Some standard content:
UDC 632.95
G 25
GB
National Standard of the People's Republic of China
GB 12686—90
Glyphosate original drug
Glyphosate technical | tt||Glyphomate technical
1 Subject content and scope of application
MedicineWww.bzxZ.net
GB 12686—90
This standard specifies the Technical requirements, test methods, inspection rules and product markings of Ganlin technical materials. Matters that should be paid attention to in packaging, transportation and storage are put forward.
This standard applies to glycine technical material synthesized from glycine, paraformaldehyde, and dialkyl phosphite as the main raw materials. Active ingredient: glycerin
Chemical name; N-glycine carboxymethylglycine
Structural formula:
o
HO
Public||tt| |HO
ＨH
Ｈ
N
H
Molecular formula: CHNOP
ＨH
o||tt| |OH
Relative molecular mass: 169.07 (according to 1987 international atomic weight) 2 Reference standards
GB 1605
GB3796
3 Technical requirements
Sampling method
General rules for pesticide packaging
31 Appearance: white or slightly yellow powder. 3.2 Glycolin technical material should meet the following index requirements: %
Indicator
Name
Glycolin content
Drying loss
Water-insoluble matter
Note, 1) Water-insoluble matter is a sampling item.
4 Test methods
4.1 Determination of glycerin content
41.1 Method summary
Country Technical Supervision Bureau approved superior product on 1990-12-30
95.0
1.0
0. 2
refers
standard
一Grade
93.0
1.0
0.3
Qualified product
90.0
2. 0
0. 5| | tt | Nitro derivatives. This compound has a maximum absorption peak at 243nrm and can be quantified by measuring the absorbance. 41.2 Reagents and solutions
When not specified, the reagents used are all analytically pure reagents, and the water is distilled water or water of corresponding purity. 41.2.1 Sulfuric acid solution, 50% (V/V)
4.1.2.2 Nitric acid solution: 50% (V/V)
41.2.3 Potassium bromide solution, 250g/L!
41.2.4 Sodium nitrite solution, 14 people/L↓Weigh about 0.28g sodium nitrite (accurate to 0.001g), dissolve it in 20mL water, and prepare the solution immediately before use. 4.1.2.5 Glycylin standard sample: ≥99.8%. 4.1.3 Instruments
41.3.1 UV spectrophotometer;
4.1.3.2 Quartz cuvette: 1cm
4.1.3.3 Graduated pipette: 1, 2, 5mL, 41.3.4 Volumetric flask; 100, 250mL.
4.1.4 Analysis steps
4.1.4.1 Drawing of standard curve
4.1.4.1.1 Preparation of standard solution
Weigh about 0.30g of glyphosate Standard product (accurate to 0.0002g). Place in a 200mL beaker, add 60mL of water, slowly heat to dissolve, cool to room temperature, quantitatively transfer to a 250mL volumetric flask, dilute to volume, shake well. This solution should not be used for more than 20 days. 4.1.4.1.2 Nitrosation
Accurately pipette 0.8, 1.1, 1.4, 1.7, 2.0mL of glyphosate standard solution into five 100mL volumetric flasks, and take another 100mL volumetric flask as a reagent blank.
Add 5mL distilled water, 0.5mL sulfuric acid solution, 0.1mL potassium bromide solution, and 0.5mL sodium nitrite solution to each of the above volumetric flasks. After adding the sodium nitrite solution, tighten the stopper immediately and shake thoroughly. Place 20mn. Then dilute with water to the mark, shake well, finally open the stopper and leave it for 15 minutes. Note that the nitrosylation reaction temperature cannot be lower than 15C. 4.1.4.1.3 Spectrophotometry
Turn on the power of the UV spectrophotometer, turn on the atmosphere lamp to preheat for 20 minutes, adjust the wavelength to 243nm, use the reagent blank as a reference, and use a quartz cuvette to measure the absorbance Measurement.
4.1.4.1.4 Draw the standard curve
Take the absorbance as the ordinate and the volume of the corresponding standard solution as the abscissa. Make sure that all points are connected into a straight line. 4.1.4.2 Analysis of glycerin technical material
Weigh about 0.20g sample (accurate to 0.0002g) and place it in a 200mL beaker. Add 60mL of water, slowly heat to dissolve, filter with quick filter paper while hot, rinse the filter paper carefully, transfer the filtrate to a 250㎡L volumetric flask, cool to room temperature, dilute to volume, and shake well. Accurately pipette 2.0mL of sample solution into a 100mL volumetric flask, and perform the following operations in accordance with the relevant provisions of (4.1.4.1.2~~4.1.4.1.3).
