Some standard content:
ICS 75.180.99
Registration No.: 8190—2001
Petroleum and Natural Gas Industry Standard of the People's Republic of ChinaSY/T55032000
The method for measurement of chloride content in rock2000-12-25Promulgated by the State Petroleum and Chemical Industry Bureau
2001-06-01Implementation
SY/T5503—2000
1Scope
3Apparatus and reagents
4Rock sample collection and chloride extraction
5Determination method
6Numerical value rounding
7Quality requirements·
8Original record content and format
Appendix A (Appendix to the standard)Original record content and format of rock cooked salt content determinationSY/T 5503—2000
This standard is revised on the basis of SY/T5503-92 "Method for determination of chloride content in rocks", and the main revisions are as follows:
1) The content and format are revised according to the provisions of GHB/T1,1-1993; 2) Chapter 2 "Principles" is added;
3) 2.3 of SY/T5503-92 is revised; 4) Chapter 6 "Numerical rounding" is added; 5) 4.2.5 of SY/T5503-92 is revised to Chapter 7 of this standard; 6) The original record table of SY/T5503-92 is revised. See the appendix of this standard A (Appendix to the standard): This standard replaces SY/T5503-92 from the date of entry into force. Appendix A of this standard is the appendix to the standard.
This standard is proposed by China National Petroleum Corporation. This standard is sponsored by the Oil and Gas Field Development Professional Standardization Committee: The drafting unit of this standard is: Exploration and Development Science Research Institute of Zhongyuan Oil Company, China Petrochemical Corporation. The main drafters of this standard are Zou Xing, Qiao Guoan, Zhao Xiaolin, He Jiang, and Wang Shuangfeng. This standard was first issued in November 1992, and this is the first revision. V
Petroleum and Natural Gas Industry Standard of the People's Republic of China Method for measuring chloride content in rock
The method for measuring chloride content in rock This standard specifies the method and technical requirements for measuring chloride content in rock. This standard is applicable to sandstone cemented rock. Other types of samples can also be implemented as a reference. 2 Principle
SY/T 55032000
Replaces SY/T5503-92
The rock sample is soaked and extracted with distilled water. After all the water-soluble chloride salts in the rock sample are dissolved in the benzene solution, it is filtered and the chloride ion content in the extract is determined, and then the chloride salt content of the rock sample is calculated. 3 Instruments and reagents
3.1 Instruments
a) Salt content tester;
b) Balance: sensitivity 0.1mg
c) Blast constant temperature T drying box;
d) High temperature furnace: air temperature ~800℃;
e) Speed regulating oscillator;
) Titration Tube: brown, 25rnl; white, 5Unl; g) Wide-mouth bottle: with stopper, 60mL;
h) Pipette: 10, 20, 25mL;
i) Erlenmeyer flask;
i) Funnel;
k) Microinjector: 10, 50zL;
I) Narrow-mouth bottle: brown, with stopper, 2500mL; m) Volumetric flask: 1000ml.;
n) Mortar;
o) Standard sieve: pore size 0.6mm;
p) Filter paper: qualitative;
q) pH test paper: 1~14.
3.2 Reagents
a) Sodium chloride (NaCI);
h) Potassium chromate (KzCrO);
c) Silver nitrate (AgNOs);
d) Potassium aluminum sulfate [KAl(S)4-{2HO];
e) Ketone sand (NazB4O-10H2O);
f) Nitric acid (HNO,);
State Administration of Petroleum and Chemical Industry 2000-12-25 Approved for implementation on June 1, 2001
g) Hydrogen peroxide (HO2):
h) Silver acetate (CH,COOAg);
i) Glacial acetic acid (CHCOOH).
All reagents used are analytically pure.
