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Chemical Industry Standard of the People's Republic of China
HG2459-93
10% Glyphosate Aqueous Solution
Published on July 5, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1994
Chemical Industry Standard of the People's Republic of Chinabzxz.net
10% Glyphosate Aqueous Solution
Subject Content and Scope of Application
HG2459-93
This standard specifies the technical requirements, test methods, inspection rules and product marking, packaging, transportation and storage requirements for 10% Glyphosate Aqueous Solution.
This standard applies to 10% Glyphosate Aqueous Solution prepared from Glyphosate Technical Material and water. Active ingredient: Glyphosate
Chemical name; N-phosphinocarboxymethylglycine
Structural formula:
Molecular formula: C.HaNO&P
-CHNHCH
Relative molecular mass: 169.07 (according to the international relative atomic mass in 1989) 2 Reference standards
GB601 Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents GB/T1601 Determination of hydrogen ion concentration of pesticides GB1604
GB1605
GB3796
3 Technical requirements
3.1 Appearance
Pesticide acceptance rules
Commercial pesticide sampling method
General rules for pesticide packaging
Light yellow to brown liquid. When precipitation occurs, place it in a constant temperature water bath at 30±2℃ for 2h, and fully shake it every 0.5h. It is qualified when the precipitation disappears.
3.2 Glyphosate aqueous solution shall meet the following index requirements: Item
N(phosphonomethyl)glycine content, %
Dilution stability (20 times)\
Low temperature stability\
Hot storage stability\》
Note: 1) Test at least once a quarter.
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993 1.0
Implemented on January 1, 1994
4 Test method
HG2459—93
Unless otherwise specified, the reagents used in this test are analytically pure reagents, and the water shall meet the third-grade water specifications in GB6682. 4.1 Determination of glyphosate content
4.1.1 High performance liquid chromatography (arbitration method) 4.1.1.1 Summary of the method
The sample is dissolved in the mobile phase, and the sample is separated and determined using a strong anion exchange column and a UV detector. 4.1.1.2 Reagents
Methanol (GB183): (re-distilled) or high-grade pure; water, double distilled water;
Potassium dihydrogen phosphate: analytical grade;
85% phosphoric acid (GB1282);
Glyphosate standard sample: known content, dried at 105℃ for 2h before weighing. 4.1.1.3 Instruments
Liquid chromatograph: with adjustable wavelength UV detector; Chromatographic column: 25cm long, 4.6mm inner diameter stainless steel column, filled with PartisilSAX10um (or equivalent strong anion exchange resin);
Recorder: 5mV (or digital microprocessor); Micro-syringe: 25uL,
pH meter.
4.1.1.4 Chromatographic operating conditions
Column temperature, ambient temperature;
Flow rate: 1.0mL/min;
Detection wavelength: 195nm;
Detector sensitivity: 0.10AUFS;
Injection volume: 20.0uL;
Retention time: about 7.6min for glyphosate;
Guard column: PartisilSAX10um, 5cm long. The above chromatographic conditions are typical operating conditions. According to the characteristics of the instrument, the analyst can make appropriate adjustments to obtain the best results. 2
4.1.1.5 Operation steps
4.1.1.5.1 Preparation of mobile phase
HG2459-93
Figure 1 Liquid chromatogram of glyphosate
Weigh 0.730.74g potassium dihydrogen phosphate into a 1000mL volumetric flask, add appropriate amount of water to dissolve it completely, then add 160mL methanol, dilute with water to the scale, mix, and adjust the pH to 1.9 with 85% phosphoric acid. Filter and degas the mobile phase before use. 4.1.1.5.2 Preparation of standard solution
Weigh 0.1g (accurate to 0.2mg) of glyphosate standard into a 50mL volumetric flask, dissolve and dilute to the scale with mobile phase, and shake well. 4.1.1.5.3 Preparation of sample solution
Weigh about 0.1g (accurate to 0.2mg) of aqueous sample containing glyphosate into a 50mL volumetric flask, dilute to scale with mobile phase, and shake well. 4.1.1.5.4 Determination
Under the chromatographic conditions of 4.1.1.4, after the instrument is stable, first inject several needles of standard solution until the difference between the peak height or peak area of two adjacent needles is less than 1.5%, and then inject and analyze in the following order: standard solution, sample solution, sample solution, standard solution. 4.1.1.5.5 Calculation of the mass percentage of glyphosate in the sample X1 is calculated according to formula (1): hamw
-the average value of the peak height or peak area of glyphosate in the same standard solution measured by two injections; where:
W2-the average value of the peak height or peak area of glyphosate in the same sample solution measured by two injections; mi-
-the sample weight of glyphosate standard, g;
-the sample weight of glyphosate aqueous solution, g;
the mass percentage of glyphosate in the standard sample (for example: 99). 4.1.1.6 Allowable difference
The relative difference between the results of two parallel determinations shall not exceed 2%. (1)
4.1.2 Nitrosation UV spectrophotometry
4.1.2.1 Method Summary
HG2459-93
The sample reacts with sodium nitrite in an acidic solution to generate nitrosoglyphosate. The absorbance of the compound is measured at a wavelength of 243 nm, and the glyphosate content in the sample is calculated. 4.1.2.2 Reagents and solutions
Sulfuric acid (GB625): 1+1 solution;
Potassium bromide (GB649): 250g/L solution; Sodium nitrite (GB633): 6.9g/L solution, prepared and used immediately; Glyphosate standard: known purity, dried at 105℃ for 2h before weighing. 4.1.2.3 Instruments
UV spectrophotometer;
Quartz cuvette: 1cm.
