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Chemical Industry Standard of the People's Republic of China
HG2322-92
Industrial Metal Sodium
Published on June 1, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on September 1, 1992
Chemical Industry Standard of the People's Republic of China
Industrial Metal Sodium
Subject Content and Scope of Application
HG2322-92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation, storage and safety requirements for industrial metal sodium.
This standard applies to industrial metal sodium obtained by salt method and alkali method electrolysis. This product is mainly used as a reducing agent for organic synthesis and certain metal smelting, a catalyst for synthetic rubber, a desulfurizing agent for petroleum, etc. It is also used as a raw material for chemical and pharmaceutical products. Molecular formula: Na
Relative molecular mass: 22.99 (according to the international relative atomic weight of 1989) 2 Reference standards
GB1250
GB3049
GB6682
3 Technical requirements
Dangerous goods packaging marking
Packaging storage and transportation pictorial marking
Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) Preparation of standard solutions for impurity determination.
Chemical reagents
Preparation of preparations and products used in chemical reagent test methods Methods for expressing and determining limit values General method for determining iron content in chemical products Specifications for laboratory water
3.1 Appearance: Silver-grey block, new cut surface is silvery white. 3.2 Industrial metallic sodium shall meet the requirements of the following table: Item
Main content (as Na)
Potassium (K) content
Calcium (Ca) content
Iron (Fe) content
Heavy metal (as Pb) content
O-phenanthroline spectrophotometry
% (m /m)
Superior quality
First quality
Note: For industrial metallic sodium produced by alkaline electrolysis, its calcium and potassium contents shall be inspected every six months during normal production. Approved by the Ministry of Chemical Industry of the People's Republic of China on June 1, 1992
Qualified products
Implemented on September 1, 1992
4 Test methods
HG2322-92
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB6682. The standard solutions, impurity standard solutions, preparations and products required in the test, unless otherwise specified, are prepared in accordance with the provisions of GB601, GB602 and GB603.
4.1 Determination of main content
4.1.1 Summary of the method
The metallic sodium sample solution is titrated with a hydrochloric acid standard titration solution using bromocresol green-methyl red as an indicator, and the main content is determined based on the consumption of the hydrochloric acid standard titration solution.
4.1.2 Reagents and materials
4.1.2.1 95% ethanol (GB679);
4.1.2.2 Hydrochloric acid (GB622) standard titration solution: c (HCI) is about 0.1 mol/L; 4.1.2.3 Bromocresol green (HG3-1226)-methyl red (HG3-938) indicator solution. 4.1.3 Analysis steps
Use filter paper to carefully remove the No. 15 white oil on the metal sodium block, cut about 2.5g of the sodium block from the middle part, clamp it with tweezers, and quickly put it into a dry weighing bottle. Weigh it by reduction method, accurate to 0.0002g. Place it in a 200mL beaker filled with 60mL ethanol and cover it with a watch glass. After the sodium is completely dissolved and the solution is cooled to room temperature, use 20-30mL water to rinse the surface blood above the cup. Transfer the solution to a 1000mL volumetric flask, dilute to the mark with water, and shake well. This solution is Solution A. Solution A is also used for the determination of potassium. Use a pipette to transfer 25mL of Solution A and place it in a 250mL conical flask. Add 2 drops of bromocresol green-methyl red indicator solution, and titrate with hydrochloric acid standard titration solution until the solution changes from green to dark red. Boil for 2 minutes, cool and continue to titrate until the solution turns dark red again. Perform a blank test at the same time.
4.1.4 Expression of analysis results
The main content (in terms of Na) (X) expressed as mass percentage shall be calculated according to formula (1): Xi
(VV.)cX0.02299
9×100
mx1000
91. 96 (V-Vo) c
Wherein: V is the volume of the standard hydrochloric acid solution consumed in titrating the sample solution, mL; V is the volume of the standard hydrochloric acid solution consumed in titrating the blank test solution, mL; c is the actual concentration of the standard hydrochloric acid solution, mol/L; m is the mass of the sample, g;
0.02299 is the mass of metallic sodium equivalent to 1.00 mL of the standard hydrochloric acid solution c (HCI=1.000mol/L), expressed in grams.
4.1.5 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 0.2%. 4.2 Determination of potassium content
4.2.1 Method summary
The potassium content in the sample is determined by measuring the absorbance of the atomic vapor generated by the sample solution and the standard solution to the radiation of a specific wavelength of potassium.
