This standard specifies the method for determining the polyethylene glycol content and nonionic active matter (adduct) content in ethoxylated derivatives of fatty alcohols and alkylphenols. This standard is applicable to nonionic surfactants containing 2-80 ethylene oxide groups. GB/T 5560-2003 Determination of polyethylene glycol content and nonionic active matter (adduct) content of nonionic surfactants - Weilbull method GB/T5560-2003 Standard download decompression password: www.bzxz.net

GB/T5560-2003/TSO2268:1972
This standard adopts IS2262:19728 nonionic surfactants! Determination of Weibull sub-3. This standard is for the determination of polyethylene glycol content and the identification method of polyethylene glycol content.
The main differences between this standard and GR/5560:985 are as follows:
The Chinese and English versions of the standard are standardized according to GBT1.1--210I. The test report is added.
For ease of use, this standard is modified as follows:
"This international standard" is changed to "this standard": 1. The decimal point \" is replaced by \"; the standard and application fields in the international standard are used; 2. The calculation formulas are respectively included in the wind measurement process and the appendix A of this standard are the current standard rates. This standard is issued by the China Chemical Industry Association since its implementation. This standard is sponsored by the Chemical Industry Surfactant Standardization Technical Committee. Standard unit: Shanghai Dyestuff Research Institute. Standard drafters: Zhuang Yongjian, Ji Juhuo. This standard was first issued in 1985.
Standard
GB/T556D-2003/IS2268:1972
Determination of the content of polyoxyethylene glycol and nonionic active matter (adduct) of nonionic surfactants
Weilbnll method
This standard stipulates "Method for determining the content of polyoxyethylene glycol and nonionic active matter (adduct) in alkyl phenols:
Weilbnll method can determine the content of alkyl phenols and alkyl phenols. This standard is suitable for nonionic surfactants containing 2 to 80 alkylene oxides. The molecular formula (1) and molecular formula (2) of the alkyl phenol ethoxylate are as follows: RO (CH.CH.O>, OH ..
-OCH,CH,O).OH
is the average number of vinyl groups in the olefinic silicon: In formula (1), R is a straight chain or branched alkyl group, generally referred to as CuCiriR
R——In formula (2), R is a branched alkyl group, usually a main group or an octyl group, 2 principle
Non-ionized adducts and ethylene glycol are all in ethyl acetate, and polyethylene glycol can also be in chlorinated adducts, which are not in the range of non-ionized adducts. The separation of glycol and adduct can be carried out as follows: Dissolve the sample in ethyl acetate, extract glycol with sodium chloride solution at 35 ± 1 °C, wash the crude sodium chloride solution with ethyl acetate, and then remove the residue with sodium chloride solution. Extract the ethyl acetate solution with chloroform to remove the residue. Evaporate the ethyl acetate solution containing the adduct and weigh the residue. 3 Reagents
The water used for the test should be water of at least equivalent purity. 3. 17. Ethyl acetate: 6, = 0. g/mL, distilled at 75,5 °C. ~ 775 °C. 3.2 Chloride solution: 300 g bottle of sodium chloride solution in 100: mL distilled water. 3. 3 Chloride solution: e = 1. 48 g/ml., grow at 59.5 ~ 61. 2r. 3.4 Two preparations, anhydrous P, -0.79/ml. Thermal spectrum at 55℃~57℃ 3.6 Petroleum ether, at 10℃~S) 4 Apparatus and equipment
In addition to conventional experimental instruments
4.1 Separation funnel 4 must be at least 25Uml. With enough stopper, month in accordance with the record A formula 1. 4.2 Separation funnel, capacity 25UmL, with Tang certificate and negative. Use Appendix A formula 24.3 Separation funnel, except for the conventional experimental instruments, Capacity 0mml. With grinding glass 4.4 Flask. Container 500mL wide neck, flat.
GB/T5560-20D3/IS02268:1972
4.5 Flask. Container 253ml. Septum collar, with glass. Table: 5 Specifications
5.1 Sample preparation wwW.bzxz.Net
5.1.1 If the sample is transparent, add support to ensure that the sample is evenly distributed. If the sample is transparent or contains precipitates, open the chamber or heat the instrument slowly, record the temperature above 45°C, add clear liquid, and stir to ensure that the sample is evenly distributed.
5.1.2 Solid product
Put the sample in a drying oven and heat it to the highest temperature of the sample. Remove it from the oven, stir and cool it naturally to room temperature.
