Some standard content:
Record number: 2769-1999
HG/T3584—1999
This industry standard is mainly formulated based on domestic enterprise standards. Compared with the existing enterprise standards, this standard has the following differences:
According to the classification principle of the standard, the three levels of the existing enterprise standards are changed to two levels; 1
The sampling volume for the determination of potassium borohydride content is appropriately adjusted, and the preparation of the test solution is added; 2
The product marking, packaging, transportation and storage are adjusted; 3
Safety requirements are added.
This standard is proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the inorganic salt 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. 1071bzxz.net
Chemical Industry Standard of the People's Republic of China
Potassium borohydride
Potassium borohydride
HG/T 3584—1999
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of potassium borohydride. This standard applies to potassium borohydride produced with sodium borohydride and potassium hydroxide as raw materials. The product is mainly used as a reducing agent in the pharmaceutical industry, pesticides, spices and other fine chemical products, and can also be used for the treatment of mercury-containing wastewater. Molecular formula: KBH4
Relative molecular mass: 53.94 (according to the 1995 international relative atomic mass) 2 Reference 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 version of the following standards. GB190
GB 191 -
Marking of dangerous goods packaging
Pictographic marking of packaging, storage and transportation
GB/T 601---1988
GB/T 603 -- 1988
GB/T 1250
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagentsPreparation of preparations and products used in test methods of chemical reagents (neg1ISO6353-1:1982)-1989
GB/T6678—1986
GI3/T 6682—1992
Methods for expressing and determining limit valuesGeneral rules for sampling of chemical products
Specifications and test methods for water for analytical laboratories (egvISO3699:1987)Appearance, white crystalline powder.
Potassium borohydride shall meet the requirements of Table 1.
Table 1 Requirements
Potassium borohydride (KBH) content
4 Test method
Qualified products
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. The 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.
Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999 1072
Implemented on April 1, 2000
HG/T3584--1999
Safety Tips: Be careful when using strong alkalis and strong acids during the test operation of this standard. When using volatile strong acids, they should be carried out in a fume hood.
4.1 Determination of potassium borohydride content
4.1.1 Summary of the method
The sample reacts with a quantitatively added potassium iodate standard solution. 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
4.1.2.1 Potassium iodide;
4.1.2.2 Sodium hydroxide solution: 40g/L;4.1.2.3 Sulfuric acid solution: 1+8;
4.1.2.4 Potassium iodate standard titration solution: c(KIO,) is about 0.1mol/L;4.1.2.5 Sodium thiosulfate standard titration solution: c(Na2Sz0O) is about 0.1mol/L;4.1.2.6 Starch indicator solution: 10g/L.
4.1.3 Analysis steps
Weigh about 0.2g of sample (accurate to 0.0002g), quickly place it in a 250ml beaker (100ml of sodium hydroxide solution has been added to the beaker in advance) 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 this 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. 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 to titrate until the blue color of the solution disappears. Perform a blank test at the same time. 4.1.4 Expression of analytical results
The potassium borohydride (KBH) content (X,) expressed as mass percentage is calculated according to formula (I): - (V/-V)e×0: 0.006 742 × 100 = .742(V -V)cX, =
Wherein: V-
0.006 742
m×250
The volume of sodium thiosulfate standard titration solution consumed in the titration of the test solution, mI; The volume of sodium thiosulfate standard titration solution consumed in the titration of the blank solution, mI; The actual concentration of the sodium thiosulfate standard titration solution, mol/L; The mass of the test sample, g;
·(1)
The mass of potassium borohydride in grams equivalent to 1.00 mL of sodium thiosulfate standard titration solution [c(Na2S2O.)=1.000 mol/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 moisture
4.2.1 Summary of method
Dry the sample at (105±2)℃ to constant weight, and determine the moisture content based on the weight loss before and after drying. 4.2.2 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place it in a weighing bottle that has been constant weight, put it in an electric heater in a drying oven, heat it at (105±2℃ for 45 min, take it out and put it in a desiccator, cool it to room temperature, and weigh it. Repeat the operation until constant weight. 4.2.3 Expression of analysis results
The moisture expressed as mass fraction (X,) is calculated according to formula (2): Xz=m=mi×100
Where: mi
The mass of the sample before drying, g;
m\"The mass of the sample, g.
·(2)
4.2.4 Allowable difference
HG/T 3584—1999
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.04%. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 Each batch of products shall not exceed 1t.
5.3 Determine the number of sampling units in accordance with the provisions of 6.6 in GB/T6678--1986. Each barrel is a packaging unit. When sampling, take out no less than 10g of sample from each selected packaging unit and mix the sampled samples. Reduce it to 500g by quartering method and immediately put it into two clean and dry wide-mouth bottles with ground stoppers and seal them. Paste labels on the bottles, indicating the manufacturer name, product name, grade, 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 leaving the factory meets the requirements of this standard. If one indicator of the inspection result does not meet the requirements of this standard, re-sampling shall be carried out from twice the amount of packaging for re-inspection. Even if only one indicator of the re-inspection result 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 standards by the rounded value comparison method specified in 5.2 of GB/T1250-1989. 6 Marking, packaging, transportation, purchase and storage
6.1 Potassium borohydride packaging barrels should have firm and clear markings, including the manufacturer's name, address, product name, trademark, grade, net content, batch number or production date, this standard number and the "flammable products when in contact with water" mark specified in GB190 and the "wet-afraid" mark specified in GB191. 6.2 Each batch of potassium borohydride shipped out of the factory should be accompanied by a quality certificate. The content includes the manufacturer's name, address, product name, trademark, grade, net content, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 6.3 Potassium borohydride is packaged in three layers: the inner packaging is a kraft paper bag lined with a polyethylene plastic film bag, with a thickness of 0.08mm~~0.1mm; the outer packaging is a special sealed, fully open iron barrel packaging, the thickness of the iron barrel is 0.5mm~~0.75mm, and its performance and inspection methods should comply with the provisions of the "Dangerous Goods Transportation Regulations". The net content of each barrel of this product is 15kg. 6.4 For the packaging of potassium borohydride, the polyethylene plastic film bag is tied with vinyl rope or a rope of equivalent quality, or sealed with other equivalent methods, and the kraft paper bag is sealed with a sewing machine; put it into the iron barrel, cover the barrel lid, and seal it. 6.5 Potassium borohydride should be loaded and unloaded carefully during transportation, and should be protected from sunlight and rain. It should not be transported together with acids and other oxidants. 6.6 Potassium borohydride should be stored in a cool, ventilated and dry place, and should be protected from rain and moisture. It should not be stored together with acids and other oxidants.
7 Safety requirements
Potassium borohydride is a secondary combustible item that will burn when in contact with water. In case of fire, it can be put out with sand and dry powder fire extinguisher. 1074
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