GB/T 38732-2020Surface active agents - Test methods of technical alkane sulfonates (English PDF)

Foreword

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

This standard uses the redrafting method to amend and adopt ISO 893.1989 "Analytical Method for Surfactant Industrial Alkyl Sulfonate".

Compared with ISO 893.1989, the structure of this standard is adjusted as follows.

---Chapter 3 of ISO 893.1989 is deleted;

--- Added Chapter 3 "Terms and Definitions";

--- Chapter 5 corresponds to 5.1 of ISO 893.1989;

--- Chapter 6 corresponds to 5.2 of ISO 893.1989;

--- Chapter 7 corresponds to 5.3 of ISO 893.1989;

--- Chapter 8 corresponds to 5.4 of ISO 893.1989;

--- Chapter 9 corresponds to 5.5 of ISO 893.1989;

--- Chapter 10 corresponds to 5.6 of ISO 893.1989;

--- Chapter 11 corresponds to 5.7 of ISO 893.1989;

--- Chapter 12 corresponds to 5.8 of ISO 893.1989;

--- Chapter 13 corresponds to 5.9 of ISO 893.1989;

--- Chapter 14 corresponds to Chapter 6 of ISO 893.1989.

The technical differences between this standard and ISO 893.1989 and the reasons are as follows.

---Regarding normative reference documents, this standard has made adjustments with technical differences to adapt to my country's technical conditions and adjustments.

The situation is collectively reflected in Chapter 2 "Normative Reference Documents", and the specific adjustments are as follows.

* Added reference to GB/T 3050 (see Chapter 13);

* Replace ISO 4314.1977 (see Chapter 7) with GB/T 6365 which is equivalent to the international standard;

* Replace ISO 6844.1983 (see Chapter 12) with GB/T 6366 modified to adopt international standards;

* Replace ISO 4316.1977 (see Chapter 5) with GB/T 6368 which is equivalent to the international standard;

* Replace ISO 4317.1977 (see Chapter 6) with GB/T 11275 modified to adopt international standards;

* Replace ISO 6122.1978 (see Chapter 9) with GB/T 11987 which is equivalent to the international standard;

* Replace ISO 6121.1988 (see Chapter 10) with GB/T 20199 modified to adopt international standards;

* Replace ISO 607.1980 (see 4.1) with GB/T 13173 equivalent to the international standard;

* Replace ISO 1104.1977 with GB/T 11989-2020, which is modified to adopt international standards (see Chapter 8, Chapter 11 and

B.5.1);

* The normative reference documents ISO 894.1977, ISO 4318.1989 and ISO 6845.1989 are deleted;

---Due to the duplication of content, the content of Chapter 3 of ISO 893.1989 is deleted;

---In order to adapt to the use of our country, the determination of water content has been modified (see Chapter 6);

---In order to adapt to the use situation in my country, the determination of alkane monosulfonate content has been modified (see Chapter 10);

--- In order to adapt to the use of our country, the determination of sodium chloride content has been modified (see Chapter 13).

This standard also made the following editorial changes.

---Modified the standard name;

---Edited the content of Chapter 1 of ISO 893.1989 and added a note.

This standard was proposed by the China National Light Industry Council.

This standard is under the jurisdiction of the National Standardization Technical Committee for Surfactants and Detergents (SAC/TC272).

Drafting organizations of this standard. China Daily Chemical Research Institute Co., Ltd. [National Detergent Products Quality Supervision and Inspection Center (Taiyuan)], Shenzhen

Bagemei Biotechnology Co., Ltd., Blue Moon (China) Co., Ltd., Surfactant and Detergent Industry Productivity Promotion Center, Xiamen Hu

Per Day Chemical Technology Co., Ltd., Dongguan Intermediate New Materials Research Institute Co., Ltd.

1 Scope

This standard specifies the pH value, water content, free alkali or free acid, petroleum ether extractables, total

Test methods for alkane sulfonate, alkane monosulfonate content, sulfite, sulfate, chloride content and other indicators.

This standard applies to powder, slurry and liquid industrial alkyl sulfonates (excluding any products that have nothing to do with the preparation).

Note. The industrial alkyl sulfonate in this standard refers to the base of monosulfonic acid or disulfonic acid prepared by sulfochlorination and sulfooxidation of linear alkyl groups without branched compounds.

Metal salt.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article

Pieces. For undated references, the latest version (including all amendments) applies to this document.

GB/T 3050 General method for determination of chloride content in inorganic chemical products Potentiometric titration (GB/T 3050-2000, neq

ISO 6227.1982)

GB/T 6365 Surfactant free alkalinity or free acidity determination titration method (GB/T 6365-2006, ISO 4314.

1977, IDT)

GB/T 6366 Surfactant inorganic sulfate content determination titration method (GB/T 6366-2012, ISO 6844.1983,

MOD)

GB/T 6368 Potentiometric method for determination of pH value of aqueous surfactant solution (GB/T 6368-2008, ISO 4316.1977,

IDT)

GB/T 11275 Determination of Water Content of Surfactants (GB/T 11275-2007, ISO 4317.1991, MOD)

GB/T 11987 Determination of total alkane sulfonate content in industrial alkane sulfonate of surfactants (GB/T 11987-1989,

eqvISO 6122.1978)

GB/T 13173 Test method for surfactant detergent (GB/T 13173-2008, ISO 607.1980, IDT)

GB/T 20199 Surface active agent industry alkane sulfonate alkane monosulfonate content determination (direct two-phase titration)

(GB/T 20199-2006, ISO 6121.1988, MOD)

GB/T 11989-2020 Industrial sodium alkylaryl sulfonate (excluding benzene derivatives) test method for surfactants (ISO 1104.