4.2.2 Materials for reagents
4.2.2.1 Standard sodium chloride (GB1253); 4.2.2.2 Hydrochloric acid (GB622) solution: 1+1; HG2322-92
4.2.2.3 Potassium standard solution: 1 mL of solution contains 0.100 mg of potassium (K); 4.2.2.4 Potassium standard solution: 1 mL of solution contains 0.010 mg of potassium (K); Preparation: Use a pipette to transfer 10 mL of potassium standard solution (4.2.2.3) into a 100 mL volumetric flask, dilute to the mark with water, and shake well.
4.2.3 Instruments and equipment
4.2.3.1 Atomic absorption spectrophotometer;
4.2.3.2 Potassium hollow cathode lamp;
4.2.3.3 Wavelength: 766.5nm;
4.2.3.4 Flame: acetylene-air.
4.2.4 Analysis steps
4.2.4.1 Drawing of working curve
Take a series of 100mL volumetric flasks, add 0.32g of standard sodium chloride to each, add 0, 1.00, 2.00, 3.00mL of potassium standard solution (4.2.2.4) to the superior products, and add 0, 0.50, 1.00, 1.50mL of potassium standard solution (4.2.2.3) to the first-class products, dilute to the scale with water, and shake. Use an atomic absorption spectrophotometer to measure the absorbance at a wavelength of 766.5nm with water as the reference. Subtract the absorbance of the reagent blank test from the absorbance of each standard reference solution, and draw a working curve with the mass concentration of potassium as the horizontal axis and the corresponding absorbance as the vertical axis.
4.2.4.2 Determination
Use a pipette to transfer 50mL of solution A in Section 4.1.3 and place it in a platinum or quartz evaporating blood. Neutralize with hydrochloric acid solution, use a wide range pH test paper to check that the pH is close to 7, then add 0.2-0.3mL of excess hydrochloric acid solution and place it on an adjustable electric furnace to evaporate to dryness. After the residue is dissolved in 20mL of water, transfer it to a 1000mL volumetric flask, add water to the scale, and shake well. This solution is solution B. Solution B is also used for the determination of calcium. Use an atomic absorption spectrophotometer to measure the absorbance at a wavelength of 766.5nm with water as the reference, and find the mass concentration of potassium from the working curve.
4.2.4.3 Blank test solution
When measuring the test solution, except for not adding the sample, other operations and the amount of reagents added are processed in the same way as the test solution. This solution is solution C. Solution C is also used for the determination of calcium. 4.2.5 Expression of analytical results
The potassium (K) content (X) expressed as mass percentage is calculated according to formula (2): X2 = (pP) X100X10-8)
mx1000
200(p2-p)
Where: P is the mass concentration of potassium in the sample solution found from the working curve, mg/mL; L is the mass concentration of potassium in the blank test solution found from the working curve, mg/mL; and L is the mass of the sample, g.
4.2.6 Allowable error
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 0.005%. 4.3 Determination of calcium content
4.3.1 Method Summary
HG2322-92
The calcium content in the sample is determined by measuring the absorbance of the atomic vapor generated by the sample solution and the standard solution to the radiation of a specific wavelength of calcium.
4.3.2 Reagents and Materials
4.3.2.1 Standard sodium chloride (GB1253); 4.3.2.2 Calcium standard solution: 1mL solution contains 0.100mL calcium (Ca); 4.3.3 Instruments and Equipment
4.3.3.1 Atomic absorption spectrophotometer;
4.3.3.2 Calcium hollow cathode lamp;
4.3.3.3 Wavelength: 422.7nm;
4.3.3.4 Flame: acetylene-air.
4.3.4 Analysis steps
4.3.4.1 Drawing of working curve
Take 5 100mL volumetric flasks, add 0.32g of standard sodium chloride to each, and add 0, 0.50, 1.00, 1.50, and 2.00mL of calcium standard solution respectively. Dilute with water to the scale and shake well. Use an atomic absorption spectrophotometer to measure the absorbance at a wavelength of 422.7nm with water as the reference. Subtract the absorbance of the reagent blank test from the absorbance of each standard reference solution, and draw a working curve with the mass concentration of calcium as the horizontal axis and the corresponding absorbance as the vertical axis. 4.3.4.2 Determination
Measure the absorbance of solution B retained in 4.2.4.2 and solution C retained in 4.2.4.3 on the atomic absorption spectrophotometer at a wavelength of 422.7nm, and find the mass concentration of calcium from the working curve. 4.3.5 Expression of analysis results
Calcium (Ca) content (X) expressed as mass percentage is calculated according to formula (3): Xs = (pp) × 100 × 10-s)
mx1000
200 (p2-)
Where: P is the mass concentration of calcium in the sample solution obtained from the working curve, mg/mL; P is the mass concentration of calcium in the blank test solution obtained from the working curve, mg/mL; pr
m is the mass of the sample, g.
4.3.6 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 0.003%. 4.4 Determination of iron content
4.4.1 Summary of method
Same as Article 2 of GB3049.
