SY/T 0531-1994 Determination of suspended particles in oil field injection water Resistance induction method SY/T0531-1994 Standard download decompression password: www.bzxz.net

Petroleum and Natural Gas Industry Standard of the People's Republic of China SY/ T 0531--94
Determination of suspended particles in oilfield injection water
Resistance induction method
Published on April 5, 1994
China National Petroleum Corporation
Implementation on October 1, 1994
1 Subject content and scope of application
Petroleum and Natural Gas Industry Standard of the People's Republic of China Determination of suspended particles in oilfield injection water
Resistance induction method
SY/ T 0531---94
This standard specifies the terminology, symbols, codes, method principles, etc. for determining suspended particles in oilfield injection water using the resistance induction method. Operation, operation steps, instrument calibration, result expression and precision. This standard is applicable to the determination of the number and size distribution of suspended particles in oilfield injection water. 2 Reference standards
GRW[E]
GBW(E)
GBW(E)
120001
Particle standard material
120002
Particle standard material
120003
Particle standard material
GBW(E)
Particle standard material
120004
3 Terms, symbols and codes
3.1 Terms
3.1.1 Empty sample: refers to the electrolyte solution in the process of measuring the instrument. 3.1.2 Conductive sample: refers to the mixture of water sample and electrolyte solution. 3.1.3 Particle size distribution: refers to the particle size distribution range. 3.1.4 Overlap error: refers to the error caused by the instrument being unable to completely separate two or more particles when they pass through the detection aperture at the same time due to the weight of the pulses generated by the particles. 3.1.5 Reading value: refers to the multiple value of the control particle size range. 3.2 Symbols: Code
Symbols and codes should comply with the provisions of Table 1.
Symbols and codes
Symbols and codes
Quantity adjustment
Nominal diameter of the pipe
Diameter of spherical particles
Diameter of standard particles
Refer to the lower value diameter
Refer to the upper value diameter
Approval statement of China National Petroleum Corporation on April 5, 1994
Implementation on April 1, 1994
Symbols and codes
Current adjustment
Number of particles measured by the instrument
Number of particles after calibration
Difference in the number of particles between adjacent particle sizes
Value adjustment
Unit particle volume
Volume of water sample added with conductive sample
SY/ T 053. --94
Preparation of conductive sampleElectrolyte volume addedCounted by injection volume
Reading valueResidual volume
Referring to the commercial volume
Aperture correction factor
Calibration validity of orifice tube
Number of particles smaller than 10 μm
Number of particles smaller than 2 μmPercentage of particles smaller than 2 μm
Accumulation of particles smaller than 2 μm
Volume ratio of particles smaller than 24%
Number of particles per channel in the original water sample
Amount of particles distributed in the whole
4 Principle of resistance induction
Fukasawa
Ratio system
Diskless
Measurementless nanometer
First, disperse the water sample to be tested in the electrolyte solution to prepare a conductive sample for measurement, and then measure the conductive sample trace. When the conductive sample passes through the small hole in the detection tube, the particles in the liquid generate impedance, resulting in an instantaneous change in the potential difference between the electrodes: the amplitude of the potential difference change is proportional to the volume of the particles, from which the number and volume of the particles can be calculated. 5 Reagents and materials
5.1 Chlorine: analytically pure
5.2 Formaldehyde: analytically pure
5.3 Standard electrolyte: National secondary standard substance or equivalent national secondary standard substance, in accordance with GBWE)120001.GBW(E)1202, GRW(E)120003.GBW(Er
5.4 Filter material: microporous membrane or its filter, the pore size should not be greater than 0.45!1. 6 Instruments and equipment
