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People's Republic of China Petroleum and Natural Gas Industry Standard SY/T 5061-93
Limestone Powder for Drilling Fluid
Published on September 9, 1993
China National Petroleum Corporation
Implemented on March 1, 1994
Main Contents and Scope of Application
People's Republic of China Petroleum and Natural Gas Industry Standard Limestone Powder for Drilling Fluid
SY/T 5061—93
This standard specifies the quality indicators, test methods, inspection rules, packaging, marking, etc. of limestone powder for drilling fluid. This standard applies to limestone powder for drilling, completion and workover fluids. Reference Standards
GB5005 Barite powder for drilling fluid
Preparation of standard solution for titration analysis (volume analysis) of chemical reagents 6011
3 Technical indicators
Numerical rounding rules
Limestone powder should meet the performance requirements specified in the following table. Item
Density,
Calcium carbonate content,
Acid insoluble content,
Water soluble content,
4 Test methods
4.1 Instruments and equipment
0.076mm Residue on sieve,
Content of particles less than 6um
8.Agitator: speed is 200～400r/minb.Constant temperature drying oven: control temperature ±2°℃;c.Constant temperature water bath: constant temperature sensitivity +0.1℃;%
d.Super constant temperature water bath: constant temperature sensitivity ±0.1℃Ce:Direct reading rotational viscometer: Fan 35 type or similar viscometer,f.High speed stirrer: GT:1 type or similar products;g.Electric furnace: 1000w
h.Lee density bottle: scale value 0.1cm2
i.Analytical balance: sensitivity 0.1mg:
j.Torsion balance, sensitivity 0.01g;
k. Standard sieve: 0.076mm aperture;
Approved by China National Petroleum Corporation on September 9, 1993
Implementation on March 1, 1994
SY/T 506193
1. Wet screener: Wet screener (7.6cm in diameter, 6.3cm in height) has screens with mesh diameters of 0.076mm and 0.043mm and a pressure gauge (including a pressure regulator)
m. Glass sieve: No. 2, 40cm;
n. Dryer: inner diameter 18cm
0. Thermometer: 0~100℃, graduation value 0.2℃;p. Stopwatch: accuracy 0.1s:
q Bonao measuring cylinder: about 15cm in height, about 6cm in diameter, scale 1000ml;r. Evaporation III: diameter 10crm;
s. Burette: acid type 25ml, graduation value 0.1nml:t. Sand core funnel: 3#;
u. Conical flask: 250ml.
4. 2 Reagents and materials
a: Anhydrous kerosene: Add 200g of chemically pure anhydrous calcium fluoride to 5kg of commercially available kerosene, shake for 5min and let stand for 24h, take the supernatant (if turbid, filter it)
b. Calcium carbonate, high-grade pure;
c. Sodium hydroxide: chemically pure:
d. Hydrochloric acid: chemically pure,
e. Triethanolamine: chemically pure,
f, Calcium indicator: 150 (calcium reagent, potassium chloride)g. EDTA standard solution: 0.0250mol/1. Prepared according to Article 4.15 of GB601;h: Calcium standard push solution: 0.0250mol/1.
i. Dispersing solution: 40g sodium hexametaphosphate and 3.6g sodium carbonate are mixed into 1000ml solution (when the pH value of the solution is less than 8, it should be re-prepared). 4.3 Test Procedure
4.3.1 Density Determination
4.3.1.1 Use a long-necked funnel to add anhydrous kerosene to the neck of a dry, clean density bottle, then wipe off the kerosene splashed from the neck with filter paper and cover the bottle with a stopper. Place it in a constant-temperature water bath so that the meniscus of the kerosene at the neck is below the water surface. Adjust the temperature of the constant-overflow water bath to be about 10°C higher than the room temperature, but the constant temperature change should be controlled within ±0.1°C. After 30 minutes of constant temperature, read the initial volume of kerosene in the constant-temperature water bath (the density bottle can also be taken out of the constant-temperature water bath and the kerosene volume can be read within 5 seconds). 4.3.1.2 Weigh 65g of the sample dried at 105±3°C for 2h (accurate to 0.01g), add it to the density bottle through a short-necked funnel, and cover the bottle with a stopper. Tap, roll or shake the density bottle to remove the mixed air, and place the density bottle in a constant temperature water bath for 30 minutes. 4.3.1.3 Take out the density bottle, tap, roll or shake the density bottle again to remove the remaining air. Place the density bottle in a constant temperature water bath again, and keep the constant temperature for 30 minutes. Immediately read the final volume.
