other information
drafter:Ma Xinghua, Liu Yun, Ma Yaguang, Sun Suhua, Sha Dan
Drafting unit:Liaoning Chemical Industry Research Institute
Focal point unit:Technology of Shenyang Chemical Research Institute, Ministry of Chemical Industry
Proposing unit:Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China
Publishing department:Ministry of Chemical Industry of the People's Republic of China
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2615-94
Diphacinone sodium salt
Published on April 4, 1994
Ministry of Chemical Industry of the People's Republic of China
Implementation on October 1, 1994
Chemical Industry Standard of the People's Republic of China
Other names, structural formulas and basic physicochemical parameters of diphacinone sodium salt are as follows: Iso Common name Diphacinonesodium salt CIPAC digital code: 131
Chemical name: 2-diphenylacetyl-1,3-dione sodium salt Structural formula:
Empirical formula: C2aH16ONa
Relative molecular mass: 362.36 (according to the international relative atomic mass in 1989) Biological properties: rodenticide
Melting point: There is no obvious melting point. It changes from yellow to red when heated to 207-208℃ and turns black and carbonized at 325℃. Solubility: Soluble in alcohol, acetone, hot water, insoluble in benzene and toluene. Stability: Stable in acid and alkaline solutions. HG2615-94
The solid state is stable, in acid solution it is keto form, in alkaline solution it is enol form, both are stable organic compounds. 1 Subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of sodium diphacin products. This standard applies to sodium diphacin produced by the reaction of 1,2-diphenylacetone and dimethyl phthalate and the impurities produced in its production, which should be free of foreign impurities. 2 Reference standards
GB/T1604 Pesticide acceptance rules
GB/T1605 Commercial pesticide sampling methods
GB3796 General rules for pesticide packaging
3 Technical conditions
3.1 Appearance: This product should be light yellow or yellow powder. 3.2 Diphacinone sodium salt should meet the following index requirements: Approved by the Ministry of Chemical Industry of the People's Republic of China on April 4, 1994 and implemented on October 1, 1994
Diphacinone sodium salt content
Moisture content
4 Test method
HG2615-94
Superior product
Unless otherwise specified, the reagents used in this test are analytically pure and the water meets the third-grade water in GB/T6682. 4.1 Determination of sodium diphacin
4.1.1 Identification test
%(m/m)
Qualified products
Ultraviolet spectrophotometry. This identification test can be carried out simultaneously with the determination of sodium diphacin. The maximum absorption wavelength of the sample solution is consistent with that of the standard solution under the same conditions, which is 286.0nm. Infrared spectroscopy: Infrared scanning is carried out in the range of wavenumbers 400 to 4000cm-1. There should be no obvious difference in the infrared absorption spectra of the sample and the standard.
4.1.2 Determination of sodium diphacin
4.1.2.1 Summary of the method
The sample is dissolved in 10g/L sodium pyrophosphate solution, and the sodium diphacin is measured by ultraviolet at 286.0nm. 4.1.2.2 Reagents and solutions
10g/L sodium pyrophosphate solution;
Sodium diphacin standard: known content 98% (m/m). 4.1.2.3 Instruments
Ultraviolet spectrophotometer;
1cm quartz cell.
4.1.2.4 Determination steps
a. Preparation of standard solution
Weigh about 0.10g (accurate to 0.0001g) of sodium diphacin standard, place it in a 100mL dry beaker, add sodium pyrophosphate solution, heat it in a water bath at about 60℃ to fully dissolve it, transfer it into a 100mL volumetric flask, cool it to room temperature, and dilute it to the scale with sodium pyrophosphate solution. Solution (I) is obtained.
Use a pipette to transfer 10 mL of solution (I) into a 100 mL volumetric flask, dilute to the mark with sodium pyrophosphate solution, shake well, and obtain solution (1).
Use a pipette to transfer 5 mL of solution (I) into a 100 mL volumetric flask, dilute to the mark with sodium pyrophosphate solution, shake well, and wait for testing. b. Preparation of sample solution
Weigh the equivalent of 0.10g sodium diphacinate sample (accurate to 0.0001g) into a 250mL stoppered glass bottle, pipette 100mL sodium pyrophosphate solution into the glass bottle, heat it in a water bath (about 60℃), and shake for 10min to fully dissolve the sample, cool it to room temperature, pipette 10mL of the solution into a 100mL volumetric flask, and dilute it to the mark with sodium pyrophosphate solution; pipette 5mL of the solution from the volumetric flask into another 100mL volumetric flask, dilute it to the mark with sodium pyrophosphate solution, shake well, and wait for measurement. c. Determination
Use sodium pyrophosphate solution as reference, use a 1cm quartz cell, and measure the absorbance of the standard sample and sample solution at a wavelength of 286.0nm. 4.1.2.5 Calculation:
The mass percentage of sodium diphacinate X1 is calculated according to formula (1): Xi-
Wherein: A1——absorbance of sodium diphacinate standard solution; A2——absorbance of sodium diphacinate sample solution; m1——mass of sodium diphacinate standard, g; m2——mass of sodium diphacinate sample, g; HG261594
P——percentage of sodium diphacinate standard, (m/m). 4.1.2.6 Allowable difference
The difference between two parallel determination results should not exceed 1.2%. 4.2 Determination of moisture
4.2.1 Instrument
Oven: 100~102℃;
Weighing bottle: 45×30mm.
