Some standard content:
GB/T5005—2001
This standard specifies the technical requirements, test methods, inspection rules, packaging and marking of barite powder, iron ore powder, drilling bentonite, untreated bentonite, OCMA bentonite, attapulgite, sepiolite, technical low-viscosity carboxymethyl fiber, technical high-viscosity carboxymethyl fiber and starch for drilling fluid.
This standard is equivalent to ISO13500:1998 "Specifications and Tests for Drilling Fluid Materials in the Petroleum and Natural Gas Industry". In the preparation of this standard, the standard format and numbering were revised as required. The four chapters of ISO13500, Chapter 2, Standard Reference Catalog (Involved International Standard Catalog), Chapter 4, Requirements (Requirements for Experimental Standard Materials), Chapter 5, Calibration (Methods for Instrument Calibration), and Chapter 6, Packaging Materials, were deleted because they are clearly stipulated in relevant laws and regulations of my country. Chapter 3 Definitions and Abbreviations is included in the standard as a suggestive appendix. Appendix A Mineral impurities in barite is retained as a suggestive appendix. Appendix B Experimental accuracy is scattered in various material chapters as standard provisions. Appendix C Calculation method examples is retained as a standard appendix. From the date of entry into force, this standard replaces GB/T5005--1994, SY/T5351--1991, SY5508--1992, SY/T 5060--1993. SY/T 5603--1993. SY/T 5093--1992. SY/T5353-1991. Appendix A, Appendix B, Appendix C, and Appendix D in this standard are all standard appendices: Appendix E and Appendix F in this standard are all suggestive appendices. This standard is proposed by China National Petroleum Corporation. This standard is under the jurisdiction of the Petroleum Drilling Engineering Professional Standardization Committee. This standard was drafted by Chengde Petroleum College. The drafting unit of this standard is: Drilling Institute of Petroleum Exploration and Development Research Institute. The main drafters of this standard are: Zhang Guozhao, Pan Xiaoyong, Huang Bugeng, Wang Kuicai, Yang Jing, Tan Bosheng, He Yaochun, Shao Xiaomo, Zheng Ruozhi. 498
GB/T5005--2001
ISOForeword
This international standard covers commonly used materials for oil and gas drilling fluids. These materials are used in large quantities and can be purchased from existing commodities through various channels. This international standard does not include products from a single or limited source, nor does it include special products. The purpose of publishing international standards is to facilitate communication between users and manufacturers, to provide reliable interchangeability for similar instruments and materials purchased from different manufacturers and/or at different times, and to provide adequate safety standards for instruments and materials when they are used in a certain way to achieve their intended purpose. This international standard gives minimum requirements, but does not intend to prevent anyone from purchasing and producing materials that meet other specifications. This international standard is essentially based on API Spec 13A, 15th edition, May 1, 1993. The purpose of this international standard is to provide product specifications for barite, hematite, drilling bentonite, untreated bentonite, Oil Company Materials Association (OCMA) grade bentonite, attapulgite, sepiolite, technical low viscosity carboxymethyl cellulose, technical high viscosity carboxymethyl cellulose and starch. The intention of this document is to merge the international standards for various drilling fluid materials into one ISO version document. Industry investigation found that only AP1 published the experimental procedures and specification standards for these materials. Since OCMA and the subsequent executive committee were declared invalid, the relevant OCMA materials have been included in the API volume, and all OCMA specifications were submitted to API in 1983. 499
1 Scope
National Standard of the People's Republic of China
Drilling fluid materials specifications
Drilling fluid materials specificationsGB/T50052001
eqv Is0 13500:1998
Replaces GB/T 50051994
