SY/T 0601-1997 Determination of emulsified oil and dissolved oil in water
Some standard content:
ICS13.060.30
Registration number: 1144-1998
Petroleum and natural gas industry standard of the People's Republic of China SY/T06011997
Determination of emulsified oil and oil-soluble in water
Determination of emulsified oil and oil-soluble in water1997-12-31 Issued
China National Petroleum Corporation
1998-07-01Implementation
SY/T 0601—1997
Cited Standards
3 Definitions
Summary of Methods
Materials and Equipmentbzxz.net
Preparation before Analysis
7 Analysis Procedures...
8 Error Allowance
9 Report
Appendix A (Appendix to the Standard)
Appendix B (Appendix to the Standard)
Appendix (Appendix to the Standard)
Determination of Oil Dissolved in Water (Infrared-Silica Gel Analysis Method) Determination of Oil Droplet Size Distribution in Water (Microscope Method) Dynamic Viscosity of Water at the Same Temperature
SY T 0601--1997
This standard is formulated according to the arrangement of the document (96) Zhongyoujilanzi No. 52 of China National Petroleum Corporation, "Notice on Issuing the National Standard for Oil and Gas in 1996 and the Plan for the Preparation and Revision of This Standard". During the formulation process, the drafting team searched for relevant literature and materials at the Standard Information Center of the State Administration of Technical Supervision and the Information Research Institute of the General Company. In order to ensure the quality and applicability of the standard, the drafting team conducted in-depth research on five oil fields such as Daqing and Shengli and obtained a large amount of data. This standard was formulated on the basis of strict analysis and test verification. Appendix A, Appendix B and Appendix C of this standard are all appendices of the standard. This standard was proposed by the Planning and Design Institute of China National Petroleum Corporation. Drafting unit of this standard: Xinjiang Petroleum Engineering and Research Institute The main contributors of this standard are Zhu Jian, Chuangwen, Xue Zhaoping, Zhao Bo, Yang Xuming 1
Petroleum and Natural Gas Industry Standard of the People's Republic of China Determination of ernutsified oil and oil-soluble oil in water
in waterSY / T 06011997
This standard specifies the definition, method summary, materials and equipment, preparation work, analysis steps, allowable error, etc. of the static floating method for determining the total amount of emulsified oil and dissolved oil in produced water treated in oil fields. The infrared spectroscopy method is recommended for the determination of dissolved oil. The microscopy method is recommended for the determination of oil droplet size distribution.
This standard is applicable to the determination of emulsified oil and dissolved oil content in produced water, injection water and boiler treated in oil fields. 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through their use in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T1884-1992 Density determination method for oil and liquid petroleum products (densitometer method) GB/T12152-1989 Analysis method for boiler water and cooling water Determination of oil Infrared photometry SY/T053093 Determination method for oil content in oilfield wastewater Spectrophotometry SY5523-92 Analysis method for oilfield water
3 Definitions
This standard adopts the following definitions.
3.1 Emulsified oil
Refers to oil droplets with a particle size of 10~3~10mm in the water sample being tested. 3.2 Soluble oil
Refers to oil droplets with a particle size of less than 10-um in the water sample being tested, which have polarity and can be adsorbed by silica gel. 3.3 Treated produced water refers to produced water that meets the water quality standards for water injection or discharge requirements after treatment. 3.4 Grain-size distribution refers to the ratio of the number of oil droplets of different diameters to the total number of oil droplets. 4 Method Summary
41 Static buoyancy method
According to formula (1), calculate the time (s) required for an oil droplet with a particle size of 10um to float 100mm. Place the water sample in a constant temperature oven with the same temperature as the on-site water using a cylindrical separatory funnel. After (s), first release 20mL of water sample from the bottom of the cylindrical separatory funnel, and then release the water sample below the 100mm mark for oil content analysis. This oil content is the total amount of emulsified oil and dissolved oil in the tested water sample. 4.2 Infrared-silica gel method
This method is mainly used to analyze the dissolved oil content in oil-treated produced water. See Appendix A (Standard Appendix). 4.3 Microscope method
China National Petroleum Corporation approved on December 31, 1997, implemented on July 1, 1998
SY/T 0601--1997
This method is mainly used to analyze the distribution of oil droplets in produced water from oil treatment, see Appendix B (Appendix to the standard). 5 Materials and equipment
a) Simple separatory funnel -4: 250mL (Figure 1), 1 [diameter ≥30mm; -200mm
Figure [Schematic diagram of cylindrical separatory funnel
b) Stopwatch:
c) Iron stand;
d) Constant temperature oven: 0~100c;
e) Plastic sampling ellipse: volume greater than 1OL; f) Latex tube.
