SY/T 5242-1991 Determination of sulfonic acid content in drilling fluid treatment agentsSY/T5242-1991 Standard download decompression password: www.bzxz.net

Petroleum and Natural Gas Industry Standard of the People's Republic of China SY /T 524291
Method for determination of sulfonate content in drilling fluid treatment agents
Issued on July 19, 1991
Ministry of Energy of the People's Republic of China
Implementation on November 1, 1991wwW.bzxz.Net
Petroleum and Natural Gas Industry Standard of the People's Republic of China Method for determination of sulfonate content in drilling fluid treatment agents 1 Subject content and scope of application
SY / T 5242-91
This standard specifies the procedure for determination of sulfonate content. This standard is applicable to the determination of sulfonate content in various water-soluble sulfonated treatment agents in drilling fluid treatment agents, so as to compare the sulfonate content in similar products.
2 Determination procedure of sulfonic group content
2.1 Definition
Sulfonic group content refers to the number of millimoles of sulfonic groups contained in each gram of sulfonated product. 2.2 Principle of the method
After separation and purification, the sample solution of the treating agent is completely converted into sulfonic acid benzene after passing through a cation exchange resin column. It is titrated with a standard sodium hydroxide solution. During the titration process, it combines with hydroxide ions to form non-conductive water molecules, and the limiting ion conductivity of sodium is less than that of hydrogen. Therefore, the conductivity of the solution gradually decreases and reaches the lowest value at the end point. After that, sodium hydroxide is continuously added, and the excess sodium ions and oxygen ions cause the conductivity to rise again.
2,3 Reagents and materials
Cation exchange resin: 723 type strong acid
Anion exchange resin: 717 type strong alkaline; Sodium cyanide: analytical grade;
Hydrochloric acid: analytical grade;
Sodium sulfate: analytical grade:
f. Ethanol: analytical grade (95%):
Filter paper: rapid, qualitative;
Glass cotton.
2.4 Instruments and apparatus
Conductivity meter: DDS-IIA type or similar products; a.
Dispenser: magnetic;
Burette: 50, 100ml, acidic, alkaline; d. Balance: sensitivity 0.001g;
Volume flask: 250ml;
Beaker: 250, 400ml
Fountain: long neck;
h, electric furnace: 1kW, adjustable.
2.5 Determination procedure
Preparation of ion exchange resin column
Approved by the Ministry of Energy of the People's Republic of China on July 19, 1991, implemented on November 1, 1991
SY/T 524291
2.5.1.1Put the cation exchange resin in a beaker, add ethanol until the cation exchange resin is submerged, stir with a glass rod to dissolve the organic matter, pour out the ethanol, and then wash with distilled water until the water is clear, and then soak it in 2mol/1 sodium hydroxide solution twice the volume of the ion exchange resin for 24h. Then wash it with distilled water to make it close to neutral. 2.5.1.2 Fill a 50ml acid burette (or a special exchange tray) with glass wool (or glass cloth) to prevent the ion exchange resin beads from clogging the small hole of the stopcock.
2.5.1,3 Pour the anion exchange resin washed to neutrality together with distilled water into the burette, so that the height of the ion exchange resin reaches about 15m, and then add distilled water, and wash the ion exchange resin to neutrality (with the pH value of distilled water) at a rate of 2 to 3 drops per second, and set aside.
2.5.1.4 Use salt instead of sodium hydroxide to treat the cation exchange resin according to steps 2.5.1.1 to 2.5.1.3. Note: After loading, ensure that the resin does not come into contact with air and keep the water surface of the burette always above the ion exchange resin. 2.5.2 Weigh 4-5g of sulfonated product sample (accurate to 0.00lg) into 200ml boiling water: add 10ml of distilled water, stir thoroughly and let stand for 24h. Heat and maintain a slight boiling state for 30min, filter with fast-setting filter paper while hot: transfer the filtrate and washing to a 250ml volumetric flask, dilute to 6 scales with distilled water, shake and set aside. 2.5. 3 Accurately pipette 25 ml of the above solution and add it to the anion exchange resin column. Leave it for 15 minutes and release the ions at a flow rate of 1 to 2 drops per second. Then wash the anion exchange resin with distilled water, and the flow rate is still 1 to 2 drops per second: collect all the effluent in a beaker. 2.5.4 Add the effluent obtained in 2.5.3 to the cation exchange resin column several times, and operate according to 2.5.3, and collect all the effluent in a 400 ml beaker.
2.5.5 In the above 2 .5.4 Connect a platinum electrode to the beaker of the effluent obtained, adjust the conductivity meter, and under stirring with a magnetic stirrer, add 0.05 mol/1 standard sodium hydroxide solution for titration. Add about 0.5 ml at a time. After stirring evenly and the conductivity is stable, record the volume of the sodium hydroxide standard solution consumed and its corresponding conductivity level. When approaching the end point, the titration speed should not be too fast, and it is better to add dropwise. After reaching the end point (i.e. the lowest point of conductivity), continue to add sodium hydroxide standard solution until the conductivity reaches the estimated value. To determine its lowest point. 2.6 Calculation
Basic content = -
m×250
Where: M-: Liquid density of sodium hydroxide standard solution, mol/1; Volume of sodium hydroxide standard solution consumed when conductivity is at the lowest value, tml; m-: Weight of sample weighed, g.
2.7 Accuracy
The relative deviation between two parallel results should be less than 2%. 2.8 Regeneration of ion exchange resin (see Appendix A) 2
SY / T 5242-91
Appendix A
Regeneration of ion exchange resin
(reference)
A1 Regeneration of anion exchange resin: Re-dose 2mol/1 sodium hydroxide solution, the amount is 3 to 5 times the volume of anion exchange resin. Alkali solution enters from the top, stays for 15 minutes, and then discharges from the bottom at a flow rate of 2 to 3 drops per second, and then rinses with distilled water until the pH value of the effluent is 7 to 8.
A2 Regeneration of cation exchange resin: Re-dose The hydrochloric acid solution is 2mal/1, and the dosage is 2 to 3 times the volume of the cation exchange resin. The acid solution enters from 1:, stays for 15 minutes, and then discharges the acid solution from the lower end at a flow rate of 2 to 3 drops per second, and then rinses with distilled water until the pH value of the effluent is 6 to 7.
Additional instructions:
This standard was proposed by the non-engineering professional standardization committee of Shanyouzhuan. This standard was drafted by Chengde Petroleum Technical College. The main contributors to this standard are Zhang Guozhao, Zheng Rongzhi, and 3
This standard is still valid after the review in 199, and the review result has been approved by the State Bureau of Petroleum and Chemical Industry.
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