Some standard content:
ICS71.100.99
Registration No. 136—1997
Chemical Industry Standard of the People's Republic of China
Granulated clay
Granulated clay
Published on February 4, 1997
Ministry of Chemical Industry of the People's Republic of China
Implemented on October 1, 1997
HG/T2825—1997
This standard is formulated with reference to the product specifications of well-known foreign companies, in accordance with the standards of various enterprises, and taking into account the requirements of domestic manufacturers and users.
This standard divides granulated clay into two types. In the index items, according to the requirements of manufacturers and users, both types have added three items of deolefination initial activity, particle pressure resistance and decolorization rate compared with foreign products. Among the index parameters, the various index parameters of type I and type I products are the same as or close to those of foreign product specifications, reaching the domestic advanced level. This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. The drafting units of this standard are: Liaoning Yixian Petroleum Clay Factory, Shanghai Petrochemical Co., Ltd. Catalysis Research Institute, Zhejiang Lin'an Bentonite Chemical Factory, Hubei Ezhou No. 2 Chemical Factory, Hangzhou Lin'an Catalyst Factory, and Tianjin Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are: Jiang Junhua, Wang Chunlin, He Xiaoyi, Wang Pinghua, Zhu Jibo, Fu Xinfa, and Fan Guoqiang. This standard is entrusted to the technical unit responsible for the standardization of inorganic salt products of the Ministry of Chemical Industry for interpretation. 1 Scope
Chemical Industry Standards of the People's Republic of China
Granulated Clay
Granulated Clay
HG/T2825—1997
This standard specifies the model, requirements, sampling, test methods, marking, packaging, transportation and storage of granulated clay. This standard applies to granulated clay made from bentonite by chemical treatment. This product is mainly used for the removal of olefins and carbonyl compounds in petrochemical plants, and is also suitable for the decolorization and refining of various fuel oils such as aviation kerosene and diesel. 2 Cited 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, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB191—90 Pictorial markings for packaging, storage and transportation
GB/T601—88 Chemical reagents
Preparation of standard solutions for titration analysis (volumetric analysis) GB/T602—88
GB/T 603—88bzxZ.net
Preparation of standard solutions for determination of impurities (neqISO6353/1:1982)Chemical reagents
Preparation of preparations and products used in test methods (neqISO6353/111982)Chemical reagents
9Expression and determination methods of limit valuesGB/T1250—89
GB/T2922—82
Chemical reagentsSpecific surface area of chromatographic carriers Determination method of volume GB/T3051—82
General method for determination of chloride content in inorganic chemical products Mercury titration method GB/T6003—85
Test sieve
GB/T6288—86
Method for determination of particle size of granular molecular sieves
GB/T6678—86
6 General rules for sampling of chemical products
GB/T6682—92
GB/T 8946—88
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987)Plastic woven bags
GB/T 9725—88
3General rules for potentiometric titration of chemical reagents
HG/T2569—94Activated clay
3Product models
Based on the specific surface area of granular clay, the products are divided into two models: Type I and Type I. 4 Requirements
4.1 Appearance: Granular clay is amorphous white or slightly colored solid particles. 4.2 Granular clay should meet the requirements of Table 1.
Approved by the Ministry of Chemical Industry of the People's Republic of China on February 4, 1997, and implemented on October 1, 1997
Specific surface area, m2/g
Free acid (in HSO.), %
Amount of particles greater than the upper limit, %
Amount of particles less than the lower limit, %
Water content, %
Bulk density, g/mL
HG/T2825—1997
Initial activity of deolefination (in terms of bromine index), mg Br/100g oil Particle pressure resistance, N
Decolorization rate, %
Note: The upper and lower limits of particle size are determined according to user requirements. 5 Sampling
5.1 Each batch of products shall not exceed 50t.
5.2 Determine the number of sampling units in accordance with the provisions of 6.6 of GB/T6678-86. Each plastic woven bag is a packaging unit. When sampling, insert the sampler obliquely from the top of the packaging bag to 3/4 of the depth of the material layer to take samples. Take out no less than 50g of sample from each selected packaging unit, mix the sample thoroughly, reduce it to about 500g by quartering, and immediately put it into two clean, dry wide-mouth bottles and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, model, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample and the other bottle is kept for three months for reference. 5.3 Test results If one indicator does not meet the requirements of this standard, re-sample from the packaging of twice the number of sampling units should be verified. If the verification results do not meet the requirements of this standard even if only one indicator does not meet the requirements of this standard, the entire batch of products is unqualified. 6 Test methods
6.1 All eight index items specified in this standard are type test items, of which specific surface area, free acid, particle size, moisture, bulk density, particle pressure resistance and decolorization rate are routine test items and should be tested batch by batch. Under normal production conditions, type tests are conducted every three months.