6 Preparation before analysis
6.1 Determination of water sample density
Determine the density of the water sample at the on-site water temperature according to the provisions of SY5523--92 sub-5.6. Determination of crude oil density
Determine the density of pure crude oil with the same content as the water sample at the on-site water temperature according to GB/T1884. 6.3 Determination of dynamic viscosity of water sample
Find the dynamic viscosity value of water at the on-site water temperature in Table C1 of Appendix C (Standard Appendix). 7 Analysis steps
The analysis steps of the static floating method are as follows,
SY / T 0601—1997
7.1 Sampling: Open the sampling valve, wait for the water to flow at a rate of 5-6L/min for 3 minutes, then take the sample, and take the water sample from the sampling port into a dry, clean plastic sampling bucket, and the sampling area shall not be less than [OL (the water sample must be analyzed within 24 hours). 7.2 Sample collection: After the sample is allowed to stand for 2 hours, use a latex tube to siphon the water sample from the middle of the sampling bucket into a 250mL cylindrical separatory funnel to 200mm, and plug the top of the cylindrical separatory funnel with a stopper. 7.3 Calculate the time required for an oil droplet with a particle size of 10um to float 100mm according to the following formula. 18H.
gipwp,)d
The time required for an oil droplet with a particle size of 10um to float 100mm. Time required for height, s; dynamic viscosity of produced water, mPa's; height of oil droplet with diameter d, floating, cm: g—acceleration due to gravity, 981cm/s:
Pw—density of water sample, g/cm';
P——density of crude oil, g/cm2;
d,-diameter of oil droplet, cm.
7.4 Fix the cylindrical separating funnel on the iron frame, and make the vertical point of the cylindrical separating funnel on the horizontal plane, then move the iron frame into a constant temperature oven with the same water temperature as the site, and start timing when it is placed in the oven. 7.5 Allow to settle (s), first drain 20mL of water sample from the bottom of the cylindrical separating funnel, and then drain the water sample below the 100mm scale into a dry volume (the cylindrical separating funnel cannot be taken out of the oven). 7.6 Measure the oil content of the released water sample according to SY/T0530 or GB/T12152. This content is the oil content of the emulsified oil and the dissolved oil in the pool. 8 Allowable error
The difference between the two test results of the same sample by the same operator should not be greater than [0% of the average value. 9 Report
The same operator shall measure the same sample twice, and take the arithmetic mean of the two test results as the test result of the water sample at the specified temperature.
Summary of AI method
SY/T 0601—1997
Appendix A
(Appendix recommended by the standard)
Determination of dissolved oil in water
(Infrared-silica gel analysis method)
Dissolved oil is generally polar: and silica gel has the ability to adsorb polar substances. Therefore, carbon tetrachloride is used to extract the oil in the water sample, and then the extract is mixed with anhydrous sodium sulfate to break the emulsion and dehydrate, and then the dehydrated extract is mixed with silica gel: the dissolved oil is naturally adsorbed by silica gel, so it is only necessary to determine the oil content before and after the extract is mixed with silica gel to determine the dissolved oil content. A2 Reagents and materials
a) Carbon tetrachloride;
b) Anhydrous sodium sulfate;
c) Hydrochloric acid: (1+1);
d) Separating funnel: 250mL;
e) Volumetric flask: 100mL;
Bamboo magnetic stirrer;
g) Silica gel: 60-100 months;
h) Pipette: 50mL;
i) Ground-mouth bottle: 100mL.
A3 Analysis steps
A3.1 Preparation of standard solution
Prepare in accordance with the provisions of 6.1 of GB/T12152--1989 A3.21 Drawing of curve
Draw in accordance with the provisions of 6.2 of GBT12152-1989. A3.3 Determination of water samples
A3.3.1 Take 100 mL of the water sample prepared in 7.5 of this standard with a glass sampling bottle: adjust its pH value to less than 2 with hydrochloric acid (1+1).
A3.3.2 Add 30 mL of carbon tetrachloride to the sampling bottle, rotate the sampling bottle to rinse the edges, and then transfer the sample to a 250 mL separatory funnel, shake it for 2 minutes, and let it stand for 10 minutes to separate into layers. A3.3.3 Add about 2 g of anhydrous sodium sulfate to the filter paper soaked with carbon tetrachloride, and then use this funnel to filter the carbon tetrachloride in the separatory funnel into a 100 mL container bottle. A.3.3.4 Take another 30mL of carbon tetrachloride and repeat A3.3.2 to A.3.3.3 twice. Collect the extract plus 1001ml, mix in a volumetric flask, and then dilute the extract to 100mL with carbon tetrachloride. A3.3.5 Use a pipette to accurately transfer 50mL of the extract prepared in A.3.3.4 to a 100mL flask, put 1.5ml of glue in the flask, cover the flask with a stopper, and then stir on a magnetic stirrer for 5 minutes. A3.3.6 Determine the infrared absorbance values of the extracts in A3.3.4 and A3.3.5, and calculate their absorbance C and Cr according to the provisions of GB, T12152-19897.
