Some standard content:
Record number: 2770-1999
HG/T3585-1999
This industry standard is in accordance with the domestic enterprise standard. Before
This standard has the following differences compared with the existing enterprise standard: 1 The standard is changed to liquid sodium borohydride;
According to the production situation and user requirements, the product quality is divided into two models on the basis of the existing enterprise standard: the sampling volume in the determination of sodium borohydride content is appropriately adjusted, and the preparation of the test solution is added; 3
The inspection rules, marking, packaging, transportation and storage of the product are adjusted; 5 Safety requirements are added.
This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China, and this standard is under the jurisdiction of the inorganic product standardization technical unit of the Ministry of Chemical Industry. The main drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Shanghai Shenyu Pharmaceutical Chemical Co., Ltd. The main drafters of this standard are: Lu Siwei, Zhang Zushao, Teng Shaoyun, Li Wenhao. This standard is entrusted to the inorganic salt product standardization technical unit of the Ministry of Chemical Industry for interpretation. 1075
Chemical Industry Standard of the People's Republic of China
Liquid sodium borohydride
Liquid sodium borohydride
HG/T 3585-—1999
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of sodium borohydride. This standard applies to sodium borohydride produced from sodium hydride and methyl borate. The product is mainly used as a reducing agent for the manufacture of potassium borohydride and for the pharmaceutical industry, pesticides, spices and other fine chemical products. It can also be used for paper bleaching, mercury-containing wastewater treatment and precious metal recovery.
Molecular formula: NaBH4
Relative molecular mass: 37.85 (according to the 1995 international relative atomic mass) 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard was published, the versions shown were all valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest version of the following standards. GB 190—1990
GB 191--1990
GB 325—1991
Dangerous goods packaging markings
Packaging storage and transportation pictorial markings
200L closed steel drums
GB/T 601-19881
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagentsGB/T 603—1988
GB/T 1250--1989
GB/T 66781986
GB/T 6680—1986
GB/T 6682--1992
3 Requirements
Preparation of preparations and products used in chemical reagent test methods (negIS () 6353-1:1982) Methods for expressing and determining limit values General rules for sampling of chemical products
General rules for sampling of liquid chemical products
Specifications and test methods for water used in analytical laboratories (eqvISO3699:1987) 3.1 Appearance: colorless or light yellow liquid.
3.2 Liquid sodium borohydride shall meet the requirements of Table 1. Table 1 Requirements
Content of sodium borohydride (NaBH.)
4 Test methods
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999 1076
Implementation on April 1, 2000
HG/T 3585—1999
Standard titration solutions, preparations and products used in the test shall be prepared in accordance with the provisions of GB/T601 and GB/T603 unless otherwise specified.
Safety Tips: When using strong alkalis and strong acids during the test operation of this standard, caution must be exercised. When using volatile strong acids, the test should be carried out in a fume hood.
4.1 Determination of Sodium Borohydride Content
4.1.1 Summary of the Method
The sample reacts with a quantitatively added potassium iodate standard solution, and the excess potassium iodate reacts with potassium iodide in an acidic medium to precipitate iodine, which is titrated with a sodium thiosulfate standard titration solution. 4.1.2 Reagents and materials
Potassium iodide:bzxz.net
4. 1. 2. 1
4.1.2.2 Sodium hydroxide solution: 0.5mol/l.; 4.1.2.3 Sulfuric acid solution: 1+8:
4.1.2.4 Potassium iodate standard titration solution: c(KI0.) is approximately 0.1mol/L; 4.1.2.5 Sodium thiosulfate standard titration solution: c(Na2S.O) is approximately 0.1mol/1.; 4.1.2.6 Starch indicator solution: 10g/L.
