SY/T 6526-2002 Determination of the dynamic reaction rate of hydrochloric acid and carbonate rock
Some standard content:
ICS 75.020
Registration No.: 10463—2002
Petroleum and Natural Gas Industry Standard of the People's Republic of China SY/T 6526—2002
Measuring method of dynamic reaction rate for hydrochloric acidwith carbonate rock
2002-05-28 Issued
National Economic and Trade Commission
2002-08-01 Implementation
2 Normative reference documents
3 Terms and definitions
4 Symbols
5 Instruments and materials
Sample preparation
7 Determination
8 Determination steps
9 Test report
Appendix A (Informative Appendix) Original records and test reports of acid rock dynamic reaction rate determination A.1 Original records of residual acid concentration changes in acid rock dynamic reaction rate determination A.2 Original records of acid rock dynamic reaction rate determination data A.3 Test report of acid rock dynamic reaction rate determination SYIT 6526-2002
SY/T 6526—2002
The dynamic reaction rate of hydrochloric acid and carbonate rock (abbreviated as acid rock dynamic reaction rate) is one of the important parameters for evaluating and selecting the performance of acid fracturing acid, and is also the basis for acid fracturing design. This standard is based on QCY256—1993 "Evaluation Method of Oil and Gas Acidizing Formula and Acid Energy" and Q/CY434-1997 "Measurement Method of Hydrochloric Acid/Carbonate Rock Dynamic Reaction Rate", summarizes the practical experience in recent years, and puts forward the technical requirements for the determination of acid rock dynamic reaction rate, so as to facilitate the evaluation of acid performance and provide a reliable technical decision-making basis for acid fracturing design and field implementation.
Appendix A of this standard is an informative appendix.
This standard is proposed by the Specialized Standardization Committee of Oil and Gas Production and is drafted by the Gas Process Research Institute of Southwest Oil and Gas Branch of China Petroleum and Natural Gas Co., Ltd. The main drafters of this standard are Li Li, Guo Jing, Yang Xu, Fan Qizhi, and Han Huifen. n
1 Scope
Determination method of dynamic reaction rate between hydrochloric acid and carbonate rockSY/T h526—2002
This standard specifies the determination method of dynamic reaction rate between acid and rock by titrating the residual acid concentration at the core outlet. This standard is applicable to the determination of dynamic reaction rate between hydrochloric acid solution system (hereinafter referred to as acid solution) and carbonate rock and the evaluation of acid solution performance.
2 Normative referenced documents
The clauses in the following documents become the clauses of this standard through reference in this standard. For any referenced document with a date, its subsequent amendment (excluding errata) or revision is not applicable to this standard. However, the parties who reach an agreement based on this standard are encouraged to use the latest versions of these documents. For any referenced document without a date, its latest version applies to this standard. GB/T601 Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) GB/T603-1988 Preparation of preparations and products used in test methods for chemical reagents Chemical reagents Hydrochloric acid
GB/I 622
GB/T 629
GB/T 1291
Chemical reagents Sodium hydroxide
Chemical reagents Potassium hydrogen phthalate
Specifications and test methods for water used in analytical laboratories GB/T 6682
GB/T10729 Chemical reagents Specifications
3 Terms and definitions
The following terms and definitions apply to this standard. rate
Acid-rock reaction rate
When hydrochloric acid reacts with carbonate rock, the amount of carbonate rock dissolved per unit time and per unit reaction area: 4 Symbols
The symbols used in the standard are as follows:
R,—dynamic reaction rate of acid rock, g/(cm2·s);A, the time when acid contacts the rock sample, cm2;
b, initial crack width, mm;
6, rock sample width, mm;
hi: 2, ha respectively The width of the rock sample measured three times, mm; cHc——molar concentration of residual acid solution, mol/L; CNaC