This standard specifies the technical requirements, test procedures, inspection rules, packaging and marking of barite powder, iron ore powder, drilling bentonite, untreated bentonite, OCMA bentonite, attapulgite, sepiolite, technical grade low viscosity carboxymethyl cellulose, technical grade high viscosity carboxymethyl cellulose and starch. This standard applies to materials such as barite powder, iron ore powder, drilling bentonite, untreated bentonite, OCMA bentonite, attapulgite, sepiolite, technical grade low viscosity carboxymethyl cellulose, technical grade high viscosity carboxymethyl cellulose and starch for oil and gas well drilling fluids. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601-1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T603--1988 Preparation of preparations and products used in test methods for chemical reagents GB/T6682-1997 Specifications and test methods for water for analytical laboratories GB8170 Rules for rounding off values
GB/T6003.1-1997 Metal wire mesh test sieve GB/T16783-1997 Field test procedures for water-based drilling fluids 3 Barite powder
3.1 Overview
3.1.1 Barite powder is produced from commercial ores containing barium sulfate. The manufacturer should keep certificates of analysis and similar documents of commercial barite powder. It can be a single ore or a mixed ore; it can be a product directly mined or a product obtained by various efficiency enhancement methods such as washing, shaking, elimination or flotation. In addition to barium sulfate, there are other incidental minerals. Due to the presence of these minerals, the color of commercial barite powder varies, from grayish white to gray, red or brown. Common incidental minerals include silicates such as quartz and stone, siderite and dolomite, as well as metal oxides and sulfides. Although these minerals are usually insoluble, under certain circumstances, they can react with other components in certain drilling fluids and have an adverse effect on the performance of the drilling fluid. 3.1.2 The barite powder provided in accordance with this standard shall meet the technical indicators specified in Table 1. Table 1 Technical indicators of barite powder
Density/(g/cm3)
Water-soluble alkaline earth metal (calculated as calcium)/(mg/kg)Mass fraction of 75μm sieve residue/%(m/m)Particles smaller than 6μm/%(m/m)
Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on December 30, 2001500
Implemented on August 1, 2002
3.2 Instruments or equipment
3.2.1 Oven: can be controlled at 105C±3C. 3.2.2 Dryer: equipped with desiccant.
GB/T 5005--2001
3.2.3 Lea density bottle: clamped or pressed to prevent floating in the water tank. Transparent thermostatic bath: temperature control range ±0.1°C (40dm water bath with heating and circulation auxiliary equipment or functional equivalent). 3.2.4
Balance: accuracy 0.01g.
Pipette: 10cm.
Magnifying glass.
Wooden stick: about 8mm diameter, 30cm length, or functional equivalent. Flat weighing bottle, 950mm×30mm.
Hard fine brush.
Conical flask with stopper: 250cm.
Graduating cylinder: 100cm2, scale 1cm.
Conical flask: 100cm2 to 150cm2.
Serological pipette or burette: scale 0.1 cm*Pipette: 10cm2.
Filter loss meter or filter funnel.
Oscillator: optional.
Volume flask: 1000cm*.
Stirring rod.
Stirrer: load speed is 11000r/min±300r/min, the shaft should be equipped with a single sine wave blade, the blade diameter is about 25mm, and its concave side faces upward.
Stirring cup: depth 180mm, upper inner diameter 97mm, lower inner diameter 70mm. 3.2.21
75μm sieve: diameter 76mm, height 69mm from upper frame to sieve cloth. Nozzle: nozzle body (or equivalent product) connected to a water pipe with a 90-degree elbow. Water pressure regulator, can be adjusted to 69kPa±7kPa. Evaporation of blood. bZxz.net
Glass sedimentation measuring cylinder: height about 457mm, diameter 63mm, scale volume is 1000cm2. Rubber stopper: No. 13.
Thermometer: Measurable temperature range 16C±0.5℃～32C±0.5℃. Density meter: With scale for reading suspension density. Timer: Mechanical or electronic type, minimum scale 1s. Mud density scale; 2.0g/cm2～~3.0g/cm2. 3.3 Reagents or materials
3.3.1 Anhydrous kerosene: add 200g anhydrous calcium chloride to 5kg commercial kerosene, shake for 5min and place for 24h, take the upper clear liquid (if turbid, filter it).
3.3.2 EDTA aqueous solution: 3.12g±0.01g disodium salt of ethylenediaminetetraacetic acid dihydrate, dilute to 1000cm2 with deionized water in a volumetric flask, calibrate before use.
3.3.3 Buffer solution: 63.5g±0.01g ammonium chloride and 510cm±1cm, 15mol/dm2 ammonium hydroxide solution, dilute to 1000cm2 with deionized water in a volumetric flask.
3.3.4 Chrome black T indicator: weigh 0.5g Chrome black T, add 20cm triethanolamine, dilute to 100cm2 with water. 3.3.5 Sodium hexametaphosphate: chemically pure.