6.2 The rounded value comparison method specified in GB/T1250 is used to determine whether the test results meet the standard. 6.3 The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682-92.
The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
6.4 Determination of specific surface area
Perform in accordance with the provisions of GB/T2922.
6.5 Determination of free acid
6.5.1 Method summary
HG/T2825—1997
Extract the free acid in the sample with water, and titrate with sodium hydroxide standard titration solution using phenolphthalein as indicator. 6.5.2 Reagents and materials
6.5.2.1 Standard sodium hydroxide titration solution: c (NaOH) is about 0.1 mol/L; 6.5.2.2 Standard sodium hydroxide titration solution: c (NaOH) is about 0.02 mol/L; Take 50 mL of sodium hydroxide standard titration solution (6.5.2.1) with known accurate concentration, place it in a 250 mL volumetric flask, dilute to the scale with carbon dioxide-free water, and shake well. 6.5.2.3 Phenol indicator solution: 10 g/L.
6.5.3 Analysis steps
Weigh 1~2g of granular clay sample (accurate to 0.0002g) crushed to a particle size of less than 75μm, place in a 150mL beaker, add 50mL of water, boil for 3min (add water continuously during heating to prevent evaporation), filter into a 250mL conical flask, wash with hot water 4~5 times (about 50mL of water in total); boil for 2min, cover with a rubber stopper, cool to room temperature; add 2~3 drops of phenolphthalein indicator solution, and titrate with sodium hydroxide standard titration solution (6.5.2.2) until it turns slightly red and remains unfaded for 30s as the end point. At the same time, take 50mL of water and perform a blank test according to the same steps. 6.5.4 Expression of analysis results
The free acid content (in terms of H2SO4) expressed as a mass percentage X is calculated according to formula (1): X1 --V): × 0.049 × 100
4.9X (Vi-Vo)·c
Wherein: V1—the volume of sodium hydroxide standard titration solution consumed by the titration test solution, mL; Vo
—the volume of sodium hydroxide standard titration solution consumed by the blank test, mL; c—the actual concentration of the sodium hydroxide standard titration solution, mol/L; m-
—the mass of the sample, g;
0.049—the mass of sulfuric acid in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c (NaOH) = 1.000mol/L).
6.5.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.04%. 6.6 Determination of particle size
6.6.1 Instruments and equipment
6.6.1.1 Oscillator (frequency 243 times/min. Load 6kg); 6.6.1.2 Test sieve: in accordance with the R40/3 series requirements in GB/T6003-85. 6.6.2 Analysis steps
Install the two test sieves with the required particle size range from bottom to top, weigh about 100g of sample (accurate to 0.1g), place it on the top test sieve, cover it, and place it on the oscillator for 5 minutes, remove the test sieve, and weigh the mass of the granular clay in the coarse-pore test sieve and the mass of the granular clay passing through the fine-pore test sieve. 6.6.3 Expression of analysis results
The amount of particles X2 greater than the upper limit expressed as a mass percentage is calculated according to formula (2): mx100
(2)
HG/T2825-1997
Where: m——the mass of the granular clay in the coarse-mesh test sieve, gm——the mass of the sample, g.
The amount of particles X less than the lower limit expressed as a mass percentage is calculated according to formula (3): m2x10.
Where: m2——the mass of the granular clay passing through the fine-mesh test sieve, g; m——the mass of the sample, g.
6.6.4 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 6.7 Determination of moisture content
6.7.1 Instruments and equipment
Weighing bottle: d40mm×25mm.
6.7.2 Analysis steps
.·(3)
Use a weighing bottle that has been dried to constant weight at 105~110℃ to weigh 1~2g of sample (accurate to 0.0002g), and dry it at 105~110℃ to constant weight.
6.7.3 Expression of analysis results
The moisture content X expressed as mass percentage is calculated according to formula (4): m1-m2×100.
Where: m1——mass of weighing bottle and sample before drying, g; m2——mass of weighing bottle and sample after drying, g; mass of sample, g.
