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GB/T 38729-2020 English PDF

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GB/T 38729-2020: Surface active agents - Test methods of technical sodium primary alkylsulphates
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Basic data

Standard ID GB/T 38729-2020 (GB/T38729-2020)
Description (Translated English) Surface active agents - Test methods of technical sodium primary alkylsulphates
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard G72
Classification of International Standard 71.100.40
Word Count Estimation 10,116
Date of Issue 2020-04-28
Date of Implementation 2020-11-01
Quoted Standard GB/T 3050; GB/T 6365; GB/T 6366; GB/T 6368; GB/T 6682; GB/T 7378; GB/T 8447-2008; GB/T 11275; QB/T 2739-2005
Adopted Standard ISO 894-1977, MOD
Issuing agency(ies) State Administration for Market Regulation, China National Standardization Administration
Summary This standard specifies the pH value, water content, free base or free acid, total alkalinity, petroleum ether extractables, ether extractables after acid hydrolysis (mixed industrial fatty alcohols) ), sodium sulfate, sodium chloride content and other indicators of the test method. This standard is applicable to the testing and evaluation of powder, slurry and liquid (aqueous solution) industrial sodium primary alkyl sulfate (without any product unrelated to preparation).

GB/T 38729-2020: Surface active agents - Test methods of technical sodium primary alkylsulphates

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Surface active agents - Test methods of technical sodium primary alkylsulphates ICS 71.100.40 G72 National Standards of People's Republic of China Surfactant Industrial primary alkyl sodium sulfate test method 2020-04-28 released 2020-11-01 implementation State Administration for Market Regulation Issued by the National Standardization Management Committee

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 894.1977 "Analytical Method for Primary Alkyl Sodium Sulfate in Surfactant Industry". Compared with ISO 894.1977, the structure of this standard is adjusted as follows. --- Chapter 1 corresponds to Chapter 1 and Chapter 2 of ISO 894.1977; --- Chapter 2 corresponds to Chapter 3 of ISO 894.1977; --- Added Chapter 3 "Terms and Definitions"; --- Deleted Chapter 4 and Chapter 5 of ISO 894.1977; --- Chapter 4 corresponds to 6.1 of ISO 894.1977; --- Chapter 5 corresponds to 6.2 of ISO 894.1977; --- Chapter 6 corresponds to 6.3 of ISO 894.1977; --- Chapter 7 corresponds to 6.4 of ISO 894.1977; --- Chapter 8 corresponds to 6.5 of ISO 894.1977, and the test content is adjusted to Appendix A; --- Chapter 9 corresponds to 6.6 of ISO 894.1977, and the test content is adjusted to Appendix B; --- Chapter 10 corresponds to 6.7 of ISO 894.1977; --- Chapter 11 corresponds to 6.8 of ISO 894.1977; --- Chapter 12 corresponds to Chapter 7 of ISO 894.1977; ---Appendix C corresponds to the appendix of ISO 894.1977. The technical differences between this standard and ISO 894.1977 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 11), GB/T 6682 (see A.2 and B.2), GB/T 8447-2008 (see A.4.2.3) and QB/T 2739-2005 (see A.2.6); ● Replace ISO 4314 with GB/T 6365 which is equivalent to adopting international standards (see Chapter 6); ● Replace ISO 4315 (see Chapter 7) with GB/T 7378 modified to adopt international standards; ● Replace ISO 4316 with GB/T 6368 which is equivalent to the international standard (see Chapter 4); ● Replace ISO 4317 (see Chapter 5) with GB/T 11275 modified to adopt international standards; ● Replace ISO 6844 with GB/T 6366 which is modified to adopt international standards (see Chapter 10); ● Deleted ISO 607, ISO 2877 and ISO 4318; ---In order to facilitate the use of the standard, Chapter 3 "Terms and Definitions" has been added; ---Because it was not used during the test, the sampling requirements in Chapter 4 of ISO 894.1977 were deleted; ---The content of Chapter 5 Principles of ISO 894.1977 has been deleted due to duplication of content; ---In order to adapt to the use situation in my country, the determination of water content has been modified (see Chapter 5); ---In order to adapt to the use situation in our country, the method for measuring sodium chloride content has been modified (see Chapter 11); ---In order to adapt to my country's usage habits and reagent specifications, the ethanol concentration has been modified (see A.2.2 and B.2.2); ---According to our country's operating habits, the type of flask has been modified (see A.3.1 and B.3.3); ---In order to adapt to the actual situation of our country, acetone is added to the reagent (see A.2.7); --- In order to adapt to the operating habits of our country, the titration endpoint is quantified (see A.4.2.2); ---In order to adapt to the actual situation in our country, the number of extractions has been increased to make the two phase separation more fully (see A.4.2.3); ---In order to adapt to the actual situation of our country, the operation method of extraction with stoppered measuring cylinder and siphon is added (see A.4.2.3); ---In order to adapt to my country's operating habits, the amount and frequency of washing solvents have been adjusted (see A.4.2.5); ---In order to make the operability stronger and facilitate the test, the temperature and time requirements of the operation process are clarified (see A.4.2.6); ---In order to adapt to the actual situation of our country, the requirements for drawing have been deleted (see A.4.2.7 and B.4.2.6); --- In order to adapt to our country's usage habits, sodium sulfate is omitted, and the description of concentrated hydrochloric acid is modified (see B.2.4). This standard also made the following editorial changes. ---Modified the standard name; ---Integrate Chapter 1 and Chapter 2 of ISO 894.1977 into Chapter 1; ---In the determination of petroleum ether extractables, the introduction is changed to note (see A.1); --- Deleted the note in 6.8.4 of ISO 894.1977 to supplement the method; ---In order to adapt to my country's operating habits, a note has been added (see A.4.2.5); --- Modified the expression of the change requirements of the two weighing results (see A.4.2.7 and B.4.2.6); --- In order to adapt to the usage habits of our country, the note has been modified (see B.5.2). 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)], Suzhou World Spectrum Testing Technology Co., Ltd., Shanghai Kaimi Technology Co., Ltd., Shenzhen Yanqian Technology Co., Ltd., Blue Moon (China) Co., Ltd., Dongguan Guozhong New Materials Research Institute Co., Ltd. The main drafters of this standard. Li Xiaorui, Yao Chenzhi, Ye Zhuhong, Gao Huanquan, Cai Jianbo, He Qiong, Wang Meiling. Surfactant Industrial primary alkyl sodium sulfate test method