4.2.2 Determination
Weigh 2g of sodium diphacinate sample (accurate to 0.0001g), place in a weighing bottle that has been dried to a constant weight, dry in an oven at 100-102℃ for 1h, cool to room temperature in a desiccator, and weigh. 4.2.3 Calculation
The moisture percentage X is calculated according to formula (2):
Where: m1 is the mass of the sample and weighing bottle after drying, g; m2 is the mass of the sample and weighing bottle before drying, g; m is the mass of the sample, g.
5 Inspection rules
5.1 Sampling method
Sampling shall be carried out in accordance with the "raw powder sampling" method in GB/T1605. The sampling packages shall be determined by random method, and the final sampling volume shall be not less than 250g.
5.2 Acceptance rules
Acceptance shall be carried out in accordance with GB/T1604 standard.
6 Marking, packaging, transportation and purchase and storage
6.1 The marking and packaging of sodium diphacin shall comply with the relevant provisions of GB3796 and shall be marked. Sodium diphacin shall be packed in plastic barrels lined with plastic bags, with a net weight of 500g per barrel, and 20 barrels shall be packed in a calcium plastic box. Net weight 10kg. 6.2 The transportation of sodium diphacin shall be carried out in accordance with the Ministry of Transportation's Transportation Rules for Dangerous and Toxic Goods (No. 1218), and shall not be transported together with food. 6.3 The packages shall be stored in a ventilated and dry indoor warehouse. They shall not be stored together with food. 6.4 Safety: Once sodium diphacin or poison bait is ingested by mistake, the patient shall be sent to the hospital immediately and detoxified with the special antidote vitamin K1. 3
A1 Method Summary
HG2615-94
Appendix A
Colorimetric Determination of Sodium Diphacin Content
(Supplement)
The sodium diphacin sample is dissolved in anhydrous ethanol. Ferric chloride is used as a colorimetric agent to determine its content at a wavelength of 510nm. Reagents
Absolute ethanol;
Toluene;
20g/ferric chloride solution: weigh 2g of ferric chloride and add 20mL of hydrochloric acid, dilute to 100mL with water. Sodium diphacinate standard: content ≥98%.
A3 Instruments
Spectrophotometer:
1cm quartz cuvette.
A4 Determination
a. Drawing of standard curve
Weigh 0.125g (accurate to 0.0001g) of sodium diphacinate standard and dry it in 100mL. Beaker, dissolve with anhydrous ethanol, transfer to a 250mL volumetric flask, and dilute to the scale with anhydrous ethanol. Use a pipette to transfer 2, 4, 6, 8, 10, 12, 14, 16, 18, and 20mL of the above solution into a 50mL volumetric flask, add 2.5mL of ferric chloride solution, dilute to the scale with anhydrous ethanol, and shake well; use the blank reagent as a reference and measure the absorbance of each solution at 510nm. Use the absorbance of each solution as the vertical coordinate and the corresponding sodium diphacin as the horizontal coordinate to draw a standard curve. b. Preparation of sample solutionbzxZ.net
Weigh 0.05g of sodium diphacin sample (accurate to 0.0001g) in a 100mL dry beaker, add 50mL toluene and heat to about 50℃, stir for 35min, and filter with qualitative filter paper. Rinse the washed sample with anhydrous ethanol into the original 100mL beaker to dissolve it completely, then transfer it to a 100mL volumetric flask, dilute it to the scale with anhydrous ethanol, and shake it. Pipette 20mL of the above test solution into a 50mL volumetric flask, add 2.5mL of ferric chloride solution. The following operation is carried out according to the standard curve drawing method, measure the absorbance, and find the corresponding mass of sodium diphacin on the standard curve.
Additional notes:
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 technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Liaoning Chemical Industry Research Institute. The main drafters of this standard are Ma Xinghua, Liu Yun, Ma Yaguang, Sun Suhua, and Sha Dan. 4
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