SY/T 0537-1994 Determination of wax content in crude oilSY/T0537-1994 Standard download decompression password: www.bzxz.net

Professional Standard of the People's Republic of China
Determination of wax content in crude oil
Subject content and scope of application
SY/T 0537-94
(No. 7BE21002-89)
This standard specifies the determination of wax content in crude oil by dewaxing with aluminum oxide adsorption and dewaxing agent. The wax referred to in this method is a hydrocarbon that is solid at room temperature.
This standard is applicable to various crude oils.
2 Method Overview
The crude oil is dissolved in petroleum ether. Polar substances are removed by adsorption with lead oxide to obtain wax and oil. The wax and oil are then dewaxed in a benzene-acetone binary mixed solution at -20°C. The dewaxed wax is filtered, washed, and weighed to a constant weight. After drumming, the white content of the wax is determined. 3 Instruments and Materials
3.1 Instruments
Adsorption column: with circulating water jacket (see Figure 1) Super constant temperature water bath.
High temperature furnace: not less than 600℃.
Constant temperature water bath.
Vacuum drying oven.
Vacuum flask.
Triangular flask: 100mL or 150ml.
Low temperature thermometer: -30~~60℃.
Wide mouth thermos flask.
Suction filter device: see Figure 2.
Vacuum desiccator.
Acid-resistant funnel, G4 or 3 type, 10mL.
Porcelain evaporator ⅢL.
Thin bottle.
Pipette.
3.2 Materials
Fast quantitative filter paper.
Solid carbon monoxide (dry ice).
Approved by China Petrochemical Corporation on May 12, 1989 and implemented on May 1, 1990
ZB E21002—89
Figure 1 Dimensions of adsorption column and adsorption flow chart
1 Solvent; 2 Alumina: 3--Cotton; 4-Super constant temperature bath vacuum
2 Suction filter
1 Suction filter bottle 2 Acid-resistant sintering bucket
4 ReagentsbzxZ.net
4.1 Alumina: for chromatography, neutral, 100-200 mesh. ZB E 21002-89
Comply with Shanghai Q/HG12-253--81 "Lead Oxide", 4.2 Petroleum ether: 60-90℃, analytical grade. 4.3 Benzene: chemically pure.
4.4 Ketone: chemically pure.
4.5 Industrial alcohol.
5 Preparation
5.1 Preparation of 1% water-containing aluminum oxide: Put aluminum oxide into porcelain evaporating blood, then put it into a high-temperature furnace, roast it at 500℃ for 6h, take it out, put it into a vacuum dryer immediately, cool it to room temperature, put it into a weighed narrow-necked bottle, and weigh the weight of aluminum oxide. Use a transfer tube to add 1% distilled water to the lead oxide, plug the rubber stopper, shake it thoroughly, and place it for 24 hours. 5.2 Benzene-acetone mixed solvent: Benzene and acetone are mixed in a ratio of 1:1 (volume ratio) and Shake thoroughly. 5.3 Constant weight conical flask: Wash the 100mL conical flask and dry it at 105±1℃ until it is heavy. 6 Test steps
6.1 Weigh 1g of sample in a 50ml conical flask (or beaker) to 0.0001g, heat it in a water bath to melt, and then add 10mL of petroleum ether to dissolve it. 6.2 Connect the adsorption column to the super constant temperature bath according to Figure 1, adjust the temperature of the constant temperature bath to 40~45℃, and circulate water. 6.3 Plug a small amount of absorbent cotton at the lower end of the adsorption column, add 30g of alumina from the upper end with a bucket and cover it tightly. 6.4 Measure 20mL of petroleum ether and pour it into the adsorption rod filled with alumina to wet the alumina. At the same time, place a weighed conical flask at the lower end of the column to receive the outflow!.
6.5 When the petroleum ether on the adsorption column does not enter the oxygen After the aluminum oxide is dissolved, pour in the sample dissolved in 6.1. Wash the residue in the bottle with 10mL petroleum ether three times, and add the washing liquid into the adsorption column respectively. 6.6 After the petroleum ether completely wets the aluminum oxide, add a small amount of lead oxide (0.3~～0.5) to the adsorption column. 6.7 Add 60mL benzene to the adsorption column to rinse the oil wax part of the sample. Note: 1) When the density of crude oil is greater than 0.9g/cm, the amount of aluminum oxide used is 40k, the amount of wetting agent petroleum ether used is 30ml, and the amount of flushing agent benzene used is 80mL6.8 When all the solution in the adsorption column flows out, move the conical flask to the water bath and evaporate the solvent. 6.9 After the solvent is evaporated, dissolve the oil wax mixture in the bottle with 30mL benzene-propylene mixed solvent while it is hot. If there is insoluble matter in the bottle, it needs to be dissolved in a water bath with slight heat, and then cooled to room temperature. ||tt| |6.10 In a thermos, use industrial ethanol and solid carbon dioxide to adjust the cold bath temperature to -25±1°C (other refrigeration equipment can also be used as a cold bath).
6-11 Place the mixed solution cooled to room temperature in a thermos at -25±1°C to cool. During the cooling process, stir the mixed solution continuously. When the temperature of the mixed solution reaches -20°C, continue to maintain it for 3 to 5 minutes. 6.12 Place a piece of rapid quantitative filter paper on the glass acid-resistant funnel, and then install the suction filter device according to Figure 2. Adjust the cold bath temperature to -25±1°C. Filter the mixed solution that has been cooled to -20°C on the filter device. When the mixed solution is completely sucked dry, there is 20mL of benzene-acetone mixed solvent cooled to -20°C. Wash the wax in the funnel twice. When washing, stir the solvent and wax thoroughly, and then filter it by suction. The triangular flask containing the mixed solution is ready for use. Note! Keep the upper edge of the acid-resistant funnel 5m to the left of the coolant liquid surface. Avoid coolant entering the acid-resistant funnel. 6.13 After the suction filtration is completed, wash the funnel with hot petroleum ether, put the wax in the Erlenmeyer flask for use in 6.12 (if there is more wax in funnel 1, use a small steel shovel to move the wax to the leaves of the flask, and then wash the remaining wax on the funnel with hot petroleum ether) and put it on a water bath to evaporate the solvent. 4 After the solvent is evaporated, put the Erlenmeyer flask in a vacuum drying oven, dry it at 100℃.66.7kPa (500mtmHg) for 1h, take it out, cool it, and weigh it until it is constant weight.
7 Calculation
ZBE21002—89
The wax content Xr% (m/m) in the sample is calculated according to the following formula: X
Where: mi
8 Precision
-mass of wax and Erlenmeyer flask·g+
mass of Erlenmeyer flask·more
mass of sample, g.
my--ng
Judge the reliability of the test results according to the following provisions (95% confidence level). 8.1 Repeatability: The difference between two results measured repeatedly by the same operator should not be greater than the following value: Wax content in crude oil, % (n/m)
8.2 Reproducibility: The difference between two results proposed by different laboratories should not be less than the following value: Wax content in crude oil, % (m/m)
9 Report
Take the arithmetic mean of the two repeated results as the test result. Additional notes:
This standard is under the technical jurisdiction of the Petrochemical Science Research Institute. This standard was drafted by the Petrochemical Science Research Institute. The main drafter of this standard is Zhu Xiuqin.
Repeatability, % (m/m)
Reproducibility, % (m/m)
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.