molarity of standard carboxylic acid hydroxide, mal爪
G——dissolution mass of the rock sample, g:
h-rock sample height, nm:
hi, h2, h2,——respectively the height of the rock sample measured three times, mm1-rock sample length, mm;
, 12——-respectively the length of the rock sample measured twice, mm: SY/T 6526—2002
t——sampling interval, s:
V——outlet acid volume, ml;
VlV—volume of sodium hydroxide standard solution consumed by sample 1 and sample 2, ml.:Vaug
V, the average of V, ml
volume of sodium hydroxide standard solution consumed, ml; linear acid mass fraction, %;
acid mass fraction, %;
residual acid density, g/ctnr;
Po—acid density, g/cm
Instruments and materials
5.1 Acid circulation tester and similar equipment
Acid circulation tester Acid-rock dynamic reaction rate determination system mainly includes storage tank, mixing machine, booster pump, system heater, acid reaction chamber, hydraulic press, cooling device and pressure Force sensor, temperature sensor and mass flowmeter etc. 5.1.1 Flow Diagram
The flow diagram of the system for measuring the dynamic reaction rate of acid rock is shown in Figure 18
, sample
1-acid tank: 2-oil tank, 3-water tank: 4-mixing pump: 5-system heater: (one increase:. Remainder: 7-experimental pipeline: 8-pipeline overflow sensor, 9-pressure sensor: 10-mass flow 11: 11 hydraulic press heating plate; 12-Junfa air conditioning: 13-water press lower acceleration plate: 14-cooling device: [5-waste liquid tank Figure 1 Flow Diagram of the System for Measuring the Dynamic Reaction Rate of Rock 5.1.2 Liquid Storage Tank
Acid tank 221., water tank 22L, oil tank 22L
5.1.3 System heater bZxz.net
Power 12kW, self-circulation system
5.1.4 Acid reaction chamber
Simulated slit width 0.5mr~5.Urun, deviation 1002mm. 5.1.5 Pressure sensor
Range 0.00MPa~13.79MP, code difference = 0.(5MP5.1.6 Temperature sensor
Range 0.0t--300.0℃, deviation ±0.1:5.1.7 Mass flow meter
Range 0.00kg/mm-20.00kg/mm, accuracy 11.0% 5.2 Other equipment
Vernier caliper; 0.00mm~300.00mm, graduation value 0.02mm; a)
b) Analytical balance: sensitivity 0.0001g;
Alkali burette: 0.00ml~25.00ml., graduation value 0.10ml; Density meter: specification 0.600g/cm2.00gh.m, graduation value .001g/md)
Pipette: 0.50rrl., graduation value 0.01l; e||tt| |Reagent bottle: 50ml.;
Conical flask: 100ml;
h) Measuring cylinder: 100mL, 200mL, 500ml., 1000ml.: Beaker: 100mL.500ml.:
J) Stopwatch: graduation value (.1s;
k) Oven: air temperature ~ 270C, temperature control accuracy ±1r5.3 Materials
a) Rock sample: specification 152.40mm×50.80mm×25.40mmb) Sealant: temperature resistance 150, repellency 10M1\a, acid resistance; phenolic acid: GB/T10729;
Hydrochloric acid: GB/T 622;
Sodium hydroxide: GB/T629;
Potassium hydrogen phthalate: GR/F1291;
g) Distilled water;
Design the additives in the acid solution formula.
6 Sample preparation
6.1 Rock sample preparation
6.1.1 Rock sample processing
SY/T 6526—2002
Cut the natural book core into two rectangular rock samples along the bedding plane. The rock sample specifications are 152.40mm×50.80mml×25.40mr, with a deviation of ±0.02mmm, and indicate the rock sample number.
6.1.2 Rock sample drying
Put the processed rock sample in the oven for drying. The drying temperature is controlled at 100.0105.06.1.3 Rock sample measurement
6.1.3.1 Use a vernier caliper to measure the length, width and height of the rock sample: the length is the inverse mean of the measurements in the orthogonal directions at both ends, and the width and height are the half-means of the three measurements between the two ends, respectively, recorded as 11, 12, 1, b, b2: b3, b, h, h2, h, and h6.1.3.2 Determine the area A and initial crack width b0c caused by the contact between the acid and the rock sample6.1.3.3 Fill the measured values into the original record table for the determination of the dynamic reaction rate of acid rock. For the table form, see Table A.2.6.1.4 Gluing rock samples
stone.1.4.1 Place two samples in the two side plates respectively. Apply 1. Hub-resistant sealant to the edge of the rock sample and the groove and the four sides of the rock sample. No bubbles should be allowed when applying the sealant.