4.3.1.4 Calculate
p--density of limestone powder, g/cm;
Where:
-mass of the sample, g;
V——final kerosene volume in the density bottle, ml; V----initial kerosene volume in the density bottle, nil. 4.3.2 Fineness determination
4.3.2.1 Weigh 50g (accurate to 0.01g) of the sample dried at 105-3°C for 2h, add it to a beaker containing 350ml of distilled water, stir it with a glass rod for 5min, then transfer the suspension into a standard sieve with a pore size of 0.076mm, and rinse the residue on the beaker wall with distilled water into the standard sieve.
4.3.2.2 Use a nozzle to spray water with a pressure of 6!kPa to rinse the sample on the sieve for 2min. When flushing, let the nozzle tip rest on the edge of the sieve: SY/T5061-93
and move the nozzle back and forth on the sieve surface to flush
4.3.2.3 After flushing the sieve residue on the sieve with distilled water twice, transfer it to an evaporating dish of known mass, evaporate it in a water bath until dry, then put it in a drying oven, dry it at 105±3℃ for 2h, take it out and put it in a desiccator, and weigh the evaporation blood and sieve residue after cooling to room temperature. 4.3.2.4 Calculate
S=m-mz×100
S-residue passing through 0.076mm mesh, %, where: Pan
m:-evaporation blood and sieve residue plate·g:
m2-mass of empty evaporating dish, g,
mass of sample, g.
4.3.3 Determination of the content of particles less than 6um
4.3.3.1 Weigh 65g of the sample dried at 105±3℃ for 2h and place it in a high stirring cup. Add 125ml of the dispersion solution, stir the sample with a plastic stick (or this stick) and dilute it to 400ml with distilled water. 4.3.3.2 Stir for 5min on a high-speed stirrer, transfer the liquid into a 1000ml measuring cylinder, rinse all the sample into the measuring cylinder and dilute it to the 1000ml mark with distilled water. After stirring the sample, turn the measuring cylinder upside down 20 times for about 1min (use your palm or rubber cloth to hold the measuring cylinder tightly).
4.3.3-3 When the measuring cylinder is turned upside down for the last time, immediately put it steady and start timing, and insert the thermometer into the suspension at the same time. Read 30.10.50, 60, 70, 80mni n, the readings of the liquid density meter and the thermometer. Calculate the corresponding diameter (D) and its weight percentage (S,). 4.3.3.4 When the rate meter reading is required, the liquid density meter should be carefully inserted to a depth approximately equal to the reading value 20 to 30 seconds before the scheduled reading time. After the reading, the liquid density meter should be immediately and carefully removed, cleaned with distilled water and wiped dry. 4.3.3.5 Calculation
4.3.3.5.1 The particle diameter D can be calculated according to formula (3): 30mL
D)=100 980 (p-1) T
I)—equivalent Stokes diameter, μm;
Where:
7—viscosity of water at the experimental temperature, m·Pa·5 (see Appendix C); L—effective depth of the density meter, cm (its calculation is shown in formula (5)); T—time interval from the start of sedimentation to the reading value, min;. - Density of the sample, g/cm2.
4.3.3.5.2 The percentage of particles with a diameter of D is calculated according to formula (4): Su
100000g
m (p-1)
Wherein: Sp—weight percentage of particles with a diameter of L, %; - Mass of the sample, area:
p-density of the sample, g/cm2;
Hc—densitometer reading—comprehensive correction value (see note). The effective depth (L) of the densitometer is calculated according to formula (5): (He-1)
1=L,+ [I2-C (V/A)] /2
L:—the distance from the top of the densitometer glass bulb to the scale of the reading, cm,Where:
L--length of the glass bulb of the densitometer, cm;
V--volume of the glass bulb of the densitometer, cm\;
A--cross-sectional area of the inner hole of the glass cylinder, cm2. 4.3.3.5.3 The percentage content S of particles with a diameter less than 6um in the sample can be calculated according to formula (6): S
-Ina-Inb
(In6-ln6) +$e
SY/T 5061---93
Where: S--percentage content of particles with a diameter equal to 6um, %; a, 6--particle diameters of the measuring points larger and smaller than 6um and adjacent to them, respectively. S, Su--percentage content of particles larger and smaller than their own diameters α and ·%, respectively. Note: The comprehensive calibration is determined by the following test: put 125 ml of the dispersion in a glass measuring tube, add distilled water to dilute to 1000 ml, put the measuring tube in a thermostatic bath, measure the density of the suspension at different temperatures, read the value at the top of the crescent, and subtract 1 from the value as the comprehensive calibration value. 4.3.4 Determination of water-soluble matter
4.3.4.1 Weigh 25 g of the sample dried at 1053°C for 2 hours (accurate to 0.01 g), put it in a 200 ml beaker, add 50 ml of distilled water, stir with a glass for 5 minutes, let it clarify, and pour the clarified liquid onto a medium-speed qualitative filter paper. Add 50 ml of distilled water, stir for 5 minutes, clarify and filter, and repeat the above
4.3.4.2 Combine the three clarified liquids, transfer to an evaporating dish of known mass, and evaporate to dryness in a water bath. Then dry it in a flat drying oven at 105-s℃ for 2h: take it out and put it in a desiccator, wait until it cools to room temperature, weigh the mass of the evaporated substance and the dry solid. 4.3.4.3 Calculation of
:
m2--evaporated substance mass.%:
m,--sample mass, H.