6.7.4 Tolerance
Take the arithmetic mean of the results of parallel determinations as the determination result. The absolute difference between the parallel determination results shall not exceed 0.3%. 6.8 Determination of bulk density
6.8.1 Summary of method
The sample is freely dropped through a funnel into a measuring cylinder of known mass and volume. The bulk density of the sample is determined by weighing and calculating. 6.8.2 Instruments and equipment
Bulk density tester
As shown in the figure: The funnel is fixed on the bracket, and the measuring cylinder is located below the center line of the funnel, with a spacing of 30mm to 50mm. 4
6.8.3 Analysis steps
HG/T2825—1997
1—Funnel; 2—Baffle; 3—Stand; 4—Measuring cylinder (500mL) Figure 1 Bulk density tester
Let the sample fall freely through the funnel into a measuring cylinder of known mass and volume within 1 min. The cone of the sample should be higher than the wall of the measuring cylinder. Use a ruler to scrape off the higher part and accurately weigh the measuring cylinder containing the sample (accurate to 0.1g). 6.8.4 Expression of analysis results
Bulk density X expressed as mass per unit volume. Calculate according to formula (5): m1
Where: m1——mass of sample and measuring cylinder, 8; m2——mass of measuring cylinder, gs
V——volume of measuring cylinder, mL.
6.8.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.02g/mL. 6.9 Determination of initial activity of deolefination (measured by bromine index) 6.9.1 Summary of method
Put the granular clay sample into a column reactor and continuously introduce standard oil (bromine index is 100mgBr/100g oil) at the specified temperature, pressure and space velocity. The effluent is titrated with bromine standard titration solution in a special titration solvent, using a platinum electrode as the measuring electrode and a glass electrode as the reference electrode. The reaction endpoint is determined by the potential jump. 6.9.2 Reagents and materials
6.9.2.1 Potassium bromide solution: 300g/L;
6.9.2.2 Mercuric chloride methanol solution: 100g/L; 100g mercuric chloride is dissolved in methanol and diluted to 1000mL with methanol. 6.9.2.3 Special titration solvent: add 134mL carbon tetrachloride, 116mL methanol, 18mL sulfuric acid, 18mL mercuric chloride methanol solution, 10mL potassium bromide solution to 704mL glacial acetic acid in turn, and shake well. 6.9.2.4 Bromine standard titration solution: c (1/6KBrO3) about 0.1mol/L; 6.9.2.5 Bromine standard titration solution: c (1/6KBrOs) about 0.02mol/L; 5
HG/T2825—1997
Take 50mL of bromine standard titration solution c (1/6KBrO3)] about 0.1mol/L with known accurate concentration, place it in a 250mL volumetric flask, dilute to the mark with water, and shake well. 6.9.2.6 Preparation of standard oil (bromine index is 100mgBr/100g oil): add 3.25g styrene (accurate to 0.001g) to 5000g xylene and shake well. 6.9.3 Instruments and equipment
6.9.3.1 Micro high-pressure horizontal flow pump: flow range 0.04~9.00mL/min, maximum discharge pressure 5MPa, pulsation rate ±1%, reproducibility accuracy ±1%;
6.9.3.2 Needle valve;
6.9.3.3 Pressure gauge,
6.9.3.4 Stainless steel U-shaped reactor: inner diameter is d10X2m/m, height is 250m/m; 6.9.3.5 Constant temperature oil bath;
6.9.3.6 Potentiometer: accuracy 2mV/grid, range 500~600mV; 6.9.3.7 Indicator electrode: platinum electrode;
6.9.3.8 Reference electrode: glass electrode;
6.9.3.9 Electromagnetic stirrer;
6.9.3.10 Micro burette: graduation value 0.02mL. 6.9.4 Analysis steps
6.9.4.1 Deolefination reaction
Install the micro high pressure horizontal flow pump, needle valve, pressure gauge, U-shaped reactor and constant temperature oil bath as shown below. 2
1 Micro high-pressure horizontal flow pump; 2—needle valve; 3—pressure gauge; 4—U-shaped reactor; 5—constant temperature oil bath Figure 2 Granular clay deolefination reaction device
Take 20mL granular clay sample and load it into the U-shaped reactor. After it is packed tightly, the upper layers at both ends are filled with quartz sand with a particle size of 850-425μm. After tightening the reactor nut to seal it, heat the oil bath to 165±2℃, turn on the micro high-pressure horizontal flow pump, and inject standard oil to make its flow rate 20mL/h. After it flows out continuously and stably for 4h, collect 30g of the outflowing oil (test solution A) to determine the initial deolefination activity. 6.9.4.2 Determination of initial activity of deolefination (measured in terms of bromine index) Take 100 mL of special titration solvent and place it in a 250 mL beaker. Add 10 g of oil [test solution A (6.9.4.1)] (accurate to 0.01 g). Insert the electrode into the solution, start the electromagnetic stirrer, and drip about 90% of the required titration volume of bromine standard titration solution (6.9.2.5) from the burette. Record the electrode potential and the consumption of bromine standard titration solution. After that, measure the potential once every time 0.02 mL of bromine standard titration solution is added. Titrate until the potential value does not change much. Record the reading of the burette and the measured potential value after each dripping of bromine standard titration solution.