61 Particle size analyzer: particle size analyzer based on the principle of electric induction. 120094.
SY/ T 053I-94
62 Filter: microporous membrane filter or its chemical type of filter equipment: 6.3 Days: sensitivity is 0.1g
6.4 Refrigerator: Commercially available
6.5 Pipette: Specifications are 5, 10, 20ml.6.6 Measuring cylinder: Specifications are 100, 200ml.
6.7 Button-mouth bottle: Specifications are 100, 125, 250, 1000, 2000, 5000mL. 68 Sampling box: Medical visit bag,
7.1 Water sample collection
7.1.1 First clean the narrow-necked bottle used for collecting water samples with distilled water (if a water pipeline is required, the pipeline should be connected in the same way). 7.1.3 Select the sample, open the valve, and flow it at a flow rate of 5~6L/min for 3min, then cover the bottle with a narrow-mouth bottle cap to receive the water sample to the bottle mouth, close it immediately, seal it with tape, and then put it into the sampling box and send it to the test site. 7.2 Water sample storage
Water samples should be tested within 24 hours. Water samples that cannot be tested should be placed in a refrigerator for cold storage. The storage time should not exceed 4811.7.3 Preparation of conductive samples
7.3.1 Use the finely filtered electrolyte bath to clean the sampling cup, volumetric tube and pipette. 7.3.2 Use a volumetric tube to measure 0U~150mL (V) of the finely filtered electrolyte solution and pour it into the sampling cup. 7.3.3 Shake the water sample bottle several times, and use a pipette to transfer the water sample with a volume of V into the sampling cup. I should be selected according to the total particle size of the water sample. The appropriate amount is: to make the overlap error of the prepared conductive sample less than [5% during the measurement, otherwise it should be increased.
8 Analytical steps
8.1 Test tube selection
Test tubes with a grid diameter of 504um or less should be selected. 8.2 Selection of electrolyte solution concentration
When using a test tube with a grid diameter of 501, the electrolyte solution concentration should be 1%-2% (m/min.). 8.2.1 When using a test tube with a D of 30um or smaller diameter: the electrolyte solution concentration should be 2%-4% (m/min.). 8.2.2 Preparation of electrolyte solution
According to the selected electrolyte solution concentration, weigh a certain amount of sodium chloride and add it to a certain amount of distilled water: stir until dissolved. If it is necessary to store, formaldehyde should be added at a ratio of 0.1% (/). 8.3 Fine filtration of electrolyte solution
8.3.1 Selection of filter material aperture
The aperture of the filter material should be selected according to the aperture L of the detection tube used by the particle size analyzer. When using a detection tube with a diameter of 50uml: a filter material with an aperture of 0.45um or less should be selected: when using a detection tube with a diameter of 30m or less, a filter material with an aperture of 0.2um or less should be selected. During use, the filter material should be pre-treated according to the manufacturer's instructions. 8.3.2 Fine filtration and technical indicators
Wash the filter equipment with distilled water, install the filter material in the filter, turn on the filter control, and exhaust the air to allow the filtrate to flow slowly to the liquid receiving bottle. If pressurized or negative pressure filtration is used, the pressure must be controlled within the pressure range that the filter material can withstand. 3
SY/ T 0531-94
The refined electrolyte solution must meet the following indicators: When D is 50um and V㎡ is 0.05mL, the total number of particles in the filtrate (effective measurement range) should not exceed 150; when D is 30um) or smaller in diameter and V㎡ is 0.05mL, the total number of particles in the filtrate (effective measurement range) should exceed 500.
8.4 Blank test
The refined electrolyte solution is measured according to the measurement steps in 8.6, and the measurement result is the blank value. If a single-channel instrument is used, the blank value should be recorded in the table in Appendix A (reference); if a multi-channel instrument is used, it should be stored in the computer and the blank value should be deducted after the sample is measured.
8.5 Instrument calibration
8.5.1 Selection of standard particles
Select appropriate standard particles according to the diameter of the test tube used: when D is 50mm, select standard particles with d of 5; when D is 30um, select standard particles with d of 2um. 8.5.2 Preparation of standard solution
Measure 100-150mL of the electrolyte solution after filtration, pour it into the sample cup, then add a few drops of the standard solution, place it on the sample table, and stir it for testing.