4.1.3 Analysis steps
Weigh about 3g (type I) or 1g (type II) of the sample (accurate to 0.0002g), quickly place it in a 250mL beaker (pre-add 100ml of sodium hydroxide solution to the beaker) to dissolve, transfer it to a 250ml volumetric flask, dilute it to the mark with sodium hydroxide solution, and shake it well. Use a pipette to transfer 25ml of the solution, inject it into a 250ml iodine volumetric flask, and then use a pipette to transfer 50ml of potassium iodate standard titration solution, shake it for 30s, add 5g of potassium iodide and 10ml of sulfuric acid solution, and shake it well. Seal the bottle mouth with water, place it in a dark place for 15min, titrate it with sodium thiosulfate standard titration solution, add 3ml of starch indicator solution when it is close to the end point, and continue titrating until the blue color of the solution disappears. Perform a blank test at the same time. 4.1.4 Expression of analytical results
The sodium borohydride (NaBH) content (X,) expressed as mass percentage is calculated according to formula (1): Xi = (Vi V)c× 0. 004 729 ×25
m×250
× 100 4. 729(Vi-V)c
Wherein: V——the volume of sodium thiosulfate standard titration solution consumed by the titration test solution, mL; V. the volume of sodium thiosulfate standard titration solution consumed by the titration empty solution, mL; -- the actual concentration of sodium thiosulfate standard titration solution, mol/Lm…-the mass of the sample, g;
0.004729-the mass of sodium borohydride in grams equivalent to 1.00mL of sodium thiosulfate standard titration solution [c(NazS2O)=1.000mol/L].
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 0.3%. 4.2 Determination of alkalinity
4.2.1 Method summary
Dissolve the sample in water, use methyl red as the indicator solution, and titrate with sulfuric acid standard titration solution. Determine the alkalinity of the product based on the consumption of sulfuric acid standard titration solution.
4.2.2 Reagents and materials
4.2.2.1 Standard sulfuric acid titration solution: c(HzSO) is about 0.5 mol/L; 4.2.2.2 Methyl red indicator solution: 1 g/1. 4.2.3 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place in a conical flask, add 25mL of water and 5 drops of methyl red indicator, and titrate with sulfuric acid standard titration solution until red, which is the end point. At the same time, perform a blank test. 4.2.4 Expression of analysis results
The alkalinity (in terms of NaOH) (X2) expressed as mass percentage is calculated according to formula (2): X2 = VV)c× 0. 040 00× 100m
Where: V—volume of sulfuric acid standard titration solution consumed by titration test solution, ml; V. -The volume of sulfuric acid standard titration solution consumed in the titration of the blank solution, mL.; c--the actual concentration of sulfuric acid standard titration solution, mol/L; m-the mass of the sample, g;
0.04000-the mass of alkalinity (in terms of NaOH) in grams equivalent to 1.00mL sulfuric acid standard titration solution Lc (No. H, SO.) = 1.000mol/LJ.
4.2.5 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 0.3%. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 Each batch of products shall not exceed 10t.
5.3 Determine the number of sampling units in accordance with the provisions of 6.6 of GB/T6678-1986. Each barrel is a packaging unit. When sampling, from each selected packaging unit, according to GB/T6680-1986 1.5.7a, take out no less than 500mL of sample, mix the sample, reduce to 200mL, immediately put into two clean and dry small-mouth bottles with rubber stoppers, and seal. Paste labels on the bottles, indicating the manufacturer's 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. 5.4 Potassium borohydride 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 each batch of products shipped from the factory meets the requirements of this standard. 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 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 shall be unqualified. 5.5 Determine whether the test results meet the standard by the rounded value comparison method specified in 5.2 of GB/T1250-1989. 6 Marking, packaging, transportation and storage
6.1 The sodium borohydride packaging barrels should be firmly and clearly marked, including the manufacturer's name, address, product name, trademark, model, net content, batch number or production date, the number of this standard and the "corrosive product" mark specified in GB190 and the "wet-afraid" mark specified in GB191. 6.2 Each batch of sodium borohydride shipped from the factory should be accompanied by a quality certificate. The content includes the manufacturer's name, address, product name, trademark, model, net content, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 6.3 Sodium borohydride is packaged in closed steel drums, and the performance and inspection methods of the steel drums should comply with the provisions of GB325. The net weight of each barrel of this product is 200 kg.
6.4 Packaging of sodium borohydride: Fill the product into steel drums, cover the drums and seal them. 6.5 Sodium borohydride should be loaded and unloaded gently during transportation, and should be protected from impact, sun exposure and rain. It should not be mixed with acids, oxidants and other substances.
6.6 Sodium borohydride should be stored in a cool, dry and ventilated place, protected from rain, and should not be mixed with acids, oxidants and other substances. 7 Safety requirements
When sodium borohydride catches fire, use a large amount of water to extinguish the fire. Sand or dry powder fire extinguishers can also be used. 1078
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