4.1.4.3 Calculation of analysis results
The glyphosate percentage (X1) is calculated according to formula (1): X1=% × 100
Ca
Formula in, c1—concentration of glycerin in the standard solution, ms/mL1—volume of the standard solution corresponding to the absorbance of the sample on the standard curve, mL2
1
Ca—test Concentration of the sample solution, mg/mL, V, - volume of the sample solution drawn, mL. GB 12686-90
4.1.4.4 Allowable difference, the difference between parallel measurement results of this method shall not be greater than 1%. Note: Wash the cuvette with nitric acid solution after use. 42 Determination of drying loss
42.1 Instrument
4.2.1.1 Weighing bottle: 50mm×30mm
42.1.2 Oven
4.2.1.3 Dryer||tt ||4.2.2 Analysis steps
Weigh about 15g of the sample (accurate to 0.0002g) into a weighing bottle with constant weight, lay it flat and put it into the oven, bake it at 105±5℃ until Constant weight.
4.2.3 Calculation of analysis results
The drying weight loss percentage (,) is calculated according to formula (2) m1me×100
X=
Class|| tt||In the formula: m1—
—the mass of the sample and weighing bottle before drying! m——the mass of the sample and the weighing bottle after drying, no m——the mass of the sample, B.
43 Determination of water-insoluble matter
4.3.1 Instruments
No. 43.1.13 glass sand core crucible
4.3.1.2 Vacuum pump.
4.3.2 Reagents and solutions
Sodium hydroxide solution: 100g/L.
43.3 Analysis steps
-2)
Weigh about 10g of the sample (accurate to 0.001g), place it in a 500mL beaker, add 200mL of water, and dissolve it with sodium hydroxide solution Mix to pH 8 to completely dissolve the glyphosate. (Heat slightly if necessary) Transfer to a No. 3 glass sand pot with constant weight and suction filter, drain it, wash it three times with 100 mL water, and drain it. Bake the glass sand at 105±5℃ until constant weight (accurate to 0.0002g). 4.3.4 Calculation of analysis results
The percentage of water-insoluble matter (.) is calculated according to formula (3): ml -m2 ×100
X, =
Class||tt ||In the formula: m1—
nt2
—the mass of the crucible and water-insoluble matter at constant weight, name;—the mass of the crucible baked to constant weight
m weigh and test Such mass g.
5 inspection rules
(3)
5.1. Glycylinum technical material should be inspected by the quality inspection department of the manufacturer. Water-insoluble matter is subject to random inspection at least once a week. The manufacturer should ensure that all glyphosate technical materials shipped from the factory meet the requirements of this standard, and each batch of glyphosate technical material shipped from the factory should be accompanied by a quality certificate. 5.2 Users have the right to inspect whether the quality of the received Glycylinum technical material meets the requirements of this standard in accordance with the provisions of this standard. 3
GB 12686—90
53 Sampling method: Follow the sampling of the original drug in GB1605. Mix the sample evenly and put it into a clean, dry, glass jar with a ground mouth. A label should be attached to the bottle, indicating: manufacturer name, product name, batch number, sampling date, and submitted to the inspection department for inspection. 5.4 If one of the indicators in the inspection results does not meet the requirements of this standard, samples must be taken from twice the packaging for inspection again. As a result of re-inspection, even if only one indicator does not meet the requirements of this standard, the entire batch of products will not be accepted. 5.5 When the supply and demand parties have objections to products that require arbitration, they can be resolved through negotiation between the two parties. Or the arbitration shall be conducted by a statutory arbitration institution in accordance with the methods stipulated in this standard.
6 Marking, packaging, transportation and storage
6.1 The marking and packaging of glyphosate technical material shall comply with the relevant regulations in GB3796. 62 Each packaged finished product should be accompanied by a quality certificate. The content includes the name of the manufacturer, product name, batch number, date of manufacture, net weight, proof that the product quality complies with this standard and the number of this standard. 6.3 During storage and transportation, moisture and sunlight should be prevented and good ventilation should be maintained. Avoid mixing with food, seeds and feed. 6.4 Within two years of storage from the date of production, the content of active ingredients shall not be lower than the indicators specified in this standard. Additional notes:
This standard is proposed by 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 Guizhou Institute of Chemical Industry. The main drafter of this standard is Lin Lijun.
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