3.3.6 Dispersant solution: 40 g ± 0.1 g sodium hexametaphosphate (chemically pure) and 3.6 g ± 0.1 g anhydrous sodium carbonate (chemically pure) per 1000 cm2. Use sodium carbonate to adjust the pH of the solution to about 9.0. 3.3.7 Deionized water or distilled water.
3.3.8 Calcium sulfate: chemically pure.
3.3.9 Tissue paper: absorbent.
Note: Laboratory grade tissue paper does not contain absorbent and is therefore not suitable for this test procedure. 3.3.10 Filter paper: Whatman 50 type, or equivalent. 3.4 Density Test Procedure
3.4.1 Add anhydrous kerosene to a dry Lethe flask to about 2 cm below the zero mark. Roll a piece of tissue paper diagonally on a wooden stick and use it to wipe the inner surface of the neck of the Lester bottle dry. The wooden stick and tissue paper must not come into contact with the kerosene in the bottle. 3.4.2 Place the Lester bottle upright in a thermostatic bath. The water level in the bath should be above the 24 cm° mark on the neck of the bottle, but below the stopper. Use a clamp or weight to ensure that the Lester bottle is stable.
3.4.3 Allow the Lester bottle and its contents to equilibrate for at least 1 hour. Use a magnifying glass to carefully observe the position of the meniscus and read the initial volume to the nearest 0.05 cm, but do not remove the Lester bottle from the thermostatic bath to read the volume. Note: If the kerosene level is not within the range of -0.2 cm to +1.2 cm2 after thermostatic bathing, use a pipette to add or remove some kerosene so that the level falls within this range. Allow the bottle to equilibrate for at least 1 hour and record the initial volume. 3.4.4 Remove the Lester bottle from the thermostatic bath, wipe dry and remove the stopper. 3.4.5 Weigh 80g ± 0.05g of barite powder dried at 105℃ ± 3℃ for 2h in a dry 100mL beaker and carefully add it to the Lein flask through a dry and clean short-necked funnel. Be careful to avoid kerosene splashing or barite powder blocking the spherical part of the bottle diameter. This process is time-consuming. The barite powder needs to be added little by little and then the bottle stopper is closed. 3.4.6 If necessary, tap the neck of the bottle or shake it carefully to brush off the barite powder adhering to the bottle wall. Do not let the kerosene contact the contact surface between the ground glass stopper and the bottle.
3.4.7 Slowly roll the bottle along a smooth surface with an inclination of no more than 15°, or place the upright bottle between the palms and rotate it quickly to remove the air entrained in the barite powder sample. Repeat the above steps until no more bubbles are seen in the barite powder. 3.4.8 Return the Lein flask to the thermostatic bath and keep the temperature constant for at least 30 minutes. 3.4.9 Remove the Lein flask from the thermostatic bath and repeat the experimental steps in 3.4.7 to remove all residual air in the barite powder. 3.4.10 Return the Lein flask to the thermostatic bath and keep it at this temperature for at least 1 hour. 3.4.11 Read the final volume as described in 3.4.3. 3.4.12 Density calculation method:
Calculate the density of barite powder according to formula (1): m
Vr V.
Where: α - —density of barite powder, g/cm; m· -mass of added barite powder, g;
V, final volume of the Lein flask, cm\;
- initial volume of the Lein flask, cm.
3.5 Test procedure for water-soluble alkaline earth metals (calcium). (1)
3.5.1 Weigh 100 g ± 0.05 g dried barite powder in a stoppered conical flask and add 100 cm ± 1 cm2 deionized water. Cover the stopper and shake 4 to 6 times within 1 hour, shaking continuously for 5 minutes each time, or shake with an oscillator for 20 minutes to 30 minutes. 3.5.2 After shaking, filter the suspension using a low-pressure filter loss meter (or filter funnel) with two layers of filter paper and collect the filtrate in a glass container. 3.5.3 Add 50 cm ± 1 cm2 deionized water to a 150 cm2 (or 100 cm2) conical flask. Add about 2 cm2 of buffer and 3 to 5 drops of chrome black T indicator to achieve a distinct blue color. Shake to mix. If the solution has a color other than distinct blue at this time, it indicates that the equipment and water are contaminated. Find and eliminate the source of contamination and repeat the experiment.
