Some standard content:
GR19306—?D3
Chapter 3, Article 4.1, Chapter 5, Chapter 6, Chapter 7 and Chapter 8 of this standard are mandatory, and the rest are recommended. This standard is formulated on the basis of Chemical Industry Standard 1C255-2001 Sodium Hydroxide. This standard shall be effective from the date of implementation: 3255:200161 Chemical Industry Standard. Appendix A of this standard is informative.
This standard is used by China Petrochemical Industry Association. This standard is under the jurisdiction of the Inorganic Chemical Industry Branch of the National Chemical Standardization Technical Committee (SAC/1Y%3/S1>). The beneficiaries of this standard are: Renyang Chemical Research and Design Institute, Sino-foreign joint venture Anjiu Anqiu Xianguang Chemical Co., Ltd., Tianze Huasheng Chemical Co., Ltd., Shanghai Petrochemical Duanjun Co., Ltd. Chemical Division, Tuokuai Chemical Co., Ltd., Jiangning Shunshunhua Chemical Enterprise Co., Ltd., Hebei Chengxin Co., Ltd. The main contributors are: Pei Fengsai, Tu Shui, Liu Youming, Zong Xinling, Ding Weifeng, Jiang Yong, Luo Wenwu, Zhongnuoshan, Jia Wensheng. The standard replaced by this standard is ZRG1202. 0—1990.TIG2::—201.1 Scope
Industrial Sodium Cyanide
B19306—2003
This standard specifies the requirements, test methods, inspection criteria, marking, labeling, packaging, transportation, storage and safety of industrial sodium cyanide. This standard is applicable to industrial sodium cyanide and sodium cyanide solution. The product is mainly used in chemical, electrical, metallurgical, and pharmaceutical industries as raw materials.
Molecular formula NaCN
Relative molecular weight: 4.01 (quality according to national standard 1550) 2 Normative references
The following are the relevant information: Many clauses in the document have become the clauses of the standard before being cited in this standard. They are dated reference texts. All the revisions (excluding the contents of the inspection and guarantee) or the versions of the documents are not applicable to this standard. However, the parties who have reached an agreement on this standard are encouraged to study whether the latest version of the document can be used. For all undated reference documents, the latest version is applicable to this standard. GB190 Labeling of dangerous goods packaging
GB/T1250 Method for indicating the value of the technical limit GB/T6578 General rules for the purchase of chemical products
GB/T5550 General rules for the purchase of liquid chemical products GB/T682 —1992 New test filling water specifications and test methods (e91S036951987) GB10268-203 Weekly new chemical packaging
EG/T359.1 Preparation of standard solutions for analysis of inorganic chemical products HG/T3691, 3 Preparation of preparations and products for chemical analysis of inorganic chemical products TJ361979 Industrial enterprise design hygiene standards 3 Requirements
3.1 Appearance:
Solid sodium chloride should be white flakes, blocks or granules. Sodium chloride concentrate should be colorless or yellowish water-soluble. 3.2 Industrial sodium chloride should meet the requirements of Table 1: Table 1 Requirements: Na2SO4 (Na2O3) (mass fraction: Na2SO4; NaOH) (mass fraction: sodium hydroxide; Na,CO3) (mass fraction: weight of water insoluble matter) Note: (1) The total mass fraction of solid high quality sodium hydroxide + sodium thiocyanate + water + methyl ketone shall not exceed 2. (5) For the oxidized product, when the circulating temperature is lower than 30°C, the oxidized mass fraction can be determined by negotiation between the supply and demand parties. The qualified product
GH19306—2003
4 Test method
4.1 Indications
The oxidized mass fraction of the product shall be strictly followed in the sampling and analysis operations in accordance with the safety requirements of this standard. The waste water after analysis shall be treated as shown in Appendix 1. The monohydrate, alkali and other corrosive test materials used in the analysis shall be used with caution to avoid contact with the skin. If contact with the skin is detected, rinse immediately with plenty of water. In severe cases, seek medical treatment in time. 4.2-1 Provisions
The formula water used in this standard, when other requirements are not specified, refers to the first-class water specified in G-2.