A4 Calculation of dissolved oil
SY / T 06011997
C,=C-02
Wherein: C—dissolved oil content in water sample, mg/L; C,2—oil content in water sample before silica gel cavity adsorption, /LC2—oil content in water sample after silica gel adsorption, mg/L. A5 Allowable error
The difference between two analysis results of the same test by the same operator should not be greater than 25% of their average value. A6 Disclosure
The same operator shall analyze the same sample twice, and take the arithmetic mean of the two analysis results as the dissolved oil content in the water sample.
B1 Method summary
SY/T 0601-1997
Appendix B
(Appendix to the standard)
Determination of particle size distribution of oil droplets in water
(Microscope method)
First, use acetone to solidify the water sample so that the oil droplets will no longer collide and aggregate during the test; then place the sample on a blood cell counting plate! Count the number and size of the oil droplets under the microscope.
B2 Reagents and materials
a) Propylene glycol
b) Micro syringe: 0.05ml.
|) Blood cell counting plate: Model XB-K-25;
d) Micrometer;
e) Objective micrometer;
f) Syringe: 10mL.
B3 Instruments
a) Microscope: 400 times magnification
b) Analytical reference: accuracy 0.01g
B4 Preparations before analysis
Prepare 100mL 20% propylene glycol solution.
B5 Analysis steps
B5.1 Sample: Use a 10ml syringe to take 10mL of water sample prepared according to standard 7.5 and put it into a small beaker. Add 2mL of 20% propylene glycol solution. Stir evenly
B5.2 Use a 0.05mL microsyringe to take 0.02mL of the sample and place it on the card blood cell counting plate, and flow it onto the cover (there should be no bubbles between the cover glass and the counting plate. First, observe under a low-power microscope to find the grids and oil droplets on the counting plate, and then count under a microscope of not less than 400 times.
B5.3 The counting method is the point counting method, that is, count the 64 small grids under the four corners (16 small grids in each corner) and the 16 small grids in the center, a total of 80 small grids, and the number of oil droplets below the sum, oil droplets of 5 to 10jun, and oil droplets above 10m. B6 Calculate
The number of oil droplets per unit volume
Where: N—the number of oil droplets per unit volume, pieces/mL; 6
SY / T 0601—1997
The number of oil droplets in the selected particle size range in 80 small grids; M—the total number of small grids on the counting plate, take 400;
C——conversion coefficient, take 50;
T is the selected number of counting grids, take 80.
B6.2 Calculation of particle size distribution
Where:
Ⅱ———the percentage of the number of oil droplets in a certain material diameter range to the total number of oil droplets, %; N——unit The number of oil droplets in the selected particle size range in the volume, pieces/mL; N——the total number of oil droplets in the unit volume. pieces/mL. B7 Allowable error
The difference between the two measurement results of the same sample by the same operator should not be greater than 40% of their average value. B8 Report
The same operator conducts two measurements on the same sample, and the arithmetic mean of the two measurement results is taken as the measurement result of the water sample. 0
mPa·s
SY / T 0601—[997
Appendix C
(Appendix of the standard)
Table of dynamic viscosity of water at different temperatures
Table of dynamic viscosity of water at different temperatures
mPa·s
mPa·s=C-02
Wherein: C—the content of dissolved oil in water sample, mg/L; C, the oil content of water sample before silica gel adsorption, /LC2—the oil content of water sample after silica gel adsorption, mg/L. A5 Permissible error
The difference between the results of two analyses of the same test by one operator should not be greater than 25% of their average value. A6 Notice
The same operator shall analyze the same sample twice, and the arithmetic mean of the two analysis results shall be taken as the content of dissolved oil in the water sample.
B1 Method Summary
SY/T 0601-1997
Appendix B
(Appendix of the standard)
Determination of the particle size distribution of oil droplets in water
(Microscope method)
First, solidify the water sample with propanol so that the oil droplets will no longer collide and aggregate during the test: then place the sample on the blood cell counting plate! Count the number and size of the oil droplets under the microscope.
B2 Reagents and materials
a) Propylene glycol
b) Micro syringe: 0.05ml.
|) Blood cell counting plate: Model XB-K-25;
d) Micrometer;
e) Objective micrometer;
f) Syringe: 10mL.
B3 Instruments
a) Microscope: 400 times magnification
b) Analytical reference: accuracy 0.01g
B4 Preparations before analysis
Prepare 100mL 20% propylene glycol solution.
