This standard specifies five methods (A, B, C, D and E) for determining the cloud point of nonionic surfactants. GB/T 5559-1993 Determination of cloud point of ethylene oxide type and ethylene oxide-propylene oxide block polymer type nonionic surfactants GB/T5559-1993 Standard download decompression password: www.bzxz.net

UDC.661.185:543.8:677.041.4
National Standard of the People's Republic of China
GB/T 5559-93
Ethylene oxide type and ethylene oxide
Propylene oxide block polymer type
Determination of cloud point of non-ionic surfactants
Non-ionic surface active agents obtained from ethylene oxide and ethylene oxide/propylene oxide blockcopolymers--Determination of cloud pointPublished on August 6, 1993
State Administration of Technical Supervision
Implemented on September 1, 1994
National Standard of the People's Republic of China
Ethylene oxide type and ethylene oxide
Propylene oxide block polymer type
Determination of cloud point of non-ionic surfactants
Non-ionic surface active agents obtained from ethylene oxide and ethylene oxide/propylene oxide Blockcopolymers-Determination of cloud pointGB/T5559-93
Replaces GB5559-85
This standard is equivalent to the international standard ISO1065-1991 "Nonionic surfactants and mixed nonionic surfactants prepared from ethylene oxide-Determination of cloud point". 1 Subject content and scope of application
This standard specifies five methods (A, B, C, D and E) for determining the cloud point of nonionic surfactants. Methods A, B and C are mainly applicable to the determination of cloud point of nonionic surfactants formed by condensation of lipophilic compounds such as fatty alcohols, fatty acids, fatty acid esters, fatty amines, alkylphenols and ethylene oxide. Methods D and E are mainly applicable to the determination of cloud point of ethylene oxide-propylene oxide block polymer nonionic surfactants. Method E is usually not applicable to nonionic surfactants formed by lipophilic compounds such as fatty acids or fatty acid esters and ethylene oxide-propylene oxide block polymers, but can only be used when it is proven to be reproducible in the determination. 2 Reference standards
GB601 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB6367 Preparation of water with known calcium hardness by surfactants 3 Selection of methods
3.1 Method A
If the aqueous solution of the sample becomes turbid between 10 and 90°C, the measurement shall be carried out in distilled water. 3.2 Method B
If the aqueous solution of the sample becomes turbid at a temperature below 10°C or the sample cannot be fully dissolved in water, the measurement shall be carried out in a 25% (m/m) diethylene glycol butyl ether aqueous solution. This method is not suitable for some samples with low ethylene oxide content and samples that are insoluble in 25% (m/m) diethylene glycol butyl ether solution.
3.3 Method C
If the aqueous solution of the sample becomes turbid at a temperature above 90°C, the measurement shall be carried out in a sealed ampoule. The use of a sealed ampoule allows the operation to be carried out under pressure to reach a temperature higher than the boiling point of the solution at atmospheric pressure. Alternatively, sodium chloride aqueous solution can be used instead of distilled water to determine the turbidity point of the sample according to method A, but the results obtained do not show a simple correlation with the results obtained using anhydrous sodium chloride.
3.4 ​​Method D
Approved by the State Administration of Technical Supervision on August 6, 1993 and implemented on September 1, 1994
GB/T 5559-93
If the acidic aqueous solution of the sample becomes turbid between 10 and 90°C, the measurement shall be carried out in a standard hydrochloric acid solution with a concentration of c(HCI) = 1.0 mol/L.
3.5 Method E
If the acidic aqueous solution of the sample becomes turbid at a temperature above 90°C, the measurement shall be carried out in an aqueous solution containing 50 g of n-butanol and 0.04 g of calcium ions (Ca2+) per liter.
4 Principle
Heat the sample solution of specified concentration under test conditions until the liquid is completely opaque, cool and stir continuously, and observe the temperature when the opacity disappears.
5 Reagents and solutions
5.1 Water: laboratory distilled water.
5.2 Diethylene glycol butyl ether solution: chemically pure, 25% (m/m) solution. Diethylene glycol ether [C, HO(CH2)2O(CH2)OH has the following properties: density p2 = 0.945 ± 0.002 g/mL.
Refractive index n = 1.432 ± 0.001.
Water content <1% (m/m).