The standard solvents, preparations and products used in the test shall be prepared in accordance with HG/13696.1 and H/356.3 when other requirements are not specified.
4.3 Determination of sodium cyanide
4.3.1 Silver nitrate method (silver nitrate method)
4. 3. 1. 1 Method specification
In a suitable medium, silver ions react with sodium cyanide to form a complex. Excess silver ions react with sodium cyanide to form an anti-precipitate, indicating the titration point. The content of cyanide is calculated by the disappearance of the standard titration solution of sodium cyanide. 4.3.1.2 Reagents and materials
4.3.1.2.1 Hydrogen nitrate solution; 24-3;
4.3.1.2.2 Standard sodium cyanide solution: r4eNO, about 0.5mri/T4. 3. 1. 2. 3 Potassium cyanide: 50 g/L-t4.3.1.2.4 Water for deacidification:
4.3.1.3 Preparation of acid solution
Take about 2g of solid sample or 8g of concentrated sample accurately to the nearest l, weigh it with water to remove the carbon dioxide, and use the water to remove the carbon dioxide to measure the concentration. This ratio is relatively good for the test solution A, and is determined by the content of sodium chloride, the total amount of sodium hydroxide and the content of sodium phosphate. 4.3.1.4 Analysis step
Take 25mL of test solution A, shake it in a 250ml standard bottle, add 75ml of water, 1ml of nitrogen solution and 1ml of potassium hydroxide solution, and titrate it with the acid-eliminating standard filtration solution in the titration chamber to see the end point: 4.3. 1.5 Calculation of results
The mass fraction of sodium nitrate in sodium carbonate is expressed in %, and is calculated using the formula: (V12002100
m(25/5(0)
Wherein;
V--the value of the volume weight of the nitric acid standard titration solution 1.3.1.2.2), in liters (m2); the exact value of the energy reduction of the silver standard titration, in mal; m--the value of the mass of the sample, in grams (g); M--the value of the mass of sodium nitrate NaCN>, in grams per unit (R/mn) (M9. The average of the results of the repeated determinations should be taken as the determination result, and the absolute difference between the results of the parallel determinations should not exceed 0.3%. 4.3.7 Confirmatory acid method
4. 3.2.1 Method Summary
In this process, the ions and ammonium ions are separated to form a precipitate in the form of a colored precipitate, indicating the titration endpoint: the content of the nitrate is calculated based on the consumption of the acid dye and the conversion coefficient of the acid standard solution and the concentration of the silver nitrate standard titration solution.
4.3.2.2 Reagents
4 .3.2.2.1 Hydrogenated water solution: 2Fh
4.3.2.2.2 Reading temperature: 50g/T
5.3.2.2.3 Standard silver hydroxide solution: c(AgN,) about 25a101/L: 4.3.2.2.4 Tincture titration solution:
GB193062003
Prepare and weigh 7.27g nitric acid NiNO, 6.6HO refined to 0.1mN, uniformly titrate the nitric acid solution against the standard titration tower to obtain the conversion coefficient: use a pipette to transfer 251mL test solution A, add 75mL water and 5-8 drops of dinitrogen aqueous solution. Titrate with a cotton wool until the concentration is high yellow and a faint red precipitate appears under constant stirring; then take 251.1g test solution A with a pipette, mix it with 75mL water, 1mL rehydration solution, and titrate with silver nitrate standard solution until the mixing point is just reached. Use a micro-titer to titrate against silver nitrate standard solution. The conversion coefficient (K) is calculated according to the following formula (2): K -
V)——Nitric acid solution The volume of the solution (4.3.1.2.2) multiplied by (4.2.2.4) is expressed in liters (aL). The volume of the solution (4.3.1.2.2) of the standard titration of molten silver is expressed in liters (mL). The result is expressed as a decimal point. The average value of the three parallel determinations is used as the potential coefficient (K). The error of three strict determinations shall not exceed 0.02ml:
4.3.2.2.5" Nitrogen aqueous solution: 32/[.: 4.3.2.3 Analysis step
Pipette 25mL of the test solution A, place it in a hot water bath, add 75mL of water and 6-~% dibutyl ether, and titrate with nitric acid to complete the determination. When the solution becomes yellow, the end point is the bright yellow precipitate. 4.3.2.4. Expression of analysis results
The mass fraction of sodium oxide (NaCN) content is expressed in % and is calculated using the following formula (3): 220k10010.0Vek
n(25/50));
The volume of the sample carrier (4.3.2..4) in milliliters (mL) is converted into the accurate value of the concentration of the standard titration solution in units of mol/l:!