B5 Analysis steps
B5.1 Sample: Use a 10ml syringe to take 10mL of water sample prepared according to standard 7.5 and put it into a small beaker. Add 2mL of 20% propylene glycol solution. Stir evenly
B5.2 Use a 0.05mL microsyringe to take 0.02mL of the sample and place it on the card blood cell counting plate, and flow it onto the cover (there should be no bubbles between the cover glass and the counting plate. First, observe under a low-power microscope to find the grids and oil droplets on the counting plate, and then count under a microscope of not less than 400 times.
B5.3 The counting method is the point counting method, that is, count the 64 small grids under the four corners (16 small grids in each corner) and the 16 small grids in the center, a total of 80 small grids, and the number of oil droplets below the sum, oil droplets of 5 to 10jun, and oil droplets above 10m. B6 Calculate
The number of oil droplets per unit volume
Where: N—the number of oil droplets per unit volume, pieces/mL; 6
SY / T 0601—1997
The number of oil droplets in the selected particle size range in 80 small grids; M—the total number of small grids on the counting plate, take 400;
C——conversion coefficient, take 50;
T is the selected number of counting grids, take 80.
B6.2 Calculation of particle size distribution
Where:
Ⅱ———the percentage of the number of oil droplets in a certain material diameter range to the total number of oil droplets, %; N——unit The number of oil droplets in the selected particle size range in the volume, pieces/mL; N——the total number of oil droplets in the unit volume. pieces/mL. B7 Allowable error
The difference between the two measurement results of the same sample by the same operator should not be greater than 40% of their average value. B8 Report
The same operator conducts two measurements on the same sample, and the arithmetic mean of the two measurement results is taken as the measurement result of the water sample. 0
mPa·s
SY / T 0601—[997
Appendix C
(Appendix of the standard)
Table of dynamic viscosity of water at different temperatures
Table of dynamic viscosity of water at different temperatures
mPa·s
mPa·s=C-02
Wherein: C—the content of dissolved oil in water sample, mg/L; C, the oil content of water sample before silica gel adsorption, /LC2—the oil content of water sample after silica gel adsorption, mg/L. A5 Permissible error
The difference between the results of two analyses of the same test by one operator should not be greater than 25% of their average value. A6 Notice
The same operator shall analyze the same sample twice, and the arithmetic mean of the two analysis results shall be taken as the content of dissolved oil in the water sample.
B1 Method Summary
SY/T 0601-1997
Appendix B
(Appendix of the standard)
Determination of the particle size distribution of oil droplets in water
(Microscope method)
First, solidify the water sample with propanol so that the oil droplets will no longer collide and aggregate during the test: then place the sample on the blood cell counting plate! Count the number and size of the oil droplets under the microscope.
B2 Reagents and materials
a) Propylene glycol
b) Micro syringe: 0.05ml.
|) Blood cell counting plate: Model XB-K-25;
d) Micrometer;
e) Objective micrometer;
f) Syringe: 10mL.
B3 Instruments
a) Microscope: 400 times magnification
b) Analytical reference: accuracy 0.01g
B4 Preparations before analysis
Prepare 100mL 20% propylene glycol solution.
B5 Analysis steps
B5.1 Sample: Use a 10ml syringe to take 10mL of water sample prepared according to standard 7.5 and put it into a small beaker. Add 2mL of 20% propylene glycol solution. Stir evenly
B5.2 Use a 0.05mL microsyringe to take 0.02mL of the sample and place it on the card blood cell counting plate, and flow it onto the cover (there should be no bubbles between the cover glass and the counting plate. First, observe under a low-power microscope to find the grids and oil droplets on the counting plate, and then count under a microscope of not less than 400 times.
B5.3 The counting method is the point counting method, that is, count the 64 small grids under the four corners (16 small grids in each corner) and the 16 small grids in the center, a total of 80 small grids, and the number of oil droplets below the sum, oil droplets of 5 to 10jun, and oil droplets above 10m. B6 Calculate
The number of oil droplets per unit volume
Where: N—the number of oil droplets per unit volume, pieces/mL; 6
SY / T 0601—1997
The number of oil droplets in the selected particle size range in 80 small grids; M—the total number of small grids on the counting plate, take 400;
C——conversion coefficient, take 50;
T is the selected number of counting grids, take 80.
B6.2 Calculation of particle size distribution
Where:
Ⅱ———the percentage of the number of oil droplets in a certain material diameter range to the total number of oil droplets, %; N——unit The number of oil droplets in the selected particle size range in the volume, pieces/mL; N——the total number of oil droplets in the unit volume. pieces/mL. B7 Allowable error
The difference between the two measurement results of the same sample by the same operator should not be greater than 40% of their average value. B8 Report
The same operator conducts two measurements on the same sample, and the arithmetic mean of the two measurement results is taken as the measurement result of the water sample. 0
mPa·s
SY / T 0601—[997
Appendix C
(Appendix of the standard)
Table of dynamic viscosity of water at different temperatures
Table of dynamic viscosity of water at different temperatures
mPa·s
mPa·s
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