4.4.2 Reagents and materials
4.4.2.1 95% ethanol (GB679);
4.4.2.2 Hydrochloric acid (GB622) solution: 1+1; 4.4.2.3 Phenolyl (GB10729) indicator solution: 1g/L; 4.4.2.4 Ammonia water (GB631);
Others are the same as Article 3 of GB3049.
4.4.3 Instruments and equipment
(3)
HG2322-92
4.4.3.1 Spectrophotometer: with a 3cm absorption cell. 4.4.4 Drawing of working curve
Draw the working curve according to Article 5.3 of GB3049 using a 3cm absorption cell and the corresponding amount of iron standard solution. 4.4.5 Analysis steps
4.4.5.1 Preparation of test solution
Use filter paper to carefully remove the No. 15 white oil on the sodium metal block, cut about 2g of the sodium metal block from the middle part, clamp it with tweezers, quickly put it into a dry weighing bottle, and weigh it by reduction method, accurate to 0.01g. Place the sample in a 200mL beaker containing 40mL of ethanol and cover it with a watch glass. After the sample is completely dissolved, add 40-50mL of water and 2 drops of phenolphthalein indicator solution. Add hydrochloric acid solution until the red color of the solution disappears, and then add 3 drops in excess. Then place the beaker on an adjustable electric furnace and heat it to evaporate until dry (note that when starting to heat, the electric furnace temperature should be controlled at about 70℃, and the temperature should be raised when the ethanol evaporates to dryness and there is no ethanol smell). Remove the beaker, cool it to room temperature, and add 2 drops of hydrochloric acid solution. Rinse the dried beaker with water, transfer all the solution into a 100mL volumetric flask, and add water to about 40mL. 4.4.5.2 Preparation of blank test solution
In another 200mL beaker, add 40mL of ethanol, 40~50mL of water, 2 drops of phenolic indicator solution, 14mL of hydrochloric acid solution, and about 16mL of ammonia water until the solution turns red. Add hydrochloric acid solution until the red color of the solution disappears, and proceed from "..add 3 drops of excess...." according to 4.4.5.1. 4.4.5.3 Determination
In two 100mL volumetric flasks containing the test solution and the blank test solution, proceed from "..add water to about 60mL if necessary." according to 5.4 of GB3049. 4.4.6 Expression of analysis results
The iron (Fe) content (X) expressed as mass percentage is calculated according to formula (4): m2-mi
Wherein: m2—the iron mass of the test solution obtained from the working curve, mg; m1—the iron mass of the blank test solution obtained from the working curve, mg; m—the mass of the sample, g.
4.4.7 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 0.005%. 4.5 Determination of heavy metal content
4.5.1 Summary of the method
(4)
Heavy metal ions react with negative divalent sulfide ions in acetic acid medium to form colored sulfide precipitates. When the heavy metal content is low, a stable dark suspension is generated, which can be used for visual colorimetric determination of heavy metals. 4.5.2 Reagents and materials
4.5.2.1 30% acetic acid (HG3—1095);
4.5.2.2 95% ethanol (GB679)
4.5.2.3 Hydrochloric acid (GB622) solution: 1+1; 4.5.2.4 Sodium hydroxide (GB629) solution: 100g/L; 4.5.2.5 Saturated hydrogen sulfide solution: This solution is freshly prepared; 5
HG2322—92
4.5.2.6 Lead standard solution: 1mL solution contains 0.025mg lead (Pb) Preparation: Use a pipette to transfer 25mL of the lead standard solution prepared according to GB602, place it in a 100mL volumetric flask, dilute to the scale with water, and shake well.
4.5.2.7 Phenol (GB10729) indicator solution: 1g/L. 4.5.3 Analysis stepsbzxZ.net
Use filter paper to carefully remove the No. 15 white oil on the metal sodium block, and cut about 2.00±0.01g of the sodium block from the middle part. Clamp it with tweezers and quickly put it into a dry weighing bottle, and weigh it by reduction method. Put it in a 200mL beaker containing 60mL ethanol and cover it with surface III. After the sample is completely dissolved, rinse the surface blood with water, transfer the test solution to a 100mL volumetric flask, dilute it to the scale with water, and shake it well. Use a pipette to transfer 25mL of the test solution into a 50mL colorimetric tube, add 1 drop of phenolic acid indicator solution, adjust the pH to neutral with hydrochloric acid solution, and add 4mL in excess. After leaving it for 10 minutes, adjust the pH to neutral with sodium hydroxide solution (check with factory-made pH test paper). Add 0.4mL acetic acid solution, add 10mL freshly prepared saturated hydrogen sulfide solution, dilute to scale, shake well. Place in dark place for 10min. Observe against white background, the dark color should not be darker than the standard. The standard is to take 1.00mL lead standard solution, place it in a 50mL colorimetric tube, add water to the volume of 25mL, and treat it in the same way as the test solution.