GB/T 5005-2001
3.5.4 Use a pipette to transfer 10 cm of the filtrate into a conical flask and shake it. If the solution is blue, it indicates that the calcium and magnesium are zero and the experiment is over. If calcium and magnesium are present, a wine red color will appear.
3.5.5 If calcium and magnesium are present, begin shaking the conical flask and titrate with EDTA solution to a blue endpoint. The endpoint of the titration is preferably when the addition of further EDTA no longer produces a color change from red to blue. The volume of EDTA used to produce the blue endpoint will be used for the calculation in Section 3.5.6. If the endpoint is unclear or cannot be reached, other experiments must be performed and the methods used and the results obtained must be recorded. 3.5.6 Calculation method of water-soluble alkaline earth metal (calculated as calcium): Calculate the water-soluble alkaline earth metal (calculated as calcium) content according to formula (2): Ca = 100 X ceV × 40.08
Wherein: Ca-water-soluble alkaline earth metal (calculated as calcium) content, mg/kgCs-concentration of EDTA standard solution, mol/dm; V-volume of consumed EDTA standard solution, cm\; 40.08-mass of calcium ion per mole, g/mol3.675μm sieve residue test procedure
3.6.1 Weigh 50g ± 0.01g of dried barite powder and add it to 350cm2 of deionized water containing approximately 0.2g of sodium hexametaphosphate and stir on a stirrer for 5min ± 1min. 3.6.2 Transfer the sample to the 75um sieve, transfer all the material in the container to the sieve with a wash bottle, and rinse the material on the sieve with a water flow of 69kPa±7kPa from the nozzle for 2min±15s. When rinsing, place the nozzle on an approximate plane on the top of the sieve, and move the water flow repeatedly over the sample. 3.6.3 Rinse the sieve residue from the sieve into the evaporation III that has been dried and cooled at 105°C±3°C and weighed, and slowly pour out the excess water.
3.6.4 Dry the evaporating dish and sieve residue in an oven at 105°C±3°C for 2h, take it out and cool it in a desiccator for 30min, and weigh the mass of the evaporation IIIl and the sieve residue.
3.6.5 Calculation method of 75 μm sieve residue:
Calculate the 75 μm sieve residue according to formula (3):
Ss=m=m×100
Where: Ss——mass fraction of 75 μm sieve residue, %; ml——mass of evaporating dish and 75 μm sieve residue, g; mo——mass of evaporating blood, g;
——weight of barite powder, g.
3.7 Test procedure for particles with equivalent spherical diameter less than 6 μm·(3)
3.7.1 Weigh 80 g ± 0.1 g of barite powder dried at 105℃±3℃ for 24 hours into a mixing cup. 3.7.2 Add 125 cm2 ± 2 cm2 (127 g ± 2 g) of dispersion solution into the mixing cup and dilute to about 400 cm2 with deionized water. Rinse all particles adhering to the scraper into the suspension. 3.7.3 Stir on the stirrer for 5min±30s. 3.7.4 Transfer the suspension to a sedimentation measuring cylinder. Rinse the mixing cup with deionized water to ensure that all sample particles are transferred to the sedimentation measuring cylinder. 3.7.5 Add deionized water to the 1000cm2 mark. Hold the No. 13 rubber stopper on the top of the measuring cylinder tightly and constantly turn the cylinder upside down for 60s±6s to fully mix the sample.