1 Scope

This standard specifies the pH value, water content, free alkali or free acid, total alkalinity, petroleum ether Test methods for the content of extracts, ether extractables after acid hydrolysis (mixed industrial fatty alcohols), sodium sulfate and sodium chloride. This standard is applicable to the testing of powder, slurry and liquid (aqueous) industrial primary alkyl sodium sulfate (without any product irrelevant to the preparation) And evaluation.

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, neqISO 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 6682 Analytical laboratory water specifications and test methods (GB/T 6682-2008, ISO 3696.1987, MOD) GB/T 7378 Surfactant alkalinity determination titration method (GB/T 7378-2012, ISO 4315.1977, MOD) GB/T 8447-2008 Industrial linear alkyl benzene sulfonic acid GB/T 11275 Determination of Water Content of Surfactants (GB/T 11275-2007, ISO 4317.1991, MOD) QB/T 2739-2005 Preparation of test solutions for titration analysis (volume analysis) commonly used test methods for detergents

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 Alkalinity The surfactant solution is weakly alkaline due to various decomposition reactions. It neutralizes the hydrochloric acid consumed by a certain amount of product and uses the quality of sodium oxide. The quantity fraction indicates the degree of alkalinity of the product.

4 Determination of pH

According to the method specified in GB/T 6368, the determination is made with a 10% (mass fraction) solution of laboratory samples. Note. If the analyzed pH is lower than 7.0, the sample and its representative batch will be unstable, so most of the test results will change over time. In this case, usually Discard this batch of samples without further analysis.

5 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 is 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%.

6 Determination of free base or free acid

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

7 Determination of total alkalinity

When the measured pH of the sample is far greater than 7, and the free alkalinity value is far greater than 0.3, in this case, it is recommended to follow the provisions of GB/T 7378 Method to determine total alkalinity.

8 Determination of petroleum ether extractables

Petroleum ether extractables include sulfur-free products and products that do not dissociate in aqueous solution although they contain sulfur. Determined according to Appendix A. 9 Determination of ether extractables after acidolysis (mixed industrial fatty alcohols) Determined in accordance with Appendix B. 10 Determination of sodium sulfate content Determined according to the method specified in GB/T 6366. 11 Determination of sodium chloride content Determined according to the method specified in GB/T 3050. 12 Test report The test result report should include the following. a) All the information needed to fully identify the sample; b) The measurement method used (No. of this standard); c) Results and presentation methods used; d) Test conditions; e) Any operation details not specified or optional in this standard, and any circumstances that will affect the results.

