Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2216-91
Atrazine Technical
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
Chemical Industry Standard of the People's Republic of China
Atrazine Technical
HG2216-91
This standard adopts the United Nations Food and Agriculture Organization (UNFAO) standard FAO91/1/S/6 "Atrazine Technical". Subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for atrazine technical. This standard applies to atrazine technical.
Active ingredient: HuCIN
Chemical name: 2-chloro-4-ethylamino-6-isolactone-1,3,5-triazine Structural formula:
(CHs)2CH-NH
Molecular formula: C.HuCIN
NH-C2H5
Relative molecular mass: 215.69 (according to the international relative atomic mass in 1987) 2 Reference standards
GB601 Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents GB1605 Sampling method for commercial pesticides
6 General rules for pesticide packaging
GB3796
3 Technical requirements
3.1 Appearance: white to light yellow powder, without visible foreign matter. 3.2 The technical requirements of atrazine shall also be met: % (m/m)
Atrazine content
Heating loss
Sodium chloride content
4 Test method
4.1 Determination of atrazine content (arbitration method)>
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991 as superior product
Qualified product
Implemented on July 1, 1992
4.1.1 Summary of method
HG2216-91
The sample was dissolved in chloroform and atrazine was separated and determined on a 3% polyethylene glycol 20000/GasChromQ chromatographic column with triadimefon as the internal standard.
4.1.2 Reagents and solutions
Chloroform (GB682);
Polyethylene glycol 20000: stationary phase for gas chromatography; GasChromQ: 150~180μm (80~100 mesh), carrier for gas chromatography; Internal standard solution: 20g/L triadimefon chloroform solution; Aminoquine standard: known content, ≥99% (m/m); Triadimefon: content greater than 95% (m/m), no interferences after gas chromatography analysis. 4.1.3 Instruments
Gas chromatograph: with flame ionization detector Column: 1.8~2.0m long, 4mm inner diameter stainless steel column; Carrier gas: nitrogen, nitrogen content greater than 99.99%, try to filter out oxygen and water; Micro-injector: 10uL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
4.1.4.1.1 Coating of stationary liquid
Weigh 0.45g of polyethylene glycol 20000 in a 100mL beaker, add about 45mL of chloroform (it is best if the solvent just immerses the carrier), and stir to dissolve it completely. Weigh 15.0g of the carrier and pour it into the above beaker at once. Place the beaker in a water bath of about 60℃, and gently shake the beaker from time to time to mix it evenly. When the solvent evaporates to near dryness, place the beaker in a 100℃ oven and dry it for 1h. 4.1.4.1.2 Filling of chromatographic column
Connect a small funnel to the inlet of the cleaned and dried chromatographic column, and wrap the outlet with gauze and connect it to the vacuum pump. Turn on the vacuum pump, pour the column filling material from the funnel, and keep tapping the column wall gently until the filling material stops falling. Remove the chromatographic column and plug a little glass wool at both ends of the column. 4.1.4.1.3 Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporizer, and do not connect the outlet end to the detector. The carrier gas flow rate is 20mL/min, and the column temperature is increased from 100℃ to 210℃ in six times within 6h, and aged at this temperature for at least 24h. 4.1.4.2 Chromatographic operating conditions
Temperature:
Column chamber 200±5℃;
Vaporizer 230℃;
Detector 230℃.
Gas flow rate:
Carrier gas 80mL/min;
Hydrogen 40mL/min,
Air 400mL/min.
Injection volume:
Retention time:
Torazine 11min;
Triadimefon: 17min.
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. 2
4.1.4.3 Preparation of standard solution and sample solution HG221691
Gas chromatogram of torazine
1-Torazine; 2-Triadimefon
Weigh the standard sample containing 0.10g of torazine and the finely ground and mixed sample (accurate to 0.0001g), respectively, and place them in each stoppered vial, and use a pipette to transfer 5.0mL of internal standard solution into each vial. Shake the vial thoroughly and let it stand. Take the supernatant for sampling and filter if necessary. 4.1.4.4 Determination
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the desazine standard solution until the relative deviation of the peak height ratio (or peak area ratio) of desazine to triadimefon between two consecutive injections is less than 0.7%, and then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution,
d. Standard solution.
Based on the chromatograms of the four injections a, d and b, c, calculate the average values of the peak height ratios (or peak area ratios) of desazine to triadimefon a, d and b, c respectively.
The mass percentage of chloramphenicol (s) is calculated according to formula (1): 1
i·m·w
Wherein: yuan--the average value of the peak height ratio (or peak area ratio) of chloramphenicol to triadimefon in the sample solution injected twice in b and c; i2--the average value of the peak height ratio (or peak area ratio) of chloramphenicol to triadimefon in the standard solution injected twice in a and d; (1)
mi--the mass of the sample, g;
m2--the mass of the standard sample, g;
--the purity of the standard sample, % (m/m).
