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Chemical Industry Standard of the People's Republic of China
HG/T2569—94
Activated White Clay
Published on February 9, 1994
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
Chemical Industry Standard of the People's Republic of China
Activated White Clay
Subject Content and Scope of Application
HG/T2569—94
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of activated white clay. This standard applies to activated white clay made from bentonite as raw material. This product is mainly used for the decolorization and refining of petroleum processing products (lubricating oil, paraffin, vaseline), industrial animal and vegetable oils and edible animal and vegetable oils; it is used as an adsorbent and catalyst carrier in the chemical industry. 2 Reference standards
Packaging, storage and transportation pictorial symbols
GB/T601
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of standard solutions for determination of impurities of chemical reagents GB/T602
Preparation of preparations and products used in test methods of chemical reagents GB/T603
GB/T610.1 General method for determination of arsenic by chemical reagents (arsenic spot method) GB1250
Expression method and determination method of limit values GB/T6678
GB/T6679
General rules for sampling of chemical products
General rules for sampling of solid chemical products
GB/T6682 Specifications and test methods for water used in analytical laboratories GB8946
Plastic woven bags
3 Product classification,
Models and codes
The classification, model and code of activated white clay are shown in Table 1. Table 1
Model and code
(Activated clay with high activity)
(Activated clay with high decolorization rate)
Main application Decolorization and refining of petroleum processing products (lubricating oil, paraffin, vaseline) 4 Technical requirements
4.1 Appearance: powdery solid, free of mechanical impurities. 4.2 Activated clay shall meet the requirements of Table 2.
Approved by the Ministry of Chemical Industry of the People's Republic of China on February 9, 1994 1
Decolorization and refining of industrial animal and vegetable oils
Decolorization and refining of edible animal and vegetable oils
Implemented on July 1, 1994
Decolorization rate, %
Activity
Free acid (in terms of HSO), %
Water, %
Particle size (through 75um sieve), %
Filtration speed, mL/min
Bulk density, g/mL
Heavy metal (in terms of Pb), %
Arsenic (As), %
Test method
HG/T256994
Qualified product
First-class product
Qualified product
Qualified product
Qualified product
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and grade 3 water specified in GB/T6682.
The standard titration solution, impurity standard solution, preparation and product required in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601GB/T602 and GB/T603.
5.1 Determination of decolorization rate
5.1.1 Summary of the method
Take a certain volume of asphalt lamp oil solution with known absorbance, add a certain amount of sample to decolorize, and determine the absorbance of the decolorized asphalt lamp oil solution. Calculate the decolorization rate expressed as a percentage based on the decrease in absorbance. 5.1.2 Reagents and materials
5.1.2.1 Kerosene for lamps (GB253).
5.1.2.2 Petroleum asphalt for construction (GB494). 5.1.3 Instruments and equipment
5.1.3.1 Spectrophotometer: equipped with a 1cm absorption cell. 5.1.3.2 Electric oscillator: frequency 240 times/min. 5.1.4 Analysis steps
5.1.4.1 Preparation of colorless lamp oil
Weigh 200g of activated white clay that has been dried at 105-110℃ in advance, place it in 1000mL lamp kerosene, stir vigorously for 10min, filter it with medium-speed qualitative filter paper and place it in a clean and dry container. Use a spectrophotometer to measure the absorbance at a wavelength of 590nm with water as a reference. Its absorbance should be zero.