At the same time, carry out a blank test without adding oil (test solution A). The treatment of waste mercury liquid after the test shall be carried out in accordance with Appendix D of GB/T3051-82. 6.9.5 Determination of endpoint (graphic method)
Perform according to Article 6.2.1 of GB/T9725-88. 6
6.9.6 Expression of analysis results
HG/T2825-1997
In 100mL of oil (test solution A), the initial activity of deolefination expressed in milligrams of bromine (mgBr/100g oil) X is calculated according to formula (6):
Xe=-V)·oX0. 079.9×1 000×100m
(V1-V.)cX7990
Wherein: V,-
the volume of the bromine standard titration solution consumed in the titration, mL; the volume of the bromine standard titration solution consumed in the blank test, mL; the actual concentration of the bromine standard titration solution, mol/L; the mass of the oil (test solution A) taken, g; (6)
0.0799——with 1.00mL bromine standard titration solution [c (1/6KBrO:) = 1.000mol/L】equivalent to the mass of bromine expressed in grams.
6.9.7 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.02mgBr/100g oil.
6.10 Determination of particle pressure resistance
6.10.1 Summary of method
Take a sample of specified particle size, dry and cool it, and use a pressure measuring instrument to measure the pressure resistance of 50 particles respectively, and take the arithmetic mean as the result.
6.10.2 Instruments and equipment
Particle pressure measuring instrument: range 010N, accuracy 0.05N. 6.10.3 Analysis steps
Take 10mL of sample, sieve through the test sieve, take 800~630um particles of Class I products, take 630~560um particles of Class I products, place in a constant temperature oven at 105~110℃, dry for 2h, move to a dryer and cool to room temperature, take 50 samples by quartering method, and place each particle in the particle pressure measuring instrument for measurement. Turn on the instrument, as the pressure on the particles on the sensor increases, the force curve indicated by the recorder rises smoothly until a sudden change occurs when the particles disintegrate as a whole, record the corresponding resistance pressure Si, and measure 50 particles continuously. 6.10.4 Expression of analysis results
The particle resistance pressure X7 expressed in N is calculated according to formula (7): X7-
Wherein, S—is the resistance pressure of each particle, N; 50——the total number of particles for which the resistance pressure is measured. 6.11 Determination of decolorization rate
Except for the following modification in the preparation of asphalt lamp oil solution, the rest shall be carried out in accordance with the provisions of Section 5.1 of HG/T256994. 6.11.1 Preparation of asphalt kerosene solution
Peel off the outer surface of the construction petroleum asphalt with a knife and cut it into filaments. Weigh 0.8g (accurate to 0.01g) and place it in a 250mL beaker. Add a small amount of colorless kerosene oil and stir continuously in a 70-80℃ water bath until it is completely dissolved. Dilute it to 1000mL with colorless kerosene oil, mix well, and let it stand for 1h. Filter the entire solution with medium-speed qualitative filter paper and measure the absorbance with a spectrophotometer at a wavelength of 590nm using colorless kerosene oil as a reference. If the absorbance is greater than 1.05, dilute and shake the entire solution with colorless kerosene oil and re-measure the absorbance until it is 1.001.05.
7 Marking, packaging, transportation and storage
7.1 The packaging of granular clay should be firmly and clearly marked, including: manufacturer name, factory address, product name, model, trademark, net weight, batch number or production date, this standard number, and the "wet-afraid" mark specified in GB191-90. 7.2 Each batch of products leaving the factory should be accompanied by a quality certificate. The content includes: manufacturer name, factory address, product name, model, trademark, net weight, batch number or production date, proof that the product quality meets this standard and this standard number. 7.3 Granular clay is double-layered, with the inner packaging being a polyethylene plastic film bag with a thickness of not less than 0.05mm. The packaging volume should be larger than the outer packaging; the outer layer is a polypropylene woven bag, and its performance and inspection methods should comply with the provisions of GB/T8946-88B. Other packaging can be agreed with the user. The net weight of each bag is 20kg, 25kg, and 50kg. 7.4 When packaging, put the granular clay into the inner bag, exhaust the remaining air in the bag, tie the inner bag with vinyl rope or other rope of equivalent quality, fold the outer bag at a distance of not less than 30mm from the bag edge, and sew the outer bag with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the bag edge. The stitch length is 7-12mm, the stitches are neat and the stitch length is uniform. There is no leakage or skipping. 7.5 During transportation, the granular clay should be protected from rain, moisture, exposure and packaging damage. It should not be mixed with acidic and alkaline substances. 7.6 The granular clay should be stored in a ventilated, dry and corrosion-free warehouse.
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