The uncertainty of the conversion coefficient of the ion determination solution to the standard titration solution of nitric acid: K-
The mass of the material, unit: g:
The numerical value of the mass of sodium nitrate (NaCN)> is g/ml (g/ml-08). The arithmetic mean of the results of the parallel determinations is taken as the determination result. The absolute difference of the half-measured results shall not be greater than (%, %. 4.4 Determination of sodium hydride
4.4.1 Method As needed
Use nitric acid to obtain sodium ions, precipitate carbonate ions with tert-butyl hydride, replace it with an indicator, and titrate with a standard titration solution.
4.4.2 Reagents
4.4.2.1 Chloride: 100 g/L:
4.4.2.2 Standard titration solution:The fraction of the sample is expressed in % and is calculated using the following formula (\): V-0cJM×109_a12.0(-Ve
mt25/500)
Wherein:
V-the volume of the hydrochloric acid standard solution (4.5.2.1>), in milliliters (mL); V:-the volume of the hydrochloric acid standard solution consumed in 4.4.4, in liters (ml);
V-the exact value of the concentration of the hydrochloric acid standard solution, in mole per year (mol/l);
V-the mass of the sample, in grams per gram of carbonic acid (NaClO2) (M=1U6.0). The arithmetic mean of the results of the parallel determinations is the absolute value before the results of the parallel determinations are reported. The difference between superior products and qualified products is not more than 0.05%, and that between standard products and qualified products is not more than 0.1%.
4.6 Determination of moisture content
4.6. Instruments and equipment
4.6.1.1 Volumetric flask, 45mm×25mm
4.6.1.2 Electric constant temperature dryer, capable of controlling the temperature between 05℃--110℃. 4.6.2 Analysis steps
GB19306-2003
Use a pre-controlled weighing bottle to take 100g of solid test sample, adjust the concentration to 0.3%, place in an electric heating thermostat, open the heat, burn at 105~120℃ for 2.5h, pour out, and place in a dryer, measure for 30min, and drop to 0.0032. 4.6. 3 Results Calculation
The mass fraction of water is expressed as given. Calculate using the following formula (5): ws=m×100
The mass of the weighing bottle and the sample before combustion, in grams () + The effective value of the mass of the weighing bottle and the sample after combustion, in grams (the mass of the sample is replaced by the digit of the mass of the sample, in grams (). Take the average of the results of the parallel determination stations as the determination result. The absolute difference of the results of the half-row determination is not greater than .1, which is 4.7. Determination of insoluble matter
4.7. 1 Reagents
4.7.1.1 Silver nitrate solution: 0R/1..
4.7.2 Instruments and equipment
4.7.2.1 Glass frit: pore size 5um--15μmR4.7.2.2 Electric heating constant temperature drying oven: control the temperature and pressure at 105℃:--110℃, 4.7.3 Analysis steps
Weigh about 100% solid sample in a weighing bottle, saturate to 0.1% in a beaker, add 1C~1S~60% hot water, dry the glass frit at 105℃--10℃ until it is straight, wash with hot water to make sure it does not contain the required ions (use acid to check). Move the glass frit together with the solid matter into the electric heating oven, and burn at 105℃--119℃ until constant temperature: 4.7. 4 Results The mass fraction of water-insoluble matter was taken out, and the value was expressed as 5. It was calculated according to the following formula (7, x 100
in Wuzhong:
glass sand is the mass fraction of the water-insoluble matter, in grams (g)! : The mass fraction of glass sand is the mass fraction of the water-insoluble matter, in grams (g) Fm The mass fraction of the sample is expressed as gram (g). (
Take the arithmetic mean of the parallel determination results as the determination result. The absolute value of the determination result is not more than 331 for superior products, and not more than 0.1% for first-class products and qualified products.
