are

determined by phosphorus molybdenum blue colorimetry after hydrolyzed.

10 Determination of toluene sulfonate content in detergents

The soluble organic matter and surface active agents are extracted from the detergent

sample by ethanol dissolution method, and the ethanol is evaporated to dryness. The

surface active agents in the residue are separated by ethyl ether/aqueous solution

extraction method, and the content of toluene sulfonic in the aqueous phase is

determined by UV absorption method (at the characteristic absorption wavelength).

11 Determination of foaming power for synthetic detergents

The sample is prepared into a certain concentration of test solution with water of certain

hardness. Under certain temperature conditions, the 200 mL test solution flows from 90

cm height to the bottom 50 mL of the graduated cylinder, and the height of the foam

measured is the foaming power of the sample.

12 Determination of EDTA content in detergents

Adjust the pH of the sample solution to about 4.6 with hydrochloric acid solution; use

1-(2-pyridylazo)-2-naphthol as indicator to titrate the chelating agent with copper

sulfate standard solution; calculate the content of chelating agent in the specimen with

ethylene diamine tetraacetic acid (EDTA) or its sodium salt.

13 Determination of apparent density of powdered detergent

Under the specified conditions, drain the specimen from a funnel with the specified

shape, fill a receiver with a known volume, then determine the mass of the powder.

The apparent density of powder may be evaluated by the mass of powder occupying a

certain volume or the volume occupied by a certain mass of powder. In both forms, the

process of transferring the powder from the original container to the measuring

container is included.

14 Determination of whiteness of powdered detergents

Irradiate the detergent using whiteness meter with D65 light source; calibrate the

whiteness meter with standard whiteboard; measure the three stimulus values X, Y and

Z of the specimen; and calculate the whiteness according to Ganz whiteness equation.

15 Determination of moisture and volatile content in detergents

Measure the content of water and volatile matter in the sample according to the mass

loss of the specimen after drying at a certain temperature.

16 Determination of active oxygen content in detergents

The hydrogen peroxide and potassium permanganate, released from the aqueous

solution of peroxyhydrate, are co-reduced in the acidic solution, accompanied by the

release of oxygen.

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