5.2 Weighing
Weigh 10.05g of the prepared sample and weigh the standard C0-R. 5.3 Determination
5.3.1 Separation of ethylene glycol and adduct
All operations during the separation process should be carried out at 35°C. The sample and the apparatus should be heated to the specified temperature. 25mL of sodium fluoride (3.2) was added to a separatory funnel (1.1A) containing ethyl acetate (3.1) and the mixture was stirred for 30 min until the anion phase disappeared. 53mL of sodium fluoride (3.2) was added to a separatory funnel (1.1A) containing ethyl acetate (3.1) and the mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The mixture was stirred for 30 min. The solution was placed in a separatory funnel (4.1B), stirred fully, and then shrouded for 3 minutes. The sodium chloride solution at the bottom was transferred to a separatory funnel (4.1C), and 2 Eml of ethyl acetate (3.1> was added. The mixture was shaken and placed for 0 minutes. The bottom layer of the solution was transferred to a separatory funnel (4.1B). The acetaldehyde (3.1) in the separatory funnel (4.1B) was weighed and filled with 4 ml of 25 ml of oxidized sodium chloride. The solution was stirred fully for 3 minutes. The sodium chloride solution at the bottom was transferred to a separatory funnel (4.1C), and the separatory funnel (4.1C) was rinsed with the solution. The rinsed solution was transferred to a separatory funnel (4.3). The sodium chloride solution containing diols in the separatory funnel (4.3) was mixed with ethyl acetate. 5.3.2 Determination of adducts Weigh the ethyl acetate in the separatory funnel (4.1A) and transfer it to the flask (4.5) to evaporate the solvent, rinse the separatory funnel (4.1A) with the ethyl acetate in the separatory funnel (4.1), transfer this rinse to the flask (4.5), and rinse the separatory funnel (4.1B) with 25ml of acetic acid (3.1). Rinse the separatory funnel (4.1A) with this rinse, and transfer this rinse to the flask (4.5). Repeat the above operation with 25mL of acetaldehyde (3.1). Then, completely recover the ethyl acetate in the flask (4.5), and use 25ml of ethyl acetate (3.1) to decompose the hot residue in the flask, and heat it to 45℃. Filter with filter paper, transfer 10 ml of warm ethyl acetate (3.1) into a weighed boiling point (4.5) each time, rinse the flask and filter for 3 times, transfer the filtrate and washing liquid into a weighed boiling point (4.5), evaporate the solvent on a water bath, add 10 ml of propylene (3.1) to decompose the residue, and the 4 evaporation residue is the ketone dry residue. Remove the solvent as much as possible by passing the dry gas through the flask (4.1). Repeat the above steps: then add 10 ml of ethyl acetate (3.5) to remove the solvent again, and pass the dry residue through the flask (4.5) with a cold downflow to remove the traces of solvent: clean the flask with a drier, open it in a dryer, open it as quickly as possible, weigh it, add 1 g of boiling point (4.) into the oven, blow it with a cold downflow, plug it and cool it again. Repeat the above-mentioned rapid heating and weighing operation until the mass of the adduct after two consecutive heatings is 3,1=2
The mass fraction of the adduct w<%) is calculated by formula (1), = 100
Where:
The mass of the sample, in grams (g):
The mass fraction of the adduct, in grams (g). 5.3.3 Determination of polyethylene glycol
GE/T5560-2003/ES0226B.1972
Add 100mL of oxygen (3.3, stir thoroughly, and let stand for 15 minutes. After the phase separation is clear, transfer the lower layer of chloroform to bell flask 4.4), repeat the above operation twice to remove the chloroform, and dissolve the residue in chloroform (3.3), filter, weigh the filter, weigh the weighed flask (1.5), rinse the flask and filter paper (times, 10ml each time. Heat (3.1), transfer each spherical condensation to the weighed flask (4.5>, and remove the solvent on the water. Add 15ml of (3.4) to decompose the residue. Stir thoroughly, evaporate the mixture, blow with cold air to remove the solvent as much as possible: repeat the above operation, then add 0nmL of petroleum aldehyde (3.5) to stir thoroughly, remove petroleum ether, blow with cold dry air, and completely remove the solvent. Put the above flask in a weighing pan, heat the original flask (5) in a 100℃ oven for 1m and cool it down to study the reaction. Blow to remove the solvent, then put it in the lower container and cool it down. Repeat the above operation until the difference between two consecutive weighings does not exceed C.1:
Use the mass fraction of ethylene glycol w, (56> Calculate w (%) according to formula (2) ~ n×1CC
Where:
The mass of the sample, in grams (g);
The mass of polyethylene glycol, in grams (g). 6 Test report
The test report should include the following:
E) All information required to fully identify the sample;
The results of the reference force method used;
D) Test conditions:
Any optional details specified in this standard, and all conditions that may affect the results. (2)
GD/T 5560—2003/150 2268:1972 Appendix
(Normative Record)
Method for maintaining the separation temperature
The separation temperature can be maintained in the same way as the two methods. 4.1 Method 1
The separation can be carried out in a small room or a room with a thermostat maintained at (35°C). The sample and the collector should always be kept in the room. The sample and all separations should be carried out at this temperature. The used separation bucket should not be removed from the air under any circumstances until all the ethylene has been removed (the ethylene can be removed from the oxidation state in the room).>
4.2 Method 2
Separation can be carried out in a centrifugal separatory funnel (1.2) with a constant inlet and outlet water supply to ensure that the sample is within the test temperature range: the dimensions and shape of this funnel are shown in 4.1. The unit is gross meter
Figure A.1 Schematic diagram of a narrow vortex separator
separator: B.1:
Z cavity
The effect of the chemical is
The separation is repeated 2
Oxidation belt A?
Good / tamt.)
Ammonia loss
1, 1, 3
Limited by Z
Limited by Z#8:3
Limited by Z2+5
Appendix B
【Normative Appendix》
Separation process diagram
Liquid resistance of ossification
Wuhan City, GR/T5560—2003/ES02268,1972
Complex chemical standard
Yellow chemical island
Oxygen pseudo 2
True chemical liquid
Yiyi 3
National B. 1 Separation process diagram
Bottle 2500)
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