This is a critical step. The suspension must be homogenous at the beginning of sedimentation. This is difficult to achieve due to the high density of barite powder. 3.7.6 Place the measuring cylinder on the counter of the constant temperature room (or in a constant temperature bath) and start the timer at the same time. Hang a thermometer in the suspension. 3.7.7 Read the density count value at intervals of 10min±6s, 20min±6s, 30min±6s and 40min±6s (or until the first experimental point under 6um). To read the density reading, carefully and slowly lower the densitometer to approximately 1.020 scale line. When the densitometer is stable, read the top of the meniscus at the specified time. Carefully and slowly remove the densitometer, rinse the densitometer with deionized water after each reading and wipe it dry. The densitometer must be removed immediately after each reading to eliminate the deposition of particles on the shoulders of the densitometer, as this will cause erroneous results. All density readings must be read with minimal disturbance to the fluid to protect the sedimentation equilibrium of the suspension. 3.7.8 Record the time (t), min; temperature (T), C; and densitometer reading (H) on the data card. 3.7.9 For each time interval, determine the water viscosity (n) and the effective depth of the densitometer (L) from Tables 2 and 3 and record them on the data card. 3.7.10 Calculation method for the experiment of particles with equivalent spherical diameter less than 6um: 3.7.10.1 Calculation of density meter correction slope (Mc) and density meter correction intercept (Bc): Calculate the density meter correction slope (Mc) and density meter correction intercept (Bc) according to formula (4) and (5). Where: Mc - the slope of the correction curve;
Mc = 1 000 -
(R R2)
the average reading of the density meter at a lower temperature; R - the average reading of the density meter at a higher temperature; T
where: Bc - the average reading of the thermometer at a lower temperature; the average reading of the thermometer at a higher temperature. Bc = (Mc × T) + [(R, — 1) × 1 000] the intercept of the correction curve;
the average reading of the thermometer at a lower temperature; the average reading of the density meter at a lower temperature. 3.7.10.2 Calculation of sample constant (Ks): Calculate the sample constant (Ks) according to formula (6) and record it on the data card. Ks-
Where: Ks
sample constant;
sample density, g/cm2;
sample mass, g.
3.7.10.3 Calculation of equivalent spherical diameter (de): 100×g
m(oi)
Calculate the equivalent spherical diameter (de) according to formula (7) and record it on the data card. de = 17.5 1
Where: de——equivalent spherical diameter, um; viscosity of water, mPa·s;
L——depth, cm.
asample density g/cm2;
time, min.
. (6)
3.7.10.4 Calculate the cumulative percentage of fine particles (SH) at the test point with an equivalent particle diameter (de) slightly larger than 6μm and the cumulative white fraction of fine particles (SL) at the test point with an equivalent particle diameter (de) slightly smaller than 6μm according to formula (8), and record them on the data card. S = Ks[(Mc ·T) - Bc + (H - 1)1 000] Where: S -
Cumulative percentage of fine particles smaller than a certain size; - sample constant;
Mc - densitometer correction slope;
T - suspension temperature, C
densitometer correction intercept;
H - densitometer reading.
......(8)
GB/T 5005—2001
3.7.10.5 Calculate the cumulative percentage of particles smaller than 6 μm (S.) according to formula (9) and record it on the data card. S
SH- SL
L(aH=a)(6 - dt)]+ sz
Wherein: S is the cumulative percentage of particles smaller than 6 μm; SH-—the cumulative percentage of fine particles at the experimental point slightly larger than 6 μm; SL———the cumulative percentage of fine particles at the experimental point slightly smaller than 6 μm; dH—-the equivalent diameter of fine particles at the experimental point slightly larger than 6 μm; dL—the equivalent diameter of fine particles at the experimental point slightly smaller than 6 μm. 3.7.10.6 Calculate the viscosity at the experimental temperature according to formula (10): 1g(n20/n-) = [1.37023(T
— 20) →+ 0.000836(T — 20)27/(109 + T)] where: 720 = 1.002;
viscosity at the experimental temperature;
T—Celsius temperature, C.
Table 2 Viscosity of water at different temperatures
Temperature/C
Uncorrected density
Count value
Viscosity/(mPa·s)
Temperature/c
Viscosity/(mPa·s）
Temperature/C
Table 3 Effective depth corresponding to the density count value of the specified depth measuring cylinder Effective depth 1./cm
Uncorrected density
Count value
Effective depth 1./cm
Uncorrected density
Count value
.........( 10 )
Viscosity/(mPa·s）
Effective depth L/cm
Sample density/（g/cm\）
3.8 Accuracy requirements
GB/T 5005
5—2001
Table 480.0g sample mass sample constant (Ks) Sample constant, Ks
Sample density/(g/cm2)
Sample constant, Ks
When the average measured values are within the allowable difference range of Table 5, take the arithmetic mean. Table 5 Experimental precision of barite powder
Density/(g/cm2)
Water-soluble alkaline earth metals (calculated as calcium)/(mg/kg)75μm sieve residue/%
Particles less than 6μm/%
3.9 Experimental report
Experimental report form, the format of which is shown in Appendix A.