5.1.4.2 Preparation of asphalt lamp oil solution
HG/T2569-94
Peel off the outer surface of building petroleum asphalt with a knife, cut it into filaments, weigh 0.74-0.75g and place it in a 250mL beaker, add a small amount of colorless lamp oil, and stir continuously in a 70-80℃ water bath until it is completely dissolved. Dilute to 1000mL with colorless kerosene, mix well, and let stand for 1h; use a spectrophotometer to measure the absorbance at a wavelength of 590nm, using colorless kerosene as a reference. The absorbance should be 1.001.05. 5.1.4.3 Determination
Weigh 1.50±0.01g of the sample and place it in a clean and dry 250mL conical flask with a ground stopper. Use a pipette to add 50mL of asphalt kerosene solution, shake it gently a few times, and place it on an electric shaker for 60min (accurate to 1min); filter the entire solution with medium-speed qualitative filter paper, shake the filtrate well, and use a spectrophotometer to measure the absorbance at a wavelength of 590nm, using colorless kerosene as a reference. 5.1.5 Expression of analytical results
The decolorization rate Xi expressed as a percentage is calculated according to formula (1): Ao-A1V
Where: A. ——Absorbance of asphalt lamp oil solution before decolorization; A1——Absorbance of asphalt lamp oil solution after decolorization. 5.1.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference between the two parallel determination results shall not exceed 2%. 5.2 Determination of activity
5.2.1 Summary of method
Replace the hydrogen ions in the sample with sodium acetate solution. Use phenolphthalein as the indicator and titrate with sodium hydroxide standard titration solution. The volume (mL) of sodium hydroxide solution consumed by 1000g sample [c (NaOH) = 1.000mol/L] represents the activity. 5.2.2 Reagents and materials
5.2.2.1 Standard titration solution of sodium hydroxide (GB/T629): c (NaOH) is about 0.1mol/L. 5.2.2.2 Sodium acetate solution: c (CHgCOONa) = 0.1mol/L. Weigh 13.60g sodium acetate trihydrate (CH2COONa·3H2O) (GB/T694) to the nearest 0.01g and dissolve in 1000mL water. 5.2.2.3 Phenolphthalein (GB/T10729) indicator solution: 10g/L. 5.2.3 Instruments and equipment
5.2.3.1 Electric oscillator: frequency 240 times/min. 5.2.4 Analysis steps
(GB/T693) or 8.20g of anhydrous sodium acetate Weigh 20.00±0.01g of sample and place it in a 250mL clean and dry conical flask with a ground stopper; add 100mL of sodium acetate solution with a pipette, cover the bottle stopper, shake it vigorously for a few times, and quickly place it on an electric shaker for 15 minutes; dry filter, discard the initial part of the filtrate, use a pipette to transfer 50mL of the filtrate and place it in another 250mL conical flask, add 3 drops of phenolphthalein indicator solution, and titrate with sodium hydroxide standard titration solution until it turns slightly red and remains unfaded for 30 seconds as the end point. At the same time, replace the sodium acetate solution with water and perform a blank test according to the above steps. Note: When performing this operation, the sample temperature and ambient temperature should be 20-25℃. 5.2.5 Expression of analysis results
The activity X2 expressed as the volume (mL) of sodium hydroxide standard titration solution [c (NaOH) = 1.000 mol/L) consumed by 1000 g of sample is calculated according to formula (2):
HG/T256994
1-V). ×1 000
20×100
=100×(Vi-V2)c
Wherein: V1——the volume of sodium hydroxide standard titration solution consumed by sodium acetate replacement solution, mL; V2——the volume of sodium hydroxide standard titration solution consumed by blank test, mL; V1——the actual concentration of sodium hydroxide standard titration solution, mol/L. 5.2.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 3. 5.3 Determination of free acid
5.3.1 Method summary
The free acid in the sample is extracted with water. Phenolphthalein is used as the indicator and titrated with sodium hydroxide standard titration solution. 5.3.2 Reagents and materials
5.3.2.1 Sodium hydroxide (GB/T629) standard titration solution: c (NaOH) about 0.02mol/L. (2)
Take 50mL of sodium hydroxide standard titration solution c (NaOH) with known accurate concentration of about 0.1mol/LJ, place it in a 250mL volumetric flask, dilute to the mark with carbon dioxide-free water, and shake the spoon to hook. 5.3.2.2 Phenol (GB/T10729) indicator solution: 10g/L. 5.3.3 Analysis steps
Weigh 1~2g of sample (accurate to 0.0002g), place it in a 150mL beaker, add 50mL of water and boil for 3min, 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 with an alkali asbestos drying tube, cool to room temperature, add 2~3 drops of phenolic indicator solution, and titrate with sodium hydroxide standard titration solution until it turns slightly red and does not fade for 30s as the end point.