5 Inspection rules
5.1 Industrial sodium metal should 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 industrial sodium metal products shipped meet the requirements of this standard. Each batch of products shipped shall be accompanied by a quality certificate, including: manufacturer name, product name, grade, net weight, batch number or production date, factory date, proof that the product quality meets this standard and the number of this standard. 5.2 The user has the right to accept the industrial sodium metal received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 4t.
5.4 Take samples from 5% of the packaging units of each batch of products, and at least two sampling units shall be taken. When sampling, randomly select a piece of metallic sodium from each barrel and quickly cut it with a knife (the amount cut shall not be less than 50g). The total sampling amount shall not be less than 200g. Divide it into two clean and dry bottles pre-filled with No. 15 white oil and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used for inspection and one bottle is kept for three months as a backup. 5.5 If one indicator of the inspection result does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging. If even one indicator of the verification result does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 5.7 This standard adopts the rounded value comparison method specified in GB1250 to determine whether the inspection results meet the standard. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging barrel should have firm and clear markings, including: manufacturer name, product name, trademark, grade, net weight, batch number or production date, factory date and this standard number, as well as mark 10 "flammable items when wet" mark specified in GB190 and mark 3 "upward" mark and mark 6 "afraid of moisture" mark specified in GB191. 6.2 Industrial metal sodium adopts three-layer packaging, the inner packaging adopts a two-layer polyethylene plastic film bag, the specification size is: 1200mm×700mm, the thickness is 0.08~0.1mm; the outer packaging adopts a special sealed full-open iron barrel, the specification size is Φ415mm in diameter, 630mm in height, and 1mm in thickness.
When packing industrial sodium metal, first dip the sodium ingot into No. 15 white oil, then put it into a special sealed fully open iron barrel lined with a two-layer polyethylene plastic film bag, remove the remaining gas in the bag, tie the bag tightly with vinyl rope (tying method: tie once, fold over and tie again), cover the barrel lid, and seal it with a foamed oil-resistant rubber gasket. Tighten it with a clamping ring and pin it with a T-shaped iron pin. The net weight of each barrel of industrial sodium metal is 40kg. 6.3 When transporting industrial sodium metal, it must be transported in a closed means of transportation to prevent water from entering the packaging barrel. During transportation, pay attention to waterproofing, heat protection, and impact protection, stay away from flammable materials, and barrels containing sodium metal are prohibited from being placed horizontally or inverted. 6
HG2322—92
6.4 Industrial sodium metal should be stored in a ventilated, dry and fireproof warehouse. The floor inside the warehouse should be higher than the outdoor floor. Water pipes and heating should not be installed in the warehouse, and water should not enter the roof doors and windows. There should be a passage for inspection and transportation in the warehouse, and necessary fire-fighting equipment should be prepared. Pay attention to moisture, heat, shock and keep away from flammable materials.
6.5 Under the storage and transportation conditions of this standard, the storage period of industrial sodium metal products is 1 year from the date of ex-factory. 7 Safety requirements
7.1 Industrial sodium metal has strong chemical activity. It can directly combine with many metals or non-metals. It oxidizes rapidly in the air. It reacts violently with water, causing combustion and explosion. Contact with the skin can easily cause burns. Sodium falling into the eyes and mucous membranes is dangerous. 7.2 Industrial sodium metal is strictly prohibited from contacting with water. The sodium metal sample must be stored in No. 15 white oil and cannot be in contact with air. In dry air, it will spontaneously ignite when the temperature reaches above 115°C. 7.3 All operators who come into contact with sodium metal must abide by the following rules: Safety regulations must be followed when using sodium metal. Operators must wear work clothes that meet standard specifications, glasses, masks, and rubber gloves to avoid burns caused by contact with the skin. 7.4 All work involving metallic sodium should be carried out in a well-ventilated, clean, dry and open place. 7.5 In the event of a fire, dry sand, dry powder and asbestos cloth can be used to extinguish the fire. The use of water, foam, acid, alkali, carbon tetrachloride and carbon dioxide fire extinguishers is not allowed.
Additional notes:
This standard is proposed by the Science and Technology 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 the Guanjin Chemical Research Institute of the Ministry of Chemical Industry and Beijing Chemical Plant No. 4. The main drafters of this standard are Liu Shuying, Shi Jie, Wang Shuli and Zhao Mingshan. This standard refers to the Soviet national standard "OCT3273-75 (valid from 1977.1.1 to 1992.1.1) "Industrial Metallic Sodium". 7
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