4.3.5 Determination of acid-insoluble matter
4.3.5.1 Weigh 1g of the sample dried at 10;3:3 for 2h (accurate to 0.01), put it into a 200ml beaker, add 25ml of 15% hydrochloric acid, cover it, wait until the reaction stops, transfer it into a glass vortex for suction filtration, and wash it with steamed water until there is no chloride ion (use 1% (m/m) silver nitrate solution to check the fragrance).
4.3.5.2 Place the glass in a dry oven at 150+3℃ and dry for 2h, take it out and place it in a desiccator, and weigh it after cooling to room temperature. 4.3.5.3 Calculate
acid insoluble matter × 100%,
where: _——mass of glass and residue, g: _——mass of glass crucible, g
-mass of sample, g
4.3.6 Determination of calcium carbonate
4.3.6.1 Summary of the method
Treat the sample with dilute acid. Filter after calcium carbonate is completely dissolved. Use triethanolamine as a blocking agent and calcium reagent as an indicator. 4.3.6.2 Operation steps: Accurately weigh 1g of the sample dried at 105-3℃ (weighing to 0.01g), place it in a 250ml beaker, add a small amount of distilled water (about 2ml) and 25ml of dilute hydrochloric acid, and after the reaction stops, heat to boiling to remove CO, filter, discard the residue, and transfer all the filtrate to a 1000ml container. Dilute to the scale and shake, aspirate 25ml of the solution, add 25ml of water, add 0ml of diethanolamine, then add 5tml of sodium hydroxide and 10mg of calcium indicator, and add EDTA standard solution until the solution changes from red to purple and then to pure blue. 4.3.6.3 Calcium carbonate content - In the formula: M. Concentration of FDTA, mol/I.;
Amount of VEDTA, cm\;
MxVx0.100J
1×100%
mX25/1000
m Sample mass: g; bZxz.net
0.1001-· Gram equivalent of calcium carbonate.
4.3.7 Test report
The test report is shown in Appendix A (Supplement).
4.3.8 Precision
SY/T 5061—93
When the parallel values determined by the same operator are within the following allowable error range, take the arithmetic mean. a. Shake:
b. Fineness:
C. Acid insoluble matter:
d. Water soluble matter:
e. Calcium carbonate:
4.3.9 Value rounding
0. 02g/cm:
According to GB 8170.
5 Inspection rules
5.1 When sampling from bagged limestone powder, the sampler shall be used to arrange sampling points at different positions of the upper, middle and lower parts of each side according to the stacking height, shape and quantity. Each batch shall not be less than 15, and the sample quantity taken at each point shall be about 700g, and the samples shall be taken as test samples. 5.2 When sampling from a truck or a storage silo with 25-100t, a sampler should be used. Sampling points should be arranged at different locations from the top to the bottom. 15 samples should be taken from each batch, and about 700g of samples should be taken from each point, and they should be combined as a test sample. When sampling from a batch of trucks or storage silos with less than 25t, the total number of samples taken should not be less than 10, and the amount of samples taken from each point should be about 700g: combined as a test sample. 5.3 The collected samples are fully mixed and divided into four parts. Take a portion, each of which is about 2.5kg, and put them into clean, dry and sealed containers and label them. The label should be filled with the date, sampler, manufacturer name and batch number. One bottle is sent for inspection, one bottle is kept for re-inspection, and one bottle is kept for three months for arbitration.