At the same time, take 100mL of water and perform a blank test in the same way. 5.3.4 Expression of analytical results
The free acid content (in terms of H,SO) expressed as a mass percentage X: calculated according to formula (3): (,-V):eX0. 049×100www.bzxz.net
4.9X (V1-Vo) c
Wherein: V1——the volume of sodium hydroxide standard titration solution consumed by the titration test solution, mL; V. The volume of sodium hydroxide standard titration solution consumed by the blank test, mL; c——the actual concentration of sodium hydroxide standard titration solution, mol/L; m——the mass of the sample, g;
(3)
0.049——the mass of sulfuric acid in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.04%. 5.4 Determination of moisture
5.4.1 Instruments and equipment
Weighing bottle: Φ40mmX25mm.
5.4.2 Analysis steps
HG/T256994
Weigh 12g of sample (accurate to 0.0002g) using a weighing bottle that has been dried to constant weight at 105~110℃. Dry at 105~110℃ to constant weight.
5.4.3 Expression of analysis results
The moisture content X expressed as mass percentage is calculated according to formula (4): ml-m2×100
Wherein: m1——mass of weighing bottle and sample before drying, g; m2——mass of weighing bottle and sample after drying, g; m——mass of sample, g.
5.4.4 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference between the two parallel determination results shall not exceed 0.5%. 5.5 Determination of particle size
5.5.1 Instruments and equipment
Test sieve (GB6003): R40/3 series, @Φ200mm×50mm/0.075mm. 5.5.2 Analysis steps
Weigh about 50g of sample (accurate to 0.01g), place it in the test sieve, shake and tap it continuously, and brush it gently with a No. 6 brush until the sample under the sieve does not exceed 0.1g within 1 minute; weigh the mass of the sieve residue. 5.5.3 Expression of analysis results
Particle size X expressed as mass percentage: Calculate according to formula (5): mml
Mass of sample, g;
Where: m
m1——Mass of sieve residue, g.
5.5.4 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference between the two parallel determination results shall not exceed 2%. 5.6 Determination of Filtration Rate
5.6.1 Summary of Method
(5)
Take a certain amount of sample and soak it with water, disperse it, and make a filter cake in a Buchner funnel of specified diameter under a certain pressure difference; keep the water surface higher than the filter cake surface and maintain a certain pressure difference for suction filtration; record the volume of filtered water within a certain period of time. 5.6.2 Instruments and Equipment
5.6.2.1 Buchner funnel: inner diameter 80mm.
5.6.2.2 Vacuum pump, equipped with a U-tube mercury vacuum pressure gauge. 5.6.3 Analysis steps
Weigh 30.0±0.1g of sample, place in a 250mL beaker, add about 100mL of water, stir thoroughly to disperse; transfer all to a Büchner funnel covered with two layers of rapid qualitative filter paper, start the vacuum pump, maintain the difference between the liquid levels at both ends of the U-tube mercury vacuum pressure gauge at 150mm, filter, drain (the filter cake must not have cracks), pour out the water in the suction flask, and reconnect the vacuum system. Add water to the Büchner funnel, start the vacuum pump, maintain the difference between the liquid levels at both ends of the U-tube mercury vacuum pressure gauge at 150mm, and filter. During the filtration process, the water level should always be higher than the filter cake surface: start the stopwatch when the first drop of water drips from the Büchner funnel, and stop filtration at 30 minutes; use a measuring cylinder to measure the volume of water in the suction flask. 5
5.6.4 Expression of analysis results
HG/T256994
Filtration rate X expressed in mL/min: Calculate according to formula (6): V
The volume of water in the suction filtration bottle, mL.