3.10 Inspection rules
Repeatability
Sample density/(g/cm3)
Sample constant, Ks
Reproducibility
3.10.1 Sampling of bagged barite powder should be based on the stacking height, shape and quantity (maximum quantity is one car), and sampling points should be arranged at the top, middle and bottom of each side. Each batch should not be less than 15. Take about 700g of sample at each sampling point and combine them as the sample of the batch of barite powder.
3.10.2 Sampling method Use a sampler or take samples from the middle of each bag. 3.10.3 When taking samples of bulk barite powder from a truck or a storage silo with 25t to 100t, a sampler should be used, and sampling points should be arranged at different locations from the top to the bottom. 15 sampling points should be taken from each batch, each sampling point is about 700g, and they are combined as samples; when sampling from a batch of trucks or storage silos with less than 25t, the total number of sampling points should not be less than 10, and each sampling point is about 1000g, and they are combined as samples. 3.10.4 After the collected samples are fully mixed, they are divided into two parts by quartering method, and they are respectively placed in clean and dry wide-mouth bottles, covered with bottle caps, and labeled. The sampling date, sampler, manufacturer name and factory batch number should be filled on the label. One bottle is sent for testing, and the other bottle is kept for three months for arbitration.
3.10.5 Sampling and acceptance work shall be completed within the period specified in the contract signed by the supply and demand parties. When a product has a technical indicator that does not meet the requirements of Table 1, it shall be retested. If the retest result still does not meet the technical indicators specified in Table 1, the product shall be considered unqualified. 3.10.6 If there is a quality dispute between the supply and demand parties and arbitration is required, it shall be arbitrated in accordance with the provisions of the National Bureau of Standards [19857035 "National Product Quality Arbitration Inspection Interim Measures" and the arbitration analysis shall be carried out according to the inspection methods specified in this standard. 3.11 Packaging, marking and quality inspection form
3.11.1 Packaging
3.11.1.1 The packaging bag of barite powder shall have sufficient strength and at least two layers. The outer layer is a rubber-coated woven bag or a polypropylene woven bag, and the inner layer is a high-strength polyethylene film bag to meet the requirements of waterproof and not easy to break. 3.11.1.2 The inner and outer seals of the packaging bag shall be tied separately. 3.11.1.3 The net weight of each bag is 25kg, and the tolerance is ±5%. However, if 40 bags are randomly sampled in each batch of products, the average value shall not be less than 25kg. 506
3.11.2 Marking
GB/T 5005-- 2001
3.11.2.1 The words "barite powder" shall be printed in bold and eye-catching font on the top of the outer layer of the packaging bag, and the manufacturer's name, factory batch number, standard code, etc. shall be printed on the bottom of the bag.
3.11.2.2 The manufacturer's trademark and the net weight of each bag shall be printed in the middle and lower middle part of the outer bag. 3.11.2.3 The barite powder transported in bulk shall be marked with the material name, transportation method, carrying capacity, manufacturer's name and factory batch number on the waybill.
3.11.3 Quality Inspection Sheet
3.11.3.1 Each batch of products shall be accompanied by a quality inspection sheet for the product. The format is shown in Appendix B. 3.11.3.2 If there is no product quality inspection sheet from the manufacturer when each batch of products is delivered to the purchaser, the purchaser may refuse to accept or pay for the goods and pursue economic liability according to the contract.
4 Iron ore powder
4.1 Overview
Iron ore powder is produced from commercial ore, or it can be a single ore or a mixed ore. Iron ore powder ore can be a product directly mined or a processed product. It will also contain a small amount of other accessory minerals besides iron oxide (Fe20)3), such as silicon oxide, aluminum oxide and magnesium oxide.
4.1.2 Iron ore powder provided in accordance with this standard shall meet the technical indicators specified in Table 6. Table 6 Technical Specifications of Iron Ore Powder
Density/(g/cm2)
Water-soluble alkaline earth metals (calculated as calcium)/(mg/kg) 75μm sieve residue/%(m/m)
45 μm sieve residue/%(m/m)
Particles smaller than 6μm/%(m/m)
4.2 Instruments or Equipment
4.2.1 Oven: controlled at 105℃±3℃. 4.2.2 Dryer: filled with desiccant.
See Appendix D
4.2.3 Lea density bottle: clamped or pressed to prevent floating in the water tank. 4.2.4
Transparent constant temperature bath: 32℃ controlled at ±0.1℃ (40dm water tank with heating and circulation auxiliary equipment or functional equivalent). Balance: accuracy of 0.01g.
