Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2204—91
Aqueous Suspension Concentrate of Dezin
Issued on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
W Chemical Industry Standard of the People's Republic of China
Aqueous Suspension Concentrate of Dezin
Subject Content and Scope of Application
HG2204—91
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for 38% aqueous suspension concentrate of dezin.
This standard applies to aqueous suspension concentrate of dezin made from dezin technical material, fillers and adjuvants. Active ingredient: Coupon
Chemical name: 2-chloro-4-ethylamino-6-isopropylamino-1,3,5-triazine Structural formula:
(CHs)2CH -NH
Molecular formula: CHuCINs
Relative molecular mass: 215.69 (according to the international relative atomic mass in 1987) Reference standards
GB1601
GB1605
GB3796
GB5451
3 Technical requirements
Method for determination of hydrogen ion concentration of pesticides
Sampling method for commercial pesticides
General rules for pesticide packaging
Method for determination of wettability of pesticide wettable powders
3.1 Appearance: Flowable suspension that is easy to measure volume. Stratification is allowed after storage, but it can still be restored to its original state after being shaken by hand. No agglomeration is allowed. 3.2 The aqueous suspension of moxacarb should meet the following requirements. Item
Moxacarb content, %(m/m)
Suspension rate, %(m/m)
Hot storage stability1)
Note: 1) is a type inspection item.
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991>
Implemented on July 1, 1992
W.bzsoso, com4 Test method
4.1 Determination of moxacarb content (arbitration method) 4.1.1 Summary of method
HG2204-91
After drying the sample to remove moisture, dissolve it in chloroform, use triadimefon as internal standard, and use 3% polyethylene glycol 20000/GaschromQ as filling material to separate and determine moxacarb. 4.1.2 Reagents and solutions
Chloroform (GB682);
Polyethylene glycol 20000 gas chromatography stationary phase; GasChromQ: 150~180um (80~100 mesh), gas chromatography carrier, internal standard solution: 20g/L triadimefon chloroform solution, chloranil standard: known content, >99% (m/m); triadimefon: content >95% (m/m), no interference after gas chromatography analysis. 4.1.3 Instruments