Appendix A

(Normative appendix) Determination of extractables of petroleum ether A.1 Principle Extract the petroleum ether extractables in the test alcohol solution with petroleum ether, distill off the petroleum ether, dry and weigh. Volatility of the product Be considered. Note. Petroleum ether extractables include unsulfonated (sulfurized) and non-sulfonated (sulfuric acid) compounds and products that contain sulfur but do not dissociate in water. A.2 Reagents Unless otherwise stated, only use reagents confirmed to be analytically pure and tertiary water in accordance with GB/T 6682 in the analysis. A.2.1 Anhydrous sodium sulfate. A.2.2 95% ethanol solution. A.2.3 Ethanol, 50% (volume fraction) solution. A.2.4 Petroleum ether, boiling range 30℃~60℃. The evaporation residue should not exceed 0.002% (mass fraction). A.2.5 Sodium hydroxide, about 0.1mol/L solution. A.2.6 Phenolphthalein, 1g/L ethanol solution, prepared in accordance with 5.1 of QB/T 2739-2005. A.2.7 Acetone. A.3 Instruments Common laboratory equipment and the following items. A.3.1 Flat-bottomed flask, 250mL, with a ground glass stopper. A.3.2 Glass condenser, length 300mm. A.3.3 Separation funnel, 500mL. A.3.4 Erlenmeyer flask, 250mL. A.3.5 Measuring cylinder with stopper, 250mL (or 300mL), with frosted glass stopper. A.3.6 Siphon tube, inner diameter 3mm~4mm, inner diameter of tube end 1mm~2mm, tube end bend upward. A.3.7 Water bath, the temperature can be controlled at 70℃. A.4 Test procedure A.4.1 Test parts Weigh about 4g (accurate to 0.01g) laboratory sample and place it in a 250mL beaker. A.4.2 Determination A.4.2.1 Dissolve the test part (A.4.1) in 50mL of hot water at about 70℃, stir with a glass rod when dissolving, and then add 50mL while stirring Ethanol solution (A.2.2). Transfer the solution to a 500 mL separatory funnel A (A.3.3). Use ethanol solution (A.2.3) to remove the residue in the beaker Wash to a separatory funnel until the total volume is about 300mL. A.4.2.2 Check whether the solution is weakly alkaline with phenolphthalein (A.2.6), and adjust to reddish and excessive with sodium hydroxide solution (A.2.5) as needed 1mL, shake well, cool, add 50mL petroleum ether (A.2.4), shake for 30s, let it stand for layering, add a small amount of ethanol (A.2.2) if necessary Demulsification. A.4.2.3 Put the lower alcohol water phase into the second separatory funnel B (A.3.3), add 50mL petroleum ether for extraction. Turn the lower layer to the third dispensing Funnel C (A.3.3), and transfer the upper layer to the first separatory funnel A. In this way, three separatory funnels were used to alternately extract the aqueous phase five times. A graduated cylinder with stopper and a siphon can also be used for extraction operations, see 5.2 in GB/T 8447-2008. A.4.2.4 Combine the petroleum ether phase in a separatory funnel, and wash the ether phase with 50 mL ethanol solution (A.2.3) each time until the washing liquid is not alkaline (use Phenolphthalein test). The lotion is incorporated into the aqueous alcohol phase, and this solution L1 is used to determine the content of the mixed industrial fatty alcohol. A.4.2.5 Place the petroleum ether extract in a dry Erlenmeyer flask (A.3.4), add 10g sodium sulfate (A.2.1), shake, and let stand for 30min. Filter with filter paper into a flat-bottomed flask (A.3.1) that has a constant weight, and wash the conical flask, sodium sulfate, funnel, and funnel with 50 mL petroleum ether 3 to 5 times. Filter paper and washing liquid were combined into a flat-bottomed flask. Note. The liquid transfer process in the separatory funnel follows the principle that the upper layer is poured from above and the lower layer flows from below. A.4.2.6 Connect the condenser (A.3.2) to the flask, heat it in a 70°C water bath to evaporate petroleum ether, wait until the solvent is basically evaporated, and cool to At 30°C, remove the condenser, add 3 mL of acetone (A.2.7) to the flask, and then place it in a water bath to evaporate. After the solvent is basically evaporated to dryness, cool the flask to approximately At 30°C, slowly pass in a stream of cold dry air to remove traces of solvent. The outer wall of the flask was wiped dry and placed in a desiccator for 20 minutes before weighing. When it contains low-carbon petroleum ether dissolved substances (such as dodecanol), especially when there is a trace amount of water, it is quite easy to volatilize and lose, so it drives away the solvent, especially Be careful when blowing the air stream, so when you can still detect some solvent smell, cool the flask to room temperature. A.4.2.7 Reheat the flask to about 30°C, blow air flow, wipe dry, cool, and weigh. Repeat the operation until two consecutive weighings The difference is not more than 1mg. A.5 Results presentation A.5.1 Calculation method Petroleum ether extractables content X1, expressed in mass fraction, calculated according to formula (A.1). B.1 Principle The alcohol aqueous solution (L1) obtained in A.4.2.4 was evaporated to 1/5 of the original volume, ethanol