5.4 Sampling and acceptance inspection work should be completed within the period specified in the contract signed by the supply and demand parties. When the product does not meet the indicators specified in Table 1, the buyer shall submit a report to the supplier within the period specified in the contract and explain the reasons for rejection. 5.5 Both the supplier and the buyer may request re-inspection within ten days after receiving the sample report. 5.6 If the supplier and the buyer cannot reach a consensus, the preserved samples shall be sent for arbitration testing. 6 Marking and packaging quality inspection form
6.1 Marking
6.11 The words "limestone powder" are printed in bold on the upper plate of the packaging bag, and the manufacturer's name and batch number shall be printed at the bottom of the bag. 6.1.2 The manufacturer's trademark and the net amount of each bag should be in the middle and below the middle of the outer bag. 6.1.3 The material name, transportation method, transportation amount, manufacturer name and factory batch number should be filled in on the bill of lava powder transported in bulk. 6.2 Packaging
6.2.1 The packaging bag of limestone powder should have sufficient strength and should have at least two layers. The outer layer is a latex-coated woven bag, or the inner layer of a polyolefin woven bag is a high-strength polyethylene film bag to meet the requirements of waterproof and not easy to break. 6.2.2 The inner and outer layers of the packaging bag should be separately tied: 6.2.3 The net weight of each bag is 25kg, and the allowable error is 5%. However, if 50 bags are randomly sampled in each batch of products, the average value should not be less than 25kg ：6.3 Quality inspection sheet
6.3.1 Each batch of products must be accompanied by a product quality inspection sheet when it is shipped to the purchaser (the format is shown in Appendix B). :5
Commissioning unit:
Sample number:
Manufacturer name:
Sample date:
Test content
Density,
0.076mm sieve residue,
SY/T5061—93
Appendix A
Test report on limestone powder for drilling fluid
(supplement)
Report number:
Sample collection date:
Sample taker,
Xiao Le Girum Content of particles
(when the inner ball diameter), %
calcium carbonate content.
water-soluble matter content,
acid-insoluble matter content,
test results
shipped to:
quantity:
ex-factory batch number:
SY/T 5061--93
Appendix B
quality inspection form for limestone powder products
(supplement)
contract number:
transportation party:
manufacturer name:
calcium carbonate
content, %
water-soluble matter
today·%
acid-insoluble
SY/T 5061—93
Viscosity of water at different temperatures
(Supplement)
mPa·?
0, 9058
Uncorrected density
Reading of density meter
Depth 1
SY/T 5061-93
Appendix D
Effective depth of density meter
(Supplement)
Uncorrected density
Reading of density meter
Use formula L—15.63-172 (Hc~1) is used as the basis for calculation. Additional remarks:
This standard is proposed and technically managed by the Petroleum Drilling Engineering Professional Standard Promotion Committee. This standard is drafted by the Drilling Institute of Beijing Petroleum Exploration and Development Research Institute and Beijing Mining and Metallurgy Research Institute. The main drafters of this standard are Zhang Yongbing, Liu Yu and Xu Jianmin. SY/T5061-93 "Limestone Powder for Drilling Fluid" No. 1 Amendment is effective
Depth L
This amendment was approved by the Technical Supervision and Safety and Environmental Protection Bureau of China National Petroleum Corporation on January 19, 1998 in the document [987 Zhongyou Jijianzi No. 32, and will be implemented from March 1, 1998. (1) Formula (7) \W[1-(\二\)]×100\ in Article 4.3.4.3 is changed to \W=”\×100 (2) The fourth line of Article 4.3.4.3 \ms-mass of evaporated blood and dry solid matter\ is changed to \mvaporized blood and dry solid matter
mass g”
SY/T5061-93 “Limestone Powder for Drilling Fluid” Amendment No. 1 This amendment is approved by China National Petroleum Corporation The Technical Supervision and Safety and Environmental Protection Bureau approved the implementation of the document [98] Zhongyou Jijianzi No. 32 on January 19, 1998, and it will be implemented from March 1, 1998. (1) Formula (7) in Article 4.3.4.3 "m-1-（-m2)×10 is changed to mx100\m
(2) The fourth line of Article 4.3.4.3 "m-mass of evaporating dish and dry solids;" is changed to "n; mass of evaporating blood and solids, g"
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