4.1.5 Allowable difference
HG2216-91
The difference between the results of two parallel determinations in this method shall not exceed 1.5%. 4.2 Determination of Heating Loss
4.2.1 Apparatus
Weighing bottle; height 30mm, diameter 50mm;
Oven: 105±2℃;
Dryer.
4.2.2 Determination Procedure
Weigh 2.5g of ground sample (accurate to 0.001g) and spread it flat in a weighing bottle that has been dried to constant weight. Separate the weighing bottle and the bottle cap and place them in the oven. After drying for about 2h, cover them, take them out, put them in the dryer, cool them to room temperature, and weigh them. Repeat the drying and weigh until the difference between two consecutive weighings is less than 0.01g.
4.2.3 Calculation
The heating loss (a2) expressed as a mass percentage is calculated according to formula (2): ma-m4×100
The mass of the sample and the weighing bottle before drying, g; where.ms
-The mass of the sample and the weighing bottle after drying, g; m4
m6——The mass of the weighed sample, 8.
4.3 Determination of sodium chloride content
4.3.1 Reagents and solutions
95% ethanol (GB679);
Sulfuric acid solution: about 50% (V/V);
Standard silver nitrate titration solution: c(AgNOs)=0.1mol/L, prepared and calibrated according to Article 4.2.1 of GB601; Standard hydrochloric acid solution: c(HCI)=0.1mol/L, prepared and calibrated according to Article 4.2 of GB601. 4.3.2 Instruments
Potentiometric titrator: readings accurate to 2mV;
Electrode system: silver-217 type calomel electrode with potassium nitrate salt bridge. 4.3.3 Determination steps
Weigh 0.8g of sample (accurate to 0.0001g), and transfer quantitatively to a 250mL beaker with 20mL 95% ethanol. Dilute with water to about 150mL, carefully acidify with sulfuric acid to pH 12, accurately add about 2mL of hydrochloric acid standard solution, and perform potentiometric titration with silver nitrate standard titration solution.
4.3.4 Calculation
The mass percentage of sodium chloride () is calculated according to formula (3): zs
0.0585(V1C1-V2C2)X100
5.85(V1C1-V2C2)
-The volume of the standard silver nitrate titration solution consumed during titration, mL; Where: Vi-
V2-The volume of the standard hydrochloric acid solution added to the sample solution, mL; Cr
-The actual concentration of the standard silver nitrate titration solution, mol/L;-The actual concentration of the standard hydrochloric acid solution, mol/L:. (3)
me-The mass of the sample, g;
HG2216-91
0.0585-The mass of NaCI expressed in grams equivalent to 1.00mL of the standard silver nitrate titration solution Cc(AgNOs)=1.000mol/L.
Inspection rules
5.1 The technical substance of quandejin should be inspected by the quality supervision and inspection department of the production unit. The production unit should ensure that all technical substances of quandejin leaving the factory meet the requirements of this standard.
5.2 The business unit and the user unit have the right to test whether the received quanqujin technical drug meets the requirements of this standard in accordance with the provisions of this standard.
5.3 The sampling method shall be carried out in accordance with GB1605. The sample shall be divided into two bottles, one bottle shall be sent to the quality supervision and inspection department for inspection, and the other bottle shall be sealed. 5.4 In the test results, when there are indicators that do not meet the requirements of this standard, re-sampling shall be conducted from twice the amount of packaging. In the results of the re-test, even if one indicator does not meet the requirements of this standard, the entire batch of quanqujin technical drug is an unqualified product. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation; or the statutory inspection agency shall conduct arbitration analysis according to the inspection methods specified in this standard.
6 Marking, packaging, transportation and purchase and storage
6.1 Marking and packaging shall comply with the relevant provisions of GB3796. 6.2 During transportation and storage, it should be strictly protected from moisture and sunlight, maintained in good ventilation, and should not be mixed with food, seeds, and feed, and should avoid contact with the skin and inhalation through the mouth and nose.
A1 Method Summary
HG2216—91
Appendix A
Gas chromatography determination method for cypermethrin content
(Supplement)
The sample was dissolved in dimethylformamide, and cypermethrin was used as the internal standard. Cypermethrin was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g/simethopine dimethylformamide solution; Moxifen standard sample: known content, ≥99% (m/m); Simethopine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N2)
020mL/min
Hydrogen 30mL/min;
Air 500mL/min.
Injection volume: luL.
Retention time:
Moxifen 7min;
Simetine 11min.
The above chromatographic operating conditions are typical operating parameters. The operating parameters can be appropriately adjusted according to the characteristics of the instrument to obtain the best effect. 6
A4 Preparation of standard solution and sample solution
HG2216-91
Figure A1 Gas chromatogram of dezin
1-dezin; 2-simethoine
Weigh the standard sample containing 0.08g dezin and the finely ground and mixed sample (accurate to 0.0001g), and place them in stoppered vials respectively. Use a pipette to transfer 2.0mL of internal standard solution into each vial, shake the vial thoroughly, and let it stand. Take the supernatant for injection. Filter if necessary. A5
Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the dezin standard solution until the relative deviation of the peak height ratio of dezin and simethoine in two consecutive injections is less than 0.7%. Then inject the samples in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
Standard solution.