was added, and evaporated to dryness. Dissolve the dry residue in water, add hydrochloric acid, and acidify at the boiling point. After the hydrolysis is complete, extract all the released fat with ether substance. These fatty substances include almost all mixed fatty alcohols, but sometimes contain a small amount of sulfo derivatives (pure sulfonates) and fatty acids. Note. When measuring, it is important that the solution is always alkaline. B.2 Reagents Unless otherwise stated, only use reagents confirmed to be analytically pure and tertiary water in accordance with GB/T 6682 in the analysis. B.2.1 Anhydrous sodium sulfate. B.2.2 95% ethanol solution, use phenolphthalein as indicator to adjust to reddish with 0.1mol/L sodium hydroxide solution. B.2.3 Ether. B.2.4 Hydrochloric acid, 37% mass fraction. B.2.5 Hydrochloric acid, about 1mol/L solution. B.2.6 Sodium hydroxide, about 0.1mol/L solution. B.3 Apparatus Common laboratory equipment and the following items. B.3.1 Saponification bottle, 250mL. B.3.2 Separation funnel, 500mL, with frosted glass stopper. B.3.3 Flat-bottomed flask, 250mL, with ground glass neck. B.3.4 Glass condenser, length 300mm. B.3.5 Erlenmeyer flask, 250mL. B.4 Test procedure B.4.1 Test parts Use petroleum ether extractables determination (A.4.2) to obtain the alcohol aqueous solution L1, also see Appendix C. B.4.2 Determination B.4.2.1 Reduce the volume of the test part (B.4.1) to about 1/5 of the original volume by evaporating on the water bath and passing air flow. Add 20mL B Alcohol solution (B.2.2) and evaporate to dryness. Dissolve the residue in 50 mL of water. If necessary, it can be heated during the dissolution process and quantitatively transferred to the saponification bottle (B.3.1) with The volume is controlled at about 100 mL. Add two glass beads to the bottle, and then carefully add 35mL hydrochloric acid solution (B.2.4) (in order to avoid evaporation Any carbonate formed at the time of drying will decompose, causing foam overflow and loss of flask contents, so care must be taken.). B.4.2.2 Install the condenser (B.3.4) and reflux for at least 4h. Cool and quantitatively transfer to a separatory funnel A (B.3.2). With ether (B.2.3) and water, carefully and quantitatively wash the condenser and flask, and merge the washing liquid into the liquid in the separatory funnel. Shake to mix well Evenly. Add 30mL ether (B.2.3), shake vigorously, and then stand. B.4.2.3 Transfer the lower layer to the second separatory funnel B (B.3.2). Extract again with 30 mL of ether. Turn the lower layer to the third separator leak Hopper C, and transfer the upper layer to the first separatory funnel A. The aqueous phase was extracted 3 times, with 30 mL of ether each time. Combine ether phases in separatory funnel A In, then wash the ether extract three times, each with 15mL hydrochloric acid solution (B.2.5). B.4.2.4 Quantitatively transfer the ether extract to a 250mL Erlenmeyer flask (B.3.5) into which about 10g sodium sulfate (B.2.1) has been placed, shake it, and let it stand still 30min, then filter through filter paper into a weighed flask (B.3.3) with a little glass beads. Wash the Erlenmeyer flask, sodium sulfate and filter paper 5 times, with 10mL ether each time. B.4.2.5 Connect the condenser and the flask, place the device on a water bath, and distill until almost all the solvent is evaporated. Remove the condenser and let in slowly Dry cold air to remove the last traces of solvent. When performing this operation, continue to inject air and turn the flask by hand to make the flask leave the water bath in Tilt position. In this way, the liquid in the flask expands into a film to facilitate the removal of the last trace of solvent. If it contains low-carbon petroleum ether dissolved substances (such as dodecanol), especially when there is a trace amount of moisture, it is quite easy to volatilize. Therefore, be careful to drive away It is especially important to pay attention to the air flow. Therefore, when you can still detect some solvent smell, cool the flask to room temperature and wipe it carefully. Dry, weigh, record quality. Reheat the flask to about 30°C, let air flow on it for 1 min, cool it, dry the flask, weigh it again, record Record quality. B.4.2.6 Repeat the above operation until the difference between two successive weighings is not more than 1mg. B.5 Results presentation B.5.1 Calculation method After acid hydrolysis, the ether extractable content X2, expressed in mass fraction, is calculated according to formula (B.1). B.5.2 Reproducibility For the same sample, the difference between the results obtained in the two laboratories should not exceed 1%. Note 1.For mixed industrial fatty alcohols separated in accordance with GB/T 6365, the alkali number and acid number need to be determined. Note 2.The acid value must be less than or equal to 2.

Appendix C

(Informative appendix) Analysis of the overall plan diagram The overall analysis scheme is shown in Figure C.1.

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