6.1.4.2 Leave for 24 hours to allow the glue to fully cure. The ideal pseudo-curing conditions are room temperature and relative humidity of 70%. SY/T 6526--2002
6.2 Preparation of reagents
6.2.1 Preparation of phenolic indicator solution
The preparation of phenolic indicator solution shall be prepared according to 4.5.22 of GH/I603-1988. 6.2.2 Preparation of distilled water
The preparation of distilled water shall be prepared according to the first-class water specification in GF/T6682. 6.2.3 Preparation and calibration of sodium hydroxide standard solution The preparation and calibration of sodium hydroxide standard solution shall be carried out in accordance with the provisions of GB/T601. e6.2.4 Preparation of acid solution
H) Preparation quantity: 20I.
[) Preparation of hydrochloric acid solution shall be prepared in accordance with 4.3.24 of (GB/T(03-1988) c) According to the ratio, add the required additives to the hydrochloric acid solution according to the preparation requirements, mix well, and prepare acid solution. d) Titrate the acid solution with the prepared sodium hydrocyanide standard solution, and calculate the acid solution concentration. 7 Preparation
7.1 Inspection of instruments and equipment
a) Check whether the measuring instruments of the instruments and equipment are within the calibration validity period. b) Check the water, electricity and gas lines of the instruments and equipment: e) Check all pipelines and valves for leaks. d) Check that there is no residual liquid in the outflow pipe of the acid reaction chamber. 7.2 Assemble the acid reaction chamber
a) Describe the surface of the rock sample and make a record. h) Install the sealing ring, place the center piece between the two side pieces, and tighten all the screws with a torque wrench. The maximum torque is 40Vm (30lif-t): See Figure 2 for the schematic diagram of the acid reaction chamber structure. c) Place the acid reaction chamber between the two cutting plates of the water climbing machine, connect the inflow and outflow pipelines of the acid reaction chamber, and insert the temperature sensor.
1 Acid liquid inlet; 2--Temperature sensor plug; 3-Acid liquid outlet 4-Sealing glue; 5-Upper crack, 6-Rock sample, 7-Side piece, 8-Core piece
Figure 2 Schematic diagram of the acid reaction chamber structure
7.3 Reserve liquid
7.3.1 Acid fin
Put the prepared acid liquid into the acid chamber for the experiment. 7.3.2 Water tank
Fill the water tank with fresh water to prepare for flushing the instrument pipeline. 8 Measurement steps
8.1 Preheating
Turn on the instrument power supply and preheat for 30mln.
8.2 Setting the number of silkworms
a) Temperature: reservoir temperature.
b) Pressure: 6MPaa
Slit width: 0.5mm~5.0mm
d) Flow rate: The shear rate of acid flow should be within the range of 100s-1~1000s-1. 8.3 Start the computer and enter the experimental program
Monitor the temperature curve until the temperature value reaches the set temperature. a)
Set the flow rate to displace the liquid in the pipeline until the pipeline is full of acid. Set the pressure, turn on the acid tank switch, pipeline switch and acid reaction chamber switch. SY/T6526—2002
Start the mixing pump and the booster pump, and continuously pump fresh acid into the acid reaction chamber at the set pressure and flow rate. d)
The residual acid after the acid and the sample react is sampled at the sampling point through the cooling device. When the acid appears at the sampling point, start the timing, and sample once every 305, and the continuous sampling shall not be less than 7 check points. f
Measure the volume and density of the residual acid at the outlet of the reaction chamber and titrate the residual acid concentration. g
After the test, release the pressure and the pipeline temperature drops below 40℃, and pump in clean water to flush the pipeline and the acid reaction rate. h)
Discharge the liquid acid solution of the flushing pipeline into the waste liquid tank, treat it with acid and alkali to pH 7, and then discharge it into the wastewater pool: 1)
) Remove the inflow and outflow arm lines and temperature sensor of the acid reaction chamber, dismantle the acid reaction chamber, observe the acid corrosion phenomenon on the surface of the rock sample, and make records or take photos.