Pipette: 10 cm.
Magnifying glass.
Wooden stick: about 8 mm in diameter, 30 cm in length, or functional equivalent. Flat weighing bottle: 50 mm × $30 mm.
Conical flask with stopper: 250 cm2.
Graduating cylinder: 100 cm2 with 1 cm2 graduation.
Conical flask: 100 cm2 to 150 cm.
Serological pipette or burette: with 0.1 cm2 graduation. Pipette: 10 cm2.
Filter loss meter or filter funnel.
4.2.16Oscillator: optional.
4.2.17Volume flask: 1000 cm2,
4.2.18Stirring rod.
GB/T 5005—2001
4.2.19 Agitator: Load speed is 11000r/min+300r/min, the shaft should be equipped with a single sinusoidal blade, the blade diameter is about 25mm, and its concave side faces upward.
4.2.20 Mixing cup: 180mm deep, upper inner diameter 97mm, lower inner diameter 70)mm. 4.2.2175jm sieve: 76mm in diameter, 69mm in height from upper frame to sieve cloth. 4.2.22
45um sieve: 76mm in diameter, 69mm in height from upper frame to sieve cloth. 4.2.23
Nozzle: Nozzle body connected to a water pipe with a 90-degree elbow or equivalent product. 4.2.24 Water pressure regulator: can be adjusted to 69kPa±7kPa. 4.2.25
Evaporated blood.
Glass sedimentation measuring cylinder: 457mm high, 63mm in diameter, graduated volume 1000cm3. Rubber stopper: No. 13.
Thermometer: Measuring range 16°C±0.5°C～32°C±0.5°C. 4.2.29
Densitometer: With a scale for reading the density of the suspension. 4.2.30Timer: Mechanical or electronic type, with an accuracy of 1$. 4.2.31 Mud density scale: 2.0g/cm3~3.0g/cm3. 4.3 Reagents or materials
4.3.1 Anhydrous kerosene: 5kg of commercially available kerosene, add 200g of anhydrous calcium chloride, shake for 5min, and let stand for 24h, then take the upper clear liquid (if turbid, filter it).
4.3.2 EDTA aqueous solution: 3.72g ± 0.01g ethylenediaminetetraacetic acid disodium salt dihydrate, dilute to 1000cm2 with deionized water in a volumetric flask, calibrate before use.
4.3.3 Buffer solution: 67.5g ± 0.1g ammonium chloride and 570cm2 ± 1cm2 15mol/dm2 ammonium hydroxide solution, dilute to 1000cm2 with deionized water in a volumetric flask.
4.3.4 Chrome black T indicator: weigh 0.5g Chrome black T. Add 20cm2 triethanolamine, dilute to 100cm2 with water. 4.3.5 Deionized water or distilled water.
4.3.6 Sodium hexametaphosphate: chemically pure.
4.3.7 Dispersant solution: 10 g ± 0.1 g sodium hexametaphosphate (chemically pure) and 3.6 g ± 0.1 g anhydrous sodium carbonate (chemically pure) per 1000 cm3 of solution. Use sodium carbonate to adjust the pH of the solution to about 9.0. 4.3.8 Tissue paper: absorbent.
Note: Laboratory grade tissue paper does not contain absorbent and is therefore not suitable for this test procedure. 4.3.9 Filter paper: Whatman type 50, or equivalent. 4.4 Density Test Procedure
4.4.1 Add anhydrous kerosene to a dry Leather flask to a point about 2 cm below the zero mark. Roll the tissue paper diagonally on a wooden stick and use it to wipe the inner surface of the neck of the Leather flask dry. The wooden stick and tissue paper must not come into contact with the kerosene in the flask. 4.4.2 Place the Leather flask upright in a constant temperature bath. The water level in the tank should be above the 24 cm mark on the neck of the bottle, but below the stopper. Use a clamp or weight to ensure that the Leinstein flask is stable.