8.5.3 Single-channel instrument calibration
8.5.3.1 Start the instrument, and after the instrument is normal, adjust the threshold 1 to 2, and adjust A and I at the same time so that the pulse area is about 2 cm. 8.5.3.2 Re-adjust the threshold value so that the main pulse reaches the maximum height, measure the sample 3-4 times and observe the repeatability. Record the threshold value of the ratio! as T.
8.5.3.3 Adjust the threshold value 1 to 0.5T and 1.5T respectively, measure 3-4 times respectively, take the average value of each and set it as 1, 2 and 3: For 1 and 3, the average value is:
8.5.3.4 After calculating,, then adjust the threshold t to 7 again, measure the sample 3-4 times and take the average value, and observe whether the ratio is close to 10, 2. Otherwise, it is necessary to re-adjust the threshold value within the following range! Until the measurement result is close to 1, 2. 8.5.3, S Substitute the values ​​of A, I, t after calibration into the following formula. The calibration constant K can be obtained: K value
8.5.,4 Multichannel instrument calibration
85.4.1 Start the instrument, and input the diameter, thickness, sampling volume, actual diameter of the standard particle, etc. according to the instrument manual. Move the select key to the calibration program.
85.4.2 Full range sampling measurement, remove the blank, observe the particle distribution of the actual quasi-particle and the diameter corresponding to the peak value. 8.5.4.3 Full range sampling measurement, observe the particle distribution of the standard particle, move the left cursor to overlap to the peak: If obvious double peaks are found: Move the left and right cursors to the left peak, press calibration (CAL), the instrument automatically calibrates and calculates the K value. 8.5.4.4 Save the calibration value to the computer.
8.5.5 Calibration cycle
One month.
8.6 Determination
8.6.1 Determination by single channel instrument
SY/ T 0531--94
8.6.1.1 Start the instrument and select the input group. The product is almost stable for 10 min. 8.6.1.2 Enter the values ​​of 1:1.A from the maximum level to the minimum level. 8.6.1.3 Start the agitator and inject the sample. Count 3~4 times for each particle size. 8.6.1.4 Record the measurement results in the table in Appendix A (reference document). 8.6.2 Use multi-channel measurement
8.6.2.1 Start the analyzer, select the injection method, enter the measurement parameters, and stabilize 101in. 8.6.2.2 Place the conductive sample under the sample table, adjust the sample table height so that the outer electrode is immersed in the sample, and start the stirrer. 8.6.2.3 Open the measurement valve and inject the sample according to the selected injection method. 8.6.2.4 Select the print format and print out the measurement results. 9 Calculation of measurement results
9.1 Unit particle volume V:
9.2 Corresponding spherical particle diameter t
fK·y
9.3 Number of re-registered particles
Where:
--average number of particles.
--pore tube correction factor,
9.4 Actual number of particles N:
Ni+ - B
9.5 Semi-average volume area of ​​particles between adjacent channels:
9.6 Number of particles between adjacent channels Al
9. Total volume of particles V of the entire distribution
8 Percentage of particles less than 2 m
9.9 Percentage of particles less than 2 m in volume
9.10 Number of particles per liter between channels in raw water: SY/ T 0531 94
An=n- -
=× :00%
×100%
Note: Due to the limitation of the resistance induction method for determining the suspended particle size of injection water, the volume of particles below the effective detection limit of the pore can be estimated by the extrapolation technique in Appendix (reference document).