8.4 Titration of residual acid solution concentration
8.4.1 Sampling
Use a 0.5mL pipette to transfer 0.2mL of residual acid solution into a conical flask, take 2 drops, add 2011-30 distilled water to dilute, 8.4.2 Titration
a) Add 2 drops of phenol indicator solution to the diluted sample. Use sodium hydroxide standard solution to titrate the pink color in the solution. If the pink color does not disappear after 30 seconds, record the volumes of sodium hydroxide standard solution Vl and V2 consumed. The maximum deviation cannot exceed 0.10 ml. Otherwise, take the residual acid sample for titration again and take the average value of Vi and V, recorded as Vi. Fill in the titration data in the original record table of residual acid concentration change in the acid-rock dynamic reaction rate determination. For the tabular form, see Table A.1 in Record A).
8.4.3 Calculation
The molar concentration of residual acid solution cHc is calculated according to (1): CIK
The mass fraction of residual acid uH is calculated according to formula (2): NHVNE
36.5c ×100%
EIK1000PHI
8.5 Calculation of dynamic reaction rate of acid rock
The dynamic reaction rate of acid rock R is calculated according to formula (3): (1)
SY/T 6526—2002
The dissolution mass of limestone G is calculated according to formula (4): R.
G =1.3699V (zenpnep1m3)
The insoluble mass G of dolomite is calculated according to formula (5): G=1.2603V(wu-OH)
Test report
The test report includes the following contents:
) Report abbreviation, name of test item, entrusting unit, test category, test period and test location. Sample name, sample specification, sample quantity, sample status/characteristic description and sample delivery date. h
Test basis, test equipment, equipment number, test conditions and test environment conditions. d) Test results.
Signatures of test personnel, reviewer and approver 6
Appendix A
[Informative Appendix]
Original records and test report of acid-rock dynamic reaction rate determination A.1 Original records of residual acid concentration changes in acid-rock dynamic reaction rate determination The original records of residual acid concentration changes in acid-rock dynamic reaction rate determination are shown in Table A.1 Table A,1 Original records of residual acid concentration changes in acid-rock dynamic reaction rate determination Test Phase II
Acid concentration formula
Acid liquid density
Tester,
Residual acid liquid
Residual acid liquid||tt ||Sodium hydroxide standard solution
Molar concentration,
Acid mass fraction, %
Residual acid sample volume
Consumed volume of sodium hydroxide standard solution
Reviewer
A.2 Original record of determination data of dynamic reaction rate of acid rock. The original record table of determination data of dynamic reaction rate of acid rock is shown in Table A.2V2
Table A, original record table of determination data of dynamic reaction rate of acid rock. Rock sample
Sample number
Rock sample length, mn.
Rock width, nm
SY/T 6526--2002
Total 5 pages
Residual acid solution
Xier Nongzhi
Residual acid was
Mass fraction
Total page
Rock sample height, nun
SY/T 6526—2002
Acid formula
Acid mass fraction, %
Temperature, C
Flow, /s
Acid and rock sample contact area A, m
Before detection:
Tester
Residual acid liquid
Mass fraction
A,3 Acid-rock dynamic reaction rate determination test report Table A.2 (continued)
Experimental data
Residual acid liquid
Reviewer:
Acid-rock dynamic reaction rate determination test report See Table A.3. Consumed rock mass
Acid density, g/m
Pressure, MPa
Initial crack width,
Test period
After test:
Consumed rock
Rock volume
Crack width
Table A.3 Acid-rock dynamic reaction rate determination test report Report No.:
Product/Sample
Entrusting Unit
Entrusting Unit
Test Type
Product Model and Specification
Registered Trademark Name
Or Sample No.
Controlled Environment Conditions
Production/Sampling Unit
Sample Status. Special
Acid volume, L
Reaction rate
g/(cm2.s)
Product/sample
Sampling unit
Sample base
Sample received
Testing date
Ten requirements for testing
Instruments and equipment
Testing personnel and
Testing date
Table A.3 (continued)
Sampling location
Sampling, sample delivery period
Testing item name
Testing basis
Testing location
(Inside or outside the laboratory)
Auditor and
Audit date
SY/T 6526--2002
Special seal for testing unit
Issuing period:
Approving person and
Issuing date
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