If it contains different amounts of impurities, it will affect the cloud point. 5.3 Sodium chloride (GB1266) solution: 50g/L; 5.4 Calcium-butanol (HG3-1012) solution: an aqueous solution containing 50g n-butanol and 0.04g calcium ion (Ca2+) per liter. Prepare water with known calcium hardness according to GB6367;
5.5 Hydrochloric acid (GB622) standard solution: concentration c(HCI) = 1.0mol/L. 6 Instruments and equipment
6.1 Thermometer: with a graduation of 0.1℃ and a range suitable for the temperature of the sample being measured: 6.2 Iodine volume flask, with a capacity of 250mL;
Measuring cylinder: with a capacity of 100mL;
Beaker: with a capacity of 1000mL, filled with a transparent heat conductor (such as ethylene glycol); 6.4
Test tube: with a capacity of 20mL;
6.6 An: made of safety glass with an outer diameter of 14mm, an inner diameter of 12mm, and a height of 120mm, covered with a wire mesh; 6.7
Analytical balance;
6.8 Conventional heater;
6.9 Magnetic stirrer with heating.
7 Determination steps
7:1 Method A
7.1.1 Sample
Weigh 0.5g of the sample to an accuracy of 0.01g.
7.1.2 Determination
Put the sample into an iodine volumetric flask, add 100mL of distilled water, shake well, and dissolve the sample completely. Instructions for use:
1] Use a conical flask in ISO1065.
GB/T5559—93
Pour 15mL of the sample solution into a test tube, insert a thermometer, and then move the test tube into a beaker, heat it, and gently stir it with a thermometer until the solution is completely turbid (the temperature of the solution should not exceed 10℃ of the turbidity temperature), then stop heating. The test tube remains in the beaker, and the solution is gently stirred with a thermometer, which is slowly cooled. Record the temperature when the turbidity disappears, and measure twice in parallel. The difference between the parallel measurement results is not greater than 0.5℃. 7.2 Method B
7.2.1 Sample
Weigh 5g of the sample to an accuracy of 0.01g.
7.2.2 Determination
Put the sample into an iodine volumetric flask, add 45g of diethylene glycol butyl ether solution (5.2), shake well, and dissolve the sample completely. The operation is the same as method A (starting from the second paragraph of 7.1.2).
7.3 Method C
7.3.1 Sample
Weigh 0.5g of the sample, accurate to 0.01g.
7.3.2 Determination
7.3.2.1 Ammonium method
Put the sample into an iodine volumetric flask, add 100mL of distilled water, shake well, and dissolve the sample completely. Use a pipette to draw the sample solution into the ammonium, with a depth of about 40mm. Seal the mouth of the ammonium with fire, and then cover the ammonium with a wire mesh, and move it into a beaker with a heat conductor, with the upper end of the ammonium slightly protruding from the beaker. To prevent the explosion of the device due to poor sealing, a safety glass or transparent plastic protective screen should be placed in front of the device. The test device is shown in the figure. 1 Safety screen
Thermometer
Sealed safety
Sample solution
·Heat exchange bath
Test device diagram of method C
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Heater
GB/T5559--93
Insert the thermometer into the heating bath, turn on the magnetic stirrer and heat. When the liquid in the device becomes turbid, stop heating, continue stirring, let it cool, and record the temperature when the turbidity disappears completely. Parallel determination is performed twice, and the difference between the parallel determination results is not greater than 0.5℃. 7.3.2.2 Salt water determination method
Put the sample into an iodine volume bottle, add 100mL of sodium chloride solution (5.3), shake well, and dissolve the sample completely. The operation is the same as method A (starting from the second paragraph of 7.1.2).
7.4 Method D
7.4.1 Sample
Weigh 1g of sample, accurate to 0.01g.
7.4.2 Determination
Put the sample in an iodine volumetric flask, add 50mL of hydrochloric acid solution (5.5), shake well to dissolve the sample completely, then add 50mL of hydrochloric acid aqueous solution (5.5). The operation is the same as method A (starting from the second paragraph of 7.1.2). 7.5 Method E
7.5.1 Sample
Weigh 1g of sample, accurate to 0.01g.
7.5.2 Determination
Put the sample in an iodine volumetric flask, add 100mL of calcium-butanol aqueous solution (5.4), shake well to dissolve the sample completely. The operation is the same as method A (starting from the second paragraph of 7.1.2).
8 Expression of analysis results
The difference between the results of parallel determinations is not greater than 0.5℃, and the arithmetic mean of the parallel determinations is taken as the determination result, and the medium used in the determination is stated. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shanghai Dyestuff Research Institute. This standard is drafted by Shanghai Dyestuff Research Institute. The drafter of this standard is Cai Mijun.
(Beijing) Xindengzi No. 023
People's Republic of China
National Standard
Ethylene oxide type and ethylene oxide
Propylene oxide block polymerization type
Determination of cloud point of non-ionic surfactants
GB/T5559-93
Published by China Standards Press
(Beijing Fuwai Sanlihe)
Printed by Beijing Printing Factory of China Standards Press Sold by Xinhua Bookstores in various places||tt ||Published by Beijing Publishing House of Xinhua Bookstore
Copyright reserved. No reproduction allowed
Format: 880×12301/16
Printing sheet: 1/2
Word count: 8,000
First edition in May 1994
First printing in May 1994
Print run: 1-1500
Book number: 155066·1-10587
Price: 1.50 yuan
Heading: 240-18
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