3.3 Solution preparation
SY/T5503—2000
3.3.1 CAeNo,=0.0250mol/L silver nitrate standard solution3.3.1.1 Preparation of silver nitrate solution
Weigh 4.2470g silver nitrate and dissolve it in 1000mL distilled water, store it in a brown stoppered reagent bottle, and use it after calibration. Different concentrations can be prepared according to the salt content of the rock Degree solution. Use and store it and calibrate it once every three months. 3.3.1.2 Calibration of silver nitrate solution
a) Weigh 1.4610g of sodium chloride burned to constant weight at 550℃±50℃ in a beaker, dissolve it with a small amount of distilled water, transfer it to a 1000mL volumetric flask, dilute to the scale, and shake well. The concentration of this solution is Cac=0.0250mol/L; b) Pipette 20mL of the prepared sodium chloride standard solution into a conical flask, take another conical flask and add 20mL of distilled water for a blank experiment; c) Add 5 drops (about 0.2mL) of potassium chromate solution (see 3.3.2) to the solution as an indicator, and titrate with the silver nitrate solution to be calibrated until the solution changes from yellow to orange-red, and record it. The consumption of silver nitrate solution V2 is used to titrate the blank solution at the same time, and the consumption of silver nitrate solution V is recorded. d) Calculate the concentration of the silver nitrate standard solution CAeNO, according to formula (1): CNacr×20
CAgNO,=V2-Vi
Wherein: CANO,
concentration of the silver nitrate standard solution, mol/; concentration of the sodium chloride solution, Inol/L;
amount of silver nitrate solution consumed when titrating the blank solution, mL; Vi
amount of silver nitrate solution consumed when titrating the sodium chloride solution, MLV
3.3.2 Potassium chromate solution
Weigh 5g of potassium chromate and dissolve it in a small amount of distilled water. Add nitric acid. Silver acid solution (see 3.3.1) until orange-red does not fade, filter after 24 hours, and dilute to 100mL with distilled water.
3.3.3 Borax solution
Weigh 5g borax and dissolve it in 100mL distilled water, shake well. 3.3.4 Dilute nitric acid solution
Add 1 part of concentrated nitric acid to 20 parts of distilled water.
3.3.5 Electrolyte
Measure 700mL glacial acetic acid, add 300mL distilled water, mix well 4 Rock sample collection and chloride salt extraction
4.1 Take about 30g sample from the center of the fresh core (uncontaminated): crush and sieve (0.6mm standard sieve) and put it in an oven, and bake it at 105℃±5℃ for 4h.
4.2 Weigh 10~15g of rock sample, weigh to 0.001g, and put it into a 100mL wide-mouth bottle, add about 0.3g of potassium aluminum sulfate, add 25mL of distilled water, cover the bottle, shake on the oscillator for 30min (or shake by hand for 3min), and let it stand and soak for more than 6h. For oil-containing rock samples, first add a small amount of distilled water to make the rock sample into a paste, and then add water to 25mL. 4.3 After the extract is clarified, filter it with qualitative filter paper into a dry wide-mouth bottle for testing. 4.4 For rock samples containing more heavy oil, first weigh 1015g, weigh to 0.001g: put it in a triangular flask, add 25mL of toluene and soak it for 24h, add 25mL of distilled water after the particles are dispersed, soak for 24h, and take its aqueous solution for testing. 5 Determination method
5.1 Silver nitrate titration methodbzxZ.net
5.1.1 Principle
SY/T5503-2000
The salt solution extracted from the rock sample is titrated with silver nitrate standard solution using potassium chromate as indicator. Silver nitrate reacts with chloride ions to form a white precipitate, and excess silver ions react with potassium chromate indicator to form an orange-red silver chromate precipitate. The chloride ion content is calculated based on the consumption of silver nitrate. The reaction equation is as follows:
Agt+C-
2Ag*+CrOh
5.1.2 Determination steps
+AgCl
Ag2CrO4
Orange-red