4.4.3 Allow the Leinstein flask and its contents to equilibrate for at least 1 hour. Use a magnifying glass to carefully observe the position of the meniscus and read the initial volume to the nearest 0.05 cm2, but do not remove the Leinstein flask from the thermostat to read the volume. Note: If the kerosene level is not within the range of -0.2 cm to -1.2 cm after thermostating, use a pipette to add or remove some kerosene so that the level falls within this range. Allow the bottle to equilibrate for at least 1 hour and record the initial volume. 4.4.4 Remove the Leinstein flask from the thermostat, wipe it dry and remove the stopper. 4.4.5 Weigh 100g ± 0.01g of iron ore powder that has been dried at 105°C ± 3°C for 2h in a dry 100ml beaker and carefully add it to the Lethe flask through a dry and clean short-necked funnel. Be careful to avoid kerosene splashing or iron ore powder blocking the spherical part of the bottleneck. This process is time-consuming and the iron ore powder needs to be added little by little. Then cover the bottle with a stopper. 4.4.6 If necessary, tap the neck of the bottle or shake it carefully to remove the iron ore powder stuck to the bottle wall. Do not let the kerosene contact the contact surface between the ground glass stopper and the bottle.
4.4.7 Slowly roll the bottle along a smooth surface with an inclination of no more than 45°, or place the upright bottle between the palms and rotate it quickly to remove the air entrained in the iron ore powder sample. Repeat the above steps until no more bubbles are seen in the iron ore powder. 4.4.8 Return the Lein flask to the thermostatic bath and keep the temperature constant for at least 30 minutes. 4.4.9 Remove the Lein flask from the thermostatic bath and repeat the experimental steps in 4.4.7 to remove all residual air in the iron ore powder. 4.4.10 Return the Quartz flask to the thermostatic bath again and keep the temperature constant for at least 1 hour. 4.4.11 Record the final volume in the same way as described in 4.4.3. 4.4.12 Density calculation method:
Calculate the density of the iron ore powder according to formula (11): p = vV.
Where: p - density, g/cm\;
m sample mass, g;
V,\ - final volume, cm\
V. — - initial volume, cm.
4.5 Test Procedure for Water-Soluble Alkaline Earth Metals (Calcium) (11)
4.5.1 Weigh 100 g ± 0.05 g of iron ore powder dried at 105°C ± 3°C for 2 h in a stoppered conical flask and add 100 cm ± 1 cm of deionized water. Cover the stopper and shake (4~~6) times within 1 h, shaking continuously for 5 min each time, or shake with an oscillator for 20 min~30 min.
4.5.2 After shaking, filter the suspension using a low-pressure filter loss meter (or filter funnel) with two layers of filter paper and collect the filtrate in a glass container. 4.5.3 Add 50 cm2 ± 1 cm2 of deionized water to a 150 cm2 conical flask. Add about 2 cm of buffer and (3~~5) drops of chrome black T indicator to achieve a distinct blue color. Shake to mix. If the solution has a color other than blue, it indicates that the equipment or water is contaminated. Find and eliminate the source of contamination and repeat the test.
4.5.4 Use a pipette to transfer 10 cm2 of the filtrate to a conical flask and shake well. If the solution is blue, it indicates that the calcium and magnesium are zero and the experiment is over. If calcium and magnesium are present, a wine red color will appear.
4.5.5 If calcium and magnesium are present, start shaking the conical flask and titrate with EDTA solution to a blue endpoint. The endpoint of the titration is preferably when the addition of EDTA no longer produces a color change from red to blue. The volume of EDTA used to produce the blue endpoint will be used in 4.5.6.
If the endpoint is unclear or cannot be reached, other experiments must be performed and the methods used and the results obtained must be recorded. 4.5.6 Calculation method for water-soluble alkaline earth metal (calculated as calcium): Calculate the content of soluble alkaline earth metal (calculated as calcium) according to formula (12): Ca = csV X 100 X 40. 08
Where: Ca-water-soluble alkaline earth metal (calculated as calcium) content, mg/kg; C--concentration of EDTA standard solution, mol/dm; V-volume of consumed EDTA standard solution, cm\; 40.08-mass of calcium ion per mole?g/mol. 4.675 μm and 45 μm sieve residue test procedure (12)
4.6.1 Weigh 50 g ± 0.01 g of dried iron ore powder and add it to 350 cm2 of water containing approximately 0.2 g of sodium hexametaphosphate and stir on a stirrer for 5 min ± 1 min.
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