10 Precision
10.1 Repeatability
The same operator uses the same instrument. In a continuous period of time, according to the specified operating conditions. Repeated measurements of the same water sample shall not exceed ±3% relative error. Report format Appendix B (reference document)
SY/ T 053I-94
Measurement result recording format
(reference document)
% Wei Jiang
(uiur)
- -1=
SY/ T 0531-94
Sample category:
Sampling location:
Orifice tube diameter:
Self-lysate falling liquid concentration:
Sampling method
SY/ T 0531--94
Appendix B
Resistance induction method particle size analysis report format (reference)
Resistance induction method particle size analysis report
Sample name:
Date of closing:
Amount of electrolyte solution:
Standard particle diameter:
Siphon injection:
Fixed feed column:
Particle size (jrm)
Determiner:
Number of particles
Number of particles, %
Auditor:
Sample number:
Date of determination:
Sample amount:
Calibration constant:
Number of particles per liter
Manual sampling
Total number of injections
No.:
Volume,
Technical person responsible:
Cumulative volume. %
C1Extrapolation methodDouble logarithmic coordinate method
SY/ T 053194
Application of extrapolation technology
(reference)
C1.1 According to the effective measurement range of the selected orifice tube, select six lowest particle size points and set them as c:e, , g, H, j respectively.C1.2 Connect each point on the double logarithmic coordinates of (·V) and d into a smooth curve as shown in Figure C1.A
C1.3 Take c and two points with the lowest particle size among the six points, extend ec and intersect them at the ordinate point a, and then connect the vertical ordinate line from point c to point b,
Set five points so that bz equals 1/ 3ba, then point z can be regarded as 100% value, C1.4i
C1.5 Assume that the total volume after extrapolation is>V, then the estimated volume percentage is: MAnV
Additional Note:
This standard is proposed by the Technical Supervision Bureau of China National Petroleum Corporation. This standard is under the jurisdiction of the Planning and Design Institute of China National Petroleum Corporation. This standard was drafted by the Daqing Oilfield Design and Research Institute. x100%
The main drafters of this standard are Yupeng, Di Jinlong, Zhang Jinsu, Zhou Baochun, and Jiang Jinxiang. 102 Place the conductive sample under the sample stage, adjust the height of the sample stage so that the outer electrode is immersed in the sample, start the stirrer 8.6.2.3 Open the measuring valve, and inject the sample according to the selected injection method 8.6.2.4 Select the print format and print out the measurement results. 9 Calculation of measurement results
9.1 Unit particle volume V:
9.2 Corresponding spherical particle diameter t
fK·y
9.3 Number of repetitive particles
Where: - Average number of particles.
--pore correction factor,
9.4 Actual number of particles N:
Ni+ - B
9.5 Semi-average volume area of ​​particles between adjacent channels:
9.6 Number of particles between adjacent channels Al
9. Total volume of particles in the entire distribution V
8 Percentage of particles smaller than 2m
9.9 Percentage of volume of particles smaller than 2m
9.10 Number of particles per liter between channels in raw water: SY/ T 0531 94
An=n- -
=×: 00%
×100%
Note: Due to the limitations of the resistance induction method for determining the range of suspended particles in injection water, the volume of particles below the effective lower limit of the pore can be inferred using the extrapolation technology in Appendix (reference material).
10 Precision
10.1 Repeatability
The same operator uses the same instrument. In a continuous period of time, according to the specified operating conditions. Repeated measurements of the same water sample shall not exceed ±3% relative error in the measurement results. Report format Appendix B (reference document) SY/ T 053I-94 Measurement result recording format (reference document) % Wei Jiang (uiur) - -1=SY/ T 0531-94 Sample category: Sampling location: Orifice tube diameter: Autolysis liquid concentration: Sample escape method SY/ T 0531--94
Appendix B
Resistance induction method particle size analysis report format (reference)
Resistance induction method particle size analysis report
Sample name:
Date of closing:
Amount of electrolyte solution:
Standard particle diameter:
Siphon injection:
Fixed feed column:
Particle size (jrm)
Measurer:
Number of particles| |tt||Number of particles, %
Auditor:
Sample number:
Date of determination:
Sample amount:
Calibration constant:
Number of particles per liter
Manual sampling
Total number of injections
No.:
Volume,
Technical person responsible:
Cumulative volume. %
C1 extrapolation methodDouble logarithmic coordinate method
SY/ T 053194
Application of extrapolation technology
(reference)
C1.1 According to the effective measurement range of the selected orifice tube, select six lowest particle size points and set them as c:e, , g, H, j respectively.C1.2 Connect each point on the double logarithmic coordinates of (·V) and d into a smooth curve as shown in Figure C1.A
C1.3 Take c and two points with the lowest particle size among the six points, extend ec and intersect them at the ordinate point a, and then connect the vertical ordinate line from point c to point b,
Set five points so that bz equals 1/ 3ba, then point z can be regarded as 100% value, C1.4i
C1.5 Assume that the total volume after extrapolation is>V, then the estimated volume percentage is: MAnV
Additional Note:
This standard is proposed by the Technical Supervision Bureau of China National Petroleum Corporation. This standard is under the jurisdiction of the Planning and Design Institute of China National Petroleum Corporation. This standard was drafted by the Daqing Oilfield Design and Research Institute. x100%
The main drafters of this standard are Yupeng, Di Jinlong, Zhang Jinsu, Zhou Baochun, and Jiang Jinxiang. 102 Place the conductive sample under the sample stage, adjust the height of the sample stage so that the outer electrode is immersed in the sample, start the stirrer 8.6.2.3 Open the measuring valve, and inject the sample according to the selected injection method 8.6.2.4 Select the print format and print out the measurement results. 9 Calculation of measurement results
9.1 Unit particle volume V:
9.2 Corresponding spherical particle diameter t
fK·y
9.3 Number of repetitive particles
Where: - Average number of particles.