5.1.2.1 Use a pipette to accurately draw 10mL of the extract into a conical flask, add 5 drops of potassium chromate solution, and titrate with silver nitrate standard solution until the solution changes from yellow to orange-red. Record the consumption of silver nitrate standard solution V3. 5.1.2.2 Use a pipette to accurately draw 10mL of distilled water for sample immersion and place it in another conical flask, add a small amount of potassium aluminum sulfate, repeat the operation in 5.1.2.1, perform blank titration, and record the consumption of silver nitrate standard solution V45.1.2.3 Calculation of measurement results
The chloride content in the rock sample is calculated according to formula (2): B-58.44×Ch:V.(Vs-Va)×103
Wherein: B——chloride content in the rock sample, mg/kg; C
concentration of silver nitrate standard solution, mol/L; -total volume of extract, mL;
-consumption of silver nitrate standard solution when measuring the sample, mL; V
-consumption of silver nitrate standard solution when measuring the blank, mL; V
Weigh the mass of the rock sample, g;
58.44——molar mass of sodium chloride, g/mol. 5.1.3 Precautions
(2)
a) The pH value of the benzene solution should be between 6.3 and 10.0 during titration. If it is lower than 6.3, add an appropriate amount of borax solution for neutralization; if it is higher than 10.0, add dilute nitric acid for neutralization;
b) If there is interference from hydrogen sulfide, add a few drops of 30% hydrogen peroxide to eliminate the interference. 5.2 Coulometric method
5.2.1 Principle
When the salt-containing aqueous solution is injected into the titration cell, chloride ions and silver ions react, and the silver ions consumed in the reaction are replenished by electrolysis at the anode. By measuring the amount of electricity consumed by the electrogenerated silver ions, the chloride ion content in the solution can be calculated according to Faraday's law. 5.2.2 Instrument calibration
5.2.2.1 Install and debug the instrument according to the instrument manual. 5.2.2.2 Select the value of the integral resistor R according to the salt content. 5.2.2.3 Start the instrument digital tube and adjust to zero. 5.2.2.4 Determine the instrument recovery rate.
Use a syringe to inject 10uL of a sodium chloride standard solution with a concentration of 0.0250mol/L into the titration cell. When the digital tube reading remains unchanged, record the reading A.
The chloride content of the standard sample is calculated according to formula (3): 3
SY/T 5503-2000
100 ×A
Cl = R x2. 722 ×0.606 × V
Where: Ci---standard sample chloride content, mg/L: A-digital tube reading;
V.--injected standard sample volume, ul;
R--integral resistance, i.e. range selection value, 2; 100--each integral value is equivalent to 100uV·s2.722--the amount of electricity consumed by 1mg chloride ion, μC; 0.606--CI/NaCI conversion factor The instrument recovery rate is calculated according to formula (4):
Where: R--recovery rate, %;
Cl--standard sample chloride content, mg/L; Ca--standard chloride content, mg/L;
When the recovery rate is within the range of 100%±10%, the instrument is in normal working condition and the sample can be measured. 5.2.3 Measurement steps
5.2.3.1 Zero the instrument digital tube.
5.2.3.2 Use a micro-injector to take 5-10 ml of the extract to be tested, and inject it into the titration cell. When the digital tube reading remains unchanged, record the reading. A5.2.4 Calculation of measurement results
The rock chloride content is calculated according to formula (5):
Where: Vs——the volume of the extracted solution injected, pL;60.56 Instrument measurement calculation constant
6 Numerical rounding
The rock nitrogen content measurement result is rounded to the single digit, the unit is mg/kg.7 Quality requirements
7.1 Take two samples of each batch of rock samples at a ratio of 10% for random inspection. When the number of samples exceeding the relative deviation accounts for 30% of the number of suppressed samples, the entire batch of samples shall be re-measured.