A6 Calculate
The mass percentage of atrazine (a4) is calculated according to formula (A1): 4
ig·mzw
Wherein: i3——the average value of the peak height ratio (or peak area ratio) of atrazine to sirtuin in the sample solution injected twice in b and c; i4—the average value of the peak height ratio (or peak area ratio) of atrazine to sirtuin in the standard solution injected twice in a and d; m1——the mass of the sample;
m2——the mass of the standard, g;
w—the purity of the standard, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations of this method should not exceed 1.5% (A1)bzxZ.net
Additional instructions:
HG2216—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengqin, and Zheng Taiyong.2 During transportation and storage, it should be strictly protected from moisture and sunlight, maintained in good ventilation, and should not be mixed with food, seeds, and feed, and should avoid contact with the skin and inhalation through the mouth and nose.
A1 Method Summary
HG2216—91
Appendix A
Gas chromatography determination method for cypermethrin content
(Supplement)
The sample was dissolved in dimethylformamide, and cypermethrin was used as the internal standard. Cypermethrin was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g/simethopine dimethylformamide solution; Moxifen standard sample: known content, ≥99% (m/m); Simethopine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N2)
020mL/min
Hydrogen 30mL/min;
Air 500mL/min.
Injection volume: luL.
Retention time:
Moxifen 7min;
Simetine 11min.
The above chromatographic operating conditions are typical operating parameters. The operating parameters can be appropriately adjusted according to the characteristics of the instrument to obtain the best effect. 6
A4 Preparation of standard solution and sample solution
HG2216-91
Figure A1 Gas chromatogram of dezin
1-dezin; 2-simethoine
Weigh the standard sample containing 0.08g dezin and the finely ground and mixed sample (accurate to 0.0001g), and place them in stoppered vials respectively. Use a pipette to transfer 2.0mL of internal standard solution into each vial, shake the vial thoroughly, and let it stand. Take the supernatant for injection. Filter if necessary. A5
Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the dezin standard solution until the relative deviation of the peak height ratio of dezin and simethoine in two consecutive injections is less than 0.7%. Then inject the samples in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
Standard solution.
A6 Calculate
The mass percentage of atrazine (a4) is calculated according to formula (A1): 4
ig·mzw
Wherein: i3——the average value of the peak height ratio (or peak area ratio) of atrazine to sirtuin in the sample solution injected twice in b and c; i4—the average value of the peak height ratio (or peak area ratio) of atrazine to sirtuin in the standard solution injected twice in a and d; m1——the mass of the sample;
m2——the mass of the standard, g;
w—the purity of the standard, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations of this method should not exceed 1.5% (A1)
Additional instructions:
HG2216—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengqin, and Zheng Taiyong.2 During transportation and storage, it should be strictly protected from moisture and sunlight, maintained in good ventilation, and should not be mixed with food, seeds, and feed, and should avoid contact with the skin and inhalation through the mouth and nose.
A1 Method Summary
HG2216—91
Appendix A
Gas chromatography determination method for cypermethrin content
(Supplement)
The sample was dissolved in dimethylformamide, and cypermethrin was used as the internal standard. Cypermethrin was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g/simethopine dimethylformamide solution; Moxifen standard sample: known content, ≥99% (m/m); Simethopine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N2)
020mL/min
Hydrogen 30mL/min;
Air 500mL/min.
Injection volume: luL.
Retention time:
Moxifen 7min;
Simetine 11min.
The above chromatographic operating conditions are typical operating parameters. The operating parameters can be appropriately adjusted according to the characteristics of the instrument to obtain the best effect. 6
A4 Preparation of standard solution and sample solution
HG2216-91
Figure A1 Gas chromatogram of dezin
1-dezin; 2-simethoine
Weigh the standard sample containing 0.08g dezin and the finely ground and mixed sample (accurate to 0.0001g), and place them in stoppered vials respectively. Use a pipette to transfer 2.0mL of internal standard solution into each vial, shake the vial thoroughly, and let it stand. Take the supernatant for injection. Filter if necessary. A5
Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the dezin standard solution until the relative deviation of the peak height ratio of dezin and simethoine in two consecutive injections is less than 0.7%. Then inject the samples in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
Standard solution.
A6 Calculate
The mass percentage of atrazine (a4) is calculated according to formula (A1): 4
ig·mzw
Wherein: i3——the average value of the peak height ratio (or peak area ratio) of atrazine to sirtuin in the sample solution injected twice in b and c; i4—the average value of the peak height ratio (or peak area ratio) of atrazine to sirtuin in the standard solution injected twice in a and d; m1——the mass of the sample;
m2——the mass of the standard, g;
w—the purity of the standard, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations of this method should not exceed 1.5% (A1)
Additional instructions:
HG2216—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengqin, and Zheng Taiyong.
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