4. Determination of sodium formaldehyde
4.1 Principle of the method
Silver ions and formic acid ions form a sodium formate precipitate to eliminate the formic acid ions. Under natural conditions, formic acid reacts with formic acid. The formic acid produced in the reaction reacts with potassium hydroxide under energy conditions. The sodium formate is reacted with thiosulfate to generate sodium formate. The iodine method is used to determine the amount of sodium formate. The reaction formula is as follows: AR + CN -AGN +
GR19306—2003
4.8.2 Reagents
4. 8.2. Potassium hydroxide 1
2Mn-HA-1 3O--2Mn-+C- +21I.
MrO- +4I -3II--Mn-+2I.+4Ha0
2Mr0: -- [0 I- 1 16 H---2Mr-- +-I. +[I. 1+250--50-:21
4.8.2.2 Hydroxide solution, 1c5 g/1.1 sulphuric acid quotient: 11S;
silver nitrate bath solution: 4/L
permanganese acid standard solution: c(1/5KMmh about 0.1ml/E;A.8.2.6 thiosulfate standard solution: 4.(Na:90:) about 0.1mnl/T.4.8.2.7 powder index g/1.
4.8.3 Preparation of test solution B
Take about S solid sample, accurate to .UO2g. Dissolve it in water and transfer it all to a 10mL flask, dilute it with water until it becomes uniform, this solution is the test solution. Determine the content with formic acid clamps, 4,8.4 Analytical step
Use a pipette to collect 50ml. The test solution will be B, 2501ml. Dimensional flask 1ml of sodium hydroxide solution was added, and the acid solution was added dropwise while adding until the standard precipitate was observed. Filtered with a quick-release qualitative filter paper, washed with water until the precipitate was not degradable, collected in a 25m2 diiodine bottle, 2:1 = mI of hydrogen peroxide solution, accurately added 425 l of high-yield acid standard solution + water, heated to room temperature, and cooled to room temperature. After 2 minutes of incubation, add water and place for 5 minutes. Use sodium sulfide standard solution to determine the end point. Add 2 ml of indicator solution, and the blue color of the sieved solution disappears as the integer. At the same time, perform the test. 2.8.5 Calculate the fraction of formic acid dissolved in the solution. The value is expressed in %. The following formula is used for calculation: L- 00le4 × Ju0 - 54. GY-Vicm(30/500)bzxZ.net
Shishi;
..-( )
—the value of the mass of the sodium thiosulfate standard titration solution (1.H.2.6) in the air test, expressed in m1). V-the value of the volumetric mass of the sodium thiosulfate standard titration solution (4.5.2.6) in the test. It is an estimate of the concentration of the standard titration solution of sodium thiosulfate (mol/l). It is expressed in coulombs (mol/l). C
—the mass of the sample, unit (
M-the value of the coulomb mass of sodium carboxylate (/2HOONa), unit (g/mnl>(M·34.) The average value of the parallel determination results is taken as the determination result. The absolute value of the parallel determination results shall not be greater than 0.1%. 5.1 This standard adopts type inspection and standard inspection. 5.1.1 Type inspection: All index items in the requirements are type inspection items. Under normal circumstances, water sources should be type inspected at least once every three months, and the total impurities should be inspected at least once a week. 5.1.2 Regular inspection, sodium cyanide content, sodium oxychloride content, sodium aldehyde content, and water content are routine inspection items and should be inspected batch by batch. 5.2 Each batch of solid sodium cyanide products shall not exceed 60 tons, and each batch of sodium cyanide solution shall not exceed 200 tons. 5.3 The number of sampling units of solid sodium cyanide shall be determined according to the provisions of /75678. When sampling, the sampler shall sample from the top of the packaging barrel to 3/4 of the depth of the material layer. When sampling the flaky and flaky products, remove the material layer of about 15cm on the upper layer of the package and take out samples of not less than 50% from each selected package. After the samples are evenly mixed, they are divided into not less than 1008 by quartering. The sodium oxide solution is sampled according to the provisions of GB/T6680. The sample is sampled from the discharge port of the tank truck. The sampling volume is not less than 1DCmL. The sample is divided into two clean and dry plastic bottles or wide-mouth bottles with inspection marks, sealed, and the bottles are labeled with: manufacturer name, product name, grade batch number, sampling date and name of the sampler. One bottle is used as the experimental sample and the other is kept for reference. The storage period of sodium oxide samples is more than 15d, and the storage period of sodium oxide flotation samples is one week. 5.4 Industrial sodium oxide should be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The production inspection ensures that each batch of products leaving the factory meets the requirements of this standard.