1977, MOD)

3 Terms and definitions

The following terms and definitions apply to this document.

3.1

Laboratory samples

Samples prepared in order to be sent to the laboratory for inspection or testing.

3.2

Test sample

Manufactured from laboratory samples, from which test parts can be directly weighed.

3.3

Free base or free acid

The alkalinity or acidity measured with phenolphthalein as an indicator.

Note. Depending on the situation, it can be expressed as "base value" or "acid value", that is, the number of milligrams of potassium hydroxide present in 1g of product, or the potassium hydroxide required to neutralize 1g of product

Milligrams.

3.4

Total salt content

The sum of the content of all alkali metal salts in the original product, namely alkali metal chloride, alkali metal sulfide, alkali metal sulfite and total alkane sulfonate

The sum of acid salts.

4 Divide the sample

Note. The samples need to be divided for the following reasons.

a) Prepare a final sample or laboratory sample of more than 250g from a mixed bulk sample of more than 500g;

b) Prepare several equal laboratory samples, reference samples and preserved samples from the final sample, and each sample has a mass of more than 250g;

c) Prepare test samples from laboratory samples.

5 Determination of pH

According to the method specified in GB/T 6368, the determination is made with a 5% (mass fraction) solution of laboratory samples.

6 Determination of water content

According to the method specified in GB/T 11275, according to the different water content in the sample, use one of the following two methods for determination.

a) Karl Fischer method, suitable for products with a moisture content of less than 10%;

b) The azeotropic distillation method is only suitable for products with water content greater than 5%.

7 Determination of free base or free acid

Determined according to the method specified in GB/T 6365.

8 Determination of extractable content of petroleum ether

Weigh about 80g (accurate to 0.05g) of the diluted sample (4.2), and measure it according to the method specified in Appendix A of GB/T 11989-2020.

The combined alcohol solution L1 (see Appendix A) can be used to determine the total salt content (see Appendix B); this determination can be used to check the original product

Measured result of extractable content in petroleum ether.

9 Determination of total alkane sulfonate content

Determined according to the method specified in GB/T 11987 to check the results obtained in Appendix B.

10 Determination of alkane monosulfonate content

Determined according to the method specified in GB/T 20199.

11 Determination of sulfite content

Weigh 10g (accurate to 0.001g) laboratory sample (4.1), and measure it according to the method specified in GB/T 11989-2020 Appendix D.

12 Determination of sulfate content

Determined according to the method specified in GB/T 6366.

13 Determination of sodium chloride content

Weigh 4g~5g (weigh to 0.001g) of the diluted sample (4.2), and measure it according to the method specified in GB/T 3050.

14 Test report

The test result report should include the following.

a) All the information needed to fully identify the sample;

b) The test method used (No. of this standard);

c) Results and presentation methods used;

d) Any operation details not specified or optional in this standard, and any circumstances that will affect the results.

Appendix A

Appendix B

(Informative appendix)

Determination of total salt content

B.1 Overview

When it is necessary to check the analysis results obtained according to the methods specified in Chapter 8 and Chapter 9, the following formula can be used.

Total alkane sulfonate content = total salt content-alkali metal chloride content, alkali metal sulfate content, alkali metal sulfite content () (B.1)

Petroleum ether extract content=100-(total salt content and water content) (B.2)

The total salt content in the formula refers to the sum of all alkali metal salt content in the original product, namely alkali metal chloride, alkali metal sulfate, and alkali metal sulfide

The sum of acid salt and total alkane sulfonate.

In view of the fact that petroleum ether extractables may contain volatiles, the direct measurement method specified in Chapter 8 will cause the loss of volatiles.

In doubt, it is best to use formula (B.2) to calculate the petroleum ether extractables content.

B.2 Principle

Evaporate the test portion (B.4.1) of the alcohol aqueous solution L1 obtained by the method specified in Chapter 8 to dryness, dry the residue at 130°C and weigh it.

B.3 Apparatus

Common laboratory equipment and the following items.

B.3.1 Crystal dish, diameter 50mm, capacity 100mL.

B.3.2 Pipette, 25mL.

B.3.3 Oven, the temperature can be controlled at 130 degrees C~135 degrees C.

B.4 Test procedure

B.4.1 Test parts

To two crystallizing dishes (B.3.1) which are pre-dried, cooled and weighed (weighed to 0.001g) in an oven (B.3.3) at 130 degrees C~135 degrees C

In, use a pipette (B.3.2) to transfer 25.0mL of the alcohol aqueous solution L1 obtained by the method specified in Chapter 8.

B.4.2 Determination

Evaporate the test portion (B.4.1) in the crystallization dish on a water bath to dryness. Transfer the evaporating dish to a 130 degrees C~135 degrees C oven (B.3.3), dry

Dry to constant weight (that is, the difference between two consecutive weighings with an interval of 30 minutes, not more than 5 mg).

B.5 Results presentation

B.5.1 Calculation method

The total salt content X in the raw materials is expressed in mass fraction and calculated according to formula (B.3).

Need to consider the sodium chloride used for demulsification (see GB/T 11989-2020 Appendix A), and subtract the corresponding mass from m2 and m3

The quality of sodium chloride.

B.5.2 Reproducibility

For the same sample, the difference between the results obtained in the two laboratories does not exceed 0.4%.