Where. V—
5.6.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.5ml/min. 5.7 Determination of bulk density
5.7.1 Instruments and equipment
Graduating cylinder: capacity 100mL, inner diameter about 25mm. 5.7.2 Analysis steps
Weigh 50.0±0.1g of sample and add it into a clean, dry 100mL measuring cylinder in four times. After each addition, vibrate on a rubber-covered test bench until the volume remains unchanged. Vibration method: lift the measuring cylinder by about 10 cm, and then let it fall naturally on the test bench. Rotate the measuring cylinder each time it is lifted.
5.7.3 Expression of analytical results
The bulk density X expressed in g/mL is calculated according to formula (7): Xr
Where: V is the volume of the sample after vibration, mL. 5.7.4 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.05 g/mL. 5.8 Determination of heavy metal content
5.8.1 Summary of the method
In a slightly acidic medium, heavy metal ions react with hydrogen sulfide to generate sulfide precipitation and form a dark suspension. Compare with the standard colorimetric solution.
5.8.2 Reagents and materials
5.8.2.1 Ascorbic acid;
5.8.2.2 Hydrochloric acid (GB/T622) solution: 1+4;5.8.2.3
Hydrochloric acid (GB/T622) solution: 1+16;
Ammonia (GB/T631) solution: 1+4;
5.8.2.5 Acetic acid-sodium acetate buffer solution: pH is about 3;5.8.2.6 Saturated hydrogen sulfide water: prepare before use;5.8.2.7 Lead standard solution: 1mL contains 0.02mgPb. Use a pipette to transfer 20mL of the lead standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute to the mark with water, and shake well. This solution is prepared when used.
5.8.3 Instruments and equipment
Colorimetric tube: 50mL.
5.8.4 Analysis steps
5.8.4.1 Preparation of test solution
Weigh 10.0±0.1g of sample and place it in a 150mL conical flask; add 50mL of hydrochloric acid solution (5.8.2.2), oscillate a few times, boil for 10min, cool, filter into a 100mL volumetric flask, wash with 10mL of water each time, wash 5 times, dilute with water to the scale, and shake well at 6
.
5.8.4.2 Determination
HG/T2569—94
Use a pipette to transfer 20 mL of the test solution (5.8.4.1), place it in evaporator III, and evaporate it to dryness in a boiling water bath; dissolve it with 10 mL of hydrochloric acid solution (5.8.2.3), transfer it all to a 50 mL colorimetric tube, and adjust the pH to about 2 with ammonia water (check with a wide range pH test paper). Add 0.1 g ascorbic acid, 5 mL of buffer solution, and 10 mL of saturated hydrogen sulfide water, dilute with water to the scale, and shake well. Place it in a dark place for 10 minutes. The color should not be darker than that of the standard colorimetric solution. Preparation of standard colorimetric solution: Pipette 5 mL of the lead standard solution, add 10 mL of water, and adjust the pH to about 2 with ammonia water or hydrochloric acid solution (5.8.2.3) (check with a wide range pH test paper). The following is handled in the same way as the sample. 5.9 Determination of arsenic content
5.9.1 Summary of method
Same as Article 3 of GB/T610.1.
5.9.2 Reagents and materials
5.9.2.1 Hydrochloric acid (GB/T622);
5.9.2.2 Arsenic-free zinc (GB/T2304);
5.9.2.3 Potassium iodide (GB/T1272);
5.9.2.4 Stannous chloride (GB/T638) solution: 400g/L;5.9.2.5
Lead acetate cotton;
5.9.2.6 Mercuric bromide test paper;
5.9.2.7 Arsenic standard solution: 1mL contains 0.002mgAs. Use a pipette to transfer 20mL of the standard solution prepared according to GB/T602, place it in a 1000mL volumetric flask, dilute with water to the scale, and shake well. This solution is prepared when used. 5.9.3 Instruments and equipment
Same as Article 5 of GB/T610.1.