5.5 The user has the right to inspect and accept the industrial sodium chloride products received in accordance with the provisions of this standard. The solid sodium chloride shall be inspected and accepted within 15 days from the date of receipt. The sodium chloride solution concentration shall be based on the delivery inspection. 5.6 If any index does not meet the requirements of this standard, the sample from the twice-packed package shall be tested. If only one index does not meet the requirements of this standard, the whole batch of products shall be unqualified. 5.7 The amplitude comparison method specified in GH/T1250 shall be used to determine whether the test results meet the standard. 6 Marking and labeling
6.1 The solid sodium cyanide in industrial sodium cyanide shall have a clear mark on the package, including: manufacturer name, address, product name, trademark, grade, net content, batch number, production date, abbreviation of this standard, 1. The solid sodium cyanide shall have a "highly toxic product" mark in accordance with the provisions of GB19J, production license number, E, 2. Each batch of industrial sodium cyanide leaving the factory shall be accompanied by a quality certificate. The content includes: manufacturer name, address, product name, trademark, grade, net content, batch number or production date, proof that the product meets the requirements of this standard, abbreviation of this standard, safety technical instructions and safety labels. 7 Packaging, transportation and storage
7.1 Industrial sodium fluoride should be stored in special steel containers. Industrial sodium fluoride solution should be transported by special vehicles. The packaging of industrial solid chemical products is recommended to comply with GR19268-2003% sodium fluoride packaging 3. The net content of each container (cut) is 25kg, 40kg, 50kg, 7kg, 380kg, 1000kg.
7.2: Industrial solid chemical packaging, the inner is sealed with vinyl or other equivalent quality steel or other equivalent methods 7.3 The production, use and transportation of industrial sodium cyanide shall be handled in accordance with the provisions of the Regulations on the Safety Management of Hazardous Chemicals of the People's Republic of China and the Regulations on Railway Freight Transportation of the Ministry of Railways of the People's Republic of China. 7.4 Industrial sodium cyanide shall be stored in a dedicated room, and the chlorinated liquid shall be stored in a dedicated car to avoid contact or interaction with acids, nitrates and nitrites. 5 The storage chain, tank car, valves and cracks of the sodium cyanide bottle shall be regularly checked to prevent dripping. 8 Safety 8.1 In order to avoid direct contact with the cyanide, the operator shall be equipped with necessary protective equipment. 2 In order to avoid inhaling the gas containing the element, protective equipment shall be worn when necessary. 3 The production and use of sodium cyanide sites shall comply with the relevant provisions of TJ36-1979. Day.4: Workers in production workshops, laboratories and sampling stations are not allowed to wear any wounds, and work can only be carried out when there are more than 2 people. Day.5 Work progress is not allowed in production workshops and laboratories where there is sodium fluoride. Smoking is not allowed. Washing and changing clothes are required after work. Day.6 For units without cyanide wastewater treatment measures, the wastewater should be collected in a special group after the test and can only be discharged after it meets the standards. The treatment method is shown in the appendix. CB19305—2003 (Information Appendix) Treatment of Wastewater in Taiwan In order to prevent the contamination of fluoride-containing liquid, the fluoride-containing liquid analyzed every day should be treated to be drainable: A1 Method Summary In alkaline medium, oxidize the ions to decompose into unchanged carbon dioxide with the oxidation test as the oxidation test. 2 Treatment Steps Place the fluoride in an instrument at about 30 °C until the concentration of the liquid is greater than 8. Check with test paper. Place in a ventilated room, cover with an appropriate amount, stir thoroughly, and place for 1 hour to drain after reaching the standard. The drugs used in the above operation are 1. Industrial grade.
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