7,2 The relative deviation of the double sample determination is;
Chloride content>500mg/kg, relative deviation<10%; chloride content<500mg/kg, relative deviation<30%. 8 Original record content and format
The original record content and format of rock chloride content determination (titration method) are shown in Table A1 in Appendix A (Appendix to the standard). The original record content and format of rock chloride content determination (coulometric method) are shown in Table A2 in Appendix A (Appendix to the standard). SY/T 5503--2000
Appendix A
(Appendix to the standard)
The original record content and format of rock chloride content determination (titration method) are shown in Table AI. A1
Table A Rock Chloride Content Determination (Titration Method) Original Record Well No.:
Analyst:
Rock Sample Quality Plate
CaeNo,
Add Distilled Water to Take Extract
Verifier:
AgNC Liquid Titration Reading
AgNO Blank Chloride Content
Ing/kg
SY/T5503—2MHO
A2 Rock Chloride Content Determination (Coulometry Method) Original Record Content and Format See Table A2 Table A2 Rock Chloride Content Determination (Coulometry Method) Original Record Well No.:
Analyst:
Rock Sample Quality
Add Distilled Water Volume Inject Benzene to Take Extract
Verifier:
Instrument Reading
Year Month Day
Chloride Content1Double samples are taken for random inspection at a ratio of 10% for each batch of rock samples. When the number of samples exceeding the relative deviation accounts for 30% of the total number of samples, the whole batch of samples shall be re-measured.
7,2 The relative deviation of double sample determination is;
Chloride content>500mg/kg, relative deviation<10%; chloride content<500mg/kg, relative deviation<30%. 8 Original record content and format
The original record content and format of rock chloride content determination (titration method) are shown in Table A1 in Appendix A (Appendix to the standard). The original record content and format of rock chloride content determination (coulometric method) are shown in Table A2 in Appendix A (Appendix to the standard). SY/T 5503--2000
Appendix A
(Appendix to the standard)
The original record content and format of rock chloride content determination (titration method) are shown in Table AI. A1
Table A Rock Chloride Content Determination (Titration Method) Original Record Well No.:
Analyst:
Rock Sample Quality Plate
CaeNo,
Add Distilled Water to Take Extract
Verifier:
AgNC Liquid Titration Reading
AgNO Blank Chloride Content
Ing/kg
SY/T5503—2MHO
A2 Rock Chloride Content Determination (Coulometry Method) Original Record Content and Format See Table A2 Table A2 Rock Chloride Content Determination (Coulometry Method) Original Record Well No.:
Analyst:
Rock Sample Quality
Add Distilled Water Volume Inject Benzene to Take Extract
Verifier:
Instrument Reading
Year Month Day
Chloride Content1Double samples are taken for random inspection at a ratio of 10% for each batch of rock samples. When the number of samples exceeding the relative deviation accounts for 30% of the total number of samples, the whole batch of samples shall be re-measured.
7,2 The relative deviation of double sample determination is;
Chloride content>500mg/kg, relative deviation<10%; chloride content<500mg/kg, relative deviation<30%. 8 Original record content and format
The original record content and format of rock chloride content determination (titration method) are shown in Table A1 in Appendix A (Appendix to the standard). The original record content and format of rock chloride content determination (coulometric method) are shown in Table A2 in Appendix A (Appendix to the standard). SY/T 5503--2000
Appendix A
(Appendix to the standard)
The original record content and format of rock chloride content determination (titration method) are shown in Table AI. A1
Table A Rock Chloride Content Determination (Titration Method) Original Record Well No.:
Analyst:
Rock Sample Quality Plate
CaeNo,
Add Distilled Water to Take Extract
Verifier:
AgNC Liquid Titration Reading
AgNO Blank Chloride Content
Ing/kg
SY/T5503—2MHO
A2 Rock Chloride Content Determination (Coulometry Method) Original Record Content and Format See Table A2 Table A2 Rock Chloride Content Determination (Coulometry Method) Original Record Well No.:
Analyst:
Rock Sample Quality
Add Distilled Water Volume Inject Benzene to Take Extract
Verifier:
Instrument Reading
Year Month Day
Chloride Content
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