--pore correction factor,
9.4 Actual number of particles N:
Ni+ - B
9.5 Semi-average volume area of ​​particles between adjacent channels:
9.6 Number of particles between adjacent channels Al
9. Total volume of particles in the entire distribution V
8 Percentage of particles smaller than 2m
9.9 Percentage of volume of particles smaller than 2m
9.10 Number of particles per liter between channels in raw water: SY/ T 0531 94
An=n- -
=×: 00%
×100%
Note: Due to the limitations of the resistance induction method for determining the range of suspended particles in injection water, the volume of particles below the effective lower limit of the pore can be inferred using the extrapolation technology in Appendix (reference material).
10 Precisionwww.bzxz.net
10.1 Repeatability
The same operator uses the same instrument. In a continuous period of time, according to the specified operating conditions. Repeated measurements of the same water sample shall not exceed ±3% relative error in the measurement results. Report format Appendix B (reference document) SY/ T 053I-94 Measurement result recording format (reference document) % Wei Jiang (uiur) - -1=SY/ T 0531-94 Sample category: Sampling location: Orifice tube diameter: Autolysis liquid concentration: Sample escape method SY/ T 0531--94
Appendix B
Resistance induction method particle size analysis report format (reference)
Resistance induction method particle size analysis report
Sample name:
Date of closing:
Amount of electrolyte solution:
Standard particle diameter:
Siphon injection:
Fixed feed column:
Particle size (jrm)
Measurer:
Number of particles| |tt||Number of particles, %
Auditor:
Sample number:
Date of determination:
Sample amount:
Calibration constant:
Number of particles per liter
Manual sampling
Total number of injections
No.:
Volume,
Technical person responsible:
Cumulative volume. %
C1 extrapolation methodDouble logarithmic coordinate method
SY/ T 053194
Application of extrapolation technology
(reference)
C1.1 According to the effective measurement range of the selected orifice tube, select six lowest particle size points and set them as c:e, , g, H, j respectively.C1.2 Connect each point on the double logarithmic coordinates of (·V) and d into a smooth curve as shown in Figure C1.A
C1.3 Take c and two points with the lowest particle size among the six points, extend ec and intersect them at the ordinate point a, and then connect the vertical ordinate line from point c to point b,
Set five points so that bz equals 1/ 3ba, then point z can be regarded as 100% value, C1.4i
C1.5 Assume that the total volume after extrapolation is>V, then the estimated volume percentage is: MAnV
Additional Note:
This standard is proposed by the Technical Supervision Bureau of China National Petroleum Corporation. This standard is under the jurisdiction of the Planning and Design Institute of China National Petroleum Corporation. This standard was drafted by the Daqing Oilfield Design and Research Institute. x100%
The main drafters of this standard are Yupeng, Di Jinlong, Zhang Jinsu, Zhou Baochun, and Jiang Jinxiang. 10
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