5.9.4 Analysis steps
Use a pipette to transfer 20mL of the test solution (5.8.4.1) and place it in a wide-mouth bottle. Add 50mL of water, 2.5mL of hydrochloric acid, 1g of potassium iodide and 5 drops of stannous chloride solution, shake well and place for 10 minutes; then add 2.5g of arsenic-free zinc and immediately put it into a glass tube pre-filled with lead acetate cotton and mercuric bromide test paper. Place it in a dark place at 25-30℃ for 1 hour. The color of the arsenic spot on the mercuric bromide test paper shall not be darker than the standard arsenic spot. Preparation of standard arsenic spot: Transfer 5mL of arsenic standard solution, place it in a wide-mouth bottle, and add about 65mL of water. Treat it in the same way as the test sample.
6 Inspection rules
6.1 Activated white clay shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality certificate, which shall include the name of the manufacturer, address, product name, category, model, grade, net weight, batch number or production date, and the certificate and standard number of the product quality in accordance with this standard. 6.2 The user has the right to inspect and accept the activated clay received in accordance with the provisions of this standard. The inspection and acceptance shall be carried out within one month from the date of arrival of the goods.
6.3 Each batch of products shall not exceed 60t.
6.4 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB/T6678. When sampling, insert the sampler along the vertical center line of the packaging bag to 2/3 of the depth of the material layer. The sample taken from each bag shall not be less than 50g; bulk products shall be sampled in accordance with the provisions of Articles 1.2.3.2 and 2.3.1.2 of GB/T6679. Mix the sample thoroughly, reduce it to about 1000g by quartering method, and immediately put it into two clean and dry wide-mouth bottles and seal them. A label is attached to the bottle, indicating the manufacturer's name, product name, category, model, grade, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other is kept for reference. 6.5 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging. If the inspection results7
HG/T2569-94
even if only one indicator does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 6.7 The rounded value comparison method specified in GB1250 shall be used to determine whether the inspection results meet the standards. 7 Marking, packaging, transportation, storage
7.1 The activated white clay packaging bag should have firm and clear markings, including the manufacturer's name, address, product name, trademark, category, model, grade, net weight, batch number or production date, this standard number and the "wet-afraid" mark specified in GB191. 7.2 Activated clay is double-layered, the inner packaging is polyethylene film bag, the thickness is not less than 0.03mm, the packaging volume should be larger than the outer packaging; the outer packaging is polypropylene plastic woven bag, its performance and inspection method should comply with the provisions of GB8946; the net weight of each bag is 25kg, 40kg, 50kg.
When the user needs, activated clay can be bulked by car or ship. 7.3 The inner bag of the package is tied with vinyl rope or other ropes of equivalent quality, and the outer bag is sewn with a sewing machine. The stitches should be neat, without leaking seams or skipping.
7.4 Activated clay should be covered during transportation to avoid rain and moisture. 7.5 Activated clay should be stored in a ventilated and dry warehouse. Additional remarks:
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. This standard is drafted by Lin'an Bentonite Chemical Plant, Yuhang Qiushan Magnetic Clay Mine, and Yixian Petroleum Clay Plant. The main drafters of this standard are Kong Bingyan, Wang Chunlin, Zhu Jianxiong, Wang Pinghua, Yu Songquan and Huang Fuyuan.5 Activated clay should be stored in a ventilated and dry warehouse. Additional remarks:
This standard was 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 the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Lin'an Bentonite Chemical Plant, Yuhang Qiushan Magnetic Clay Mine, and Yixian Petroleum Clay Plant. The main drafters of this standard are Kong Bingyan, Wang Chunlin, Zhu Jianxiong, Wang Pinghua, Yu Songquan, and Huang Fuyuan. 85 Activated clay should be stored in a ventilated and dry warehouse. Additional remarks:
This standard was 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 the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Lin'an Bentonite Chemical Plant, Yuhang Qiushan Magnetic Clay Mine, and Yixian Petroleum Clay Plant. The main drafters of this standard are Kong Bingyan, Wang Chunlin, Zhu Jianxiong, Wang Pinghua, Yu Songquan, and Huang Fuyuan. 8
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