4.1.2.4 Drawing of standard curve.
a. Preparation of standard solution
Weigh 0.1g (accurate to 0.2mg) of glyphosate standard into a 250mL volumetric flask, dissolve it with distilled water and dilute to the mark, shake well. b. Nitrosation reaction
Use a pipette to draw 2.0, 4.0, 6.0, 8.0, and 10.0mL of the above standard solution into 5 100mL brown volumetric flasks, add 30mL of distilled water, 2mL of sulfuric acid solution, and 1mL of potassium bromide solution to each, mix them, add 2.0mL of sodium nitrite solution with a pipette, immediately plug the bottle, shake well, let it stand at room temperature (room temperature not less than 15℃) for 30min, dilute to the mark with distilled water, and shake well. Perform a reagent blank test under the same conditions. c.
Absorbance determination
After the instrument is stable, use a 1 cm quartz cuvette at a wavelength of 243 nm and use the reagent blank solution as a reference to determine the absorbance of the above solutions.
Standard curve drawing
Draw a standard curve with glyphosate concentration p (ug/mL) as the horizontal axis and absorbance as the vertical axis. 4.1.2.5 Operation steps
a. Solution preparation
Weigh an aqueous sample containing about 0.1 g (accurate to 0.2 mg) of glyphosate into a 250 mL volumetric flask, dilute to the scale with distilled water, and shake well.
b. Nitrosation reaction and absorbance determination. Pipette 5.0mL of the above solution into a 100mL brown volumetric flask, perform nitrosation reaction according to the operating steps in 4.1.2.4.b, and determine its absorbance A1 according to 4.1.2.4.c. c. Determination of absorbance of sample solution (unnitrosated). Pipette 5.0mL of the sample solution in 4.1.2.5.a into a 100mL volumetric flask, dilute to the scale with distilled water, and shake well. Using distilled water as a reference, determine its absorbance A2 using a 1cm quartz colorimetric III at a wavelength of 243nm. The absorbance A of nitroso glyphosate in the sample solution = A1-A2. Check the glyphosate concentration p (ug/mL) corresponding to the absorbance A from the standard curve.
d. Calculation of results
The mass percentage X2 of glyphosate in the glyphosate aqueous solution sample is calculated according to formula (2): X:=PX100X250Xm2—
m×5X×10%
Wherein: p is the glyphosate concentration obtained from the standard curve, ug/mLm—the weight of the glyphosate sample, g;
-200m2m
HG2459—93
w is the mass percentage of glyphosate in the standard sample (for example: 99). 4.1.2.6 Allowable difference
The relative difference of the results of the two parallel determinations shall not exceed 1.5%. 4.2 Determination of pH value
The sample shall be determined without dilution according to the pH meter method in GB/T1601. 4.3 Dilution stability test
4.3.1 Reagents and instruments
Standard hard water: 342mg/L;
Measuring cylinder: 100mL;
Constant temperature water bath: 30±1℃.
4.3.2 Test steps
Pipette 5mL of the sample and place it in a 100mL measuring cylinder. Dilute it to the mark with standard hard water and mix it. Place the dilution in a 30±1℃ water bath and let it stand for 1h. If the dilution is uniform and there is no precipitate, it is qualified. 4.4 Hot storage stability
4.4.1 Instruments
Constant temperature box: temperature control accuracy is 54±2℃; ampoule: capacity is about 20~50mL, neck length is about 5cm. 4.4.2 Operation steps
Put 20g of sample in a clean ampoule and seal it with fire to avoid water evaporation when sealing. After weighing, store it in a 54±2℃ thermostat for 14 days, take it out and cool it to room temperature and weigh it. Take the sample whose weight has not changed to determine its content and calculate the decomposition rate. The relative decomposition rate after hot storage is less than 5% to be qualified. 4.5 Low temperature stability determination
Take 100mL of sample in a 250mL conical flask, cover it, and place it in a 0±1℃ thermostat for 7 days. Take it out without crystallization and precipitation to be qualified. If there is precipitation, place it at room temperature for 24 hours and shake it thoroughly. If the precipitation is completely dissolved, it is also qualified. 5 Inspection rules
5.1 Glyphosate aqueous solution should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that the glyphosate aqueous solution shipped from the factory meets the requirements of this standard, and each batch of products shipped from the factory should be accompanied by a quality certificate. 5.2 The user has the right to inspect the quality of the received glyphosate aqueous solution in accordance with the provisions of this standard to see if it meets the requirements of this standard. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 When there is a quality dispute between the supply and demand parties over the product quality, the arbitration unit may conduct arbitration analysis in accordance with the test methods specified in this standard. 6 Packaging, marking, transportation and purchase and storage
6.1 The marking and packaging of glyphosate aqueous solution shall comply with the relevant provisions of GB3796 and be labeled. 6.2 Glyphosate aqueous solution is packaged in clean glass bottles or plastic bottles with inner and outer covers, with a net weight of 0.5kg or 1kg per bottle, and is padded with straw sleeves or corrugated paper. Other forms of packaging may also be used according to user requirements. Each box and each bottle shall be marked with: manufacturer name, product name, batch number, production date, trademark, this standard number and usage instructions, and marked with transportation marks such as "fragile" and "not inverted". 6.3 During storage and transportation, it must be strictly protected from moisture, heat, and sunlight, and good ventilation must be maintained. It must not be mixed with food, seeds, and feed. 6.4 Under normal storage and transportation conditions, the various indicators of this product should meet the requirements of the standard within 2 years. 5
Additional instructions:
HG2459-93
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Pesticide Testing Institute of the Ministry of Agriculture. The main drafters of this standard are Ye Jiming, Liu Shaoren, Zhang Baizhen, Jiang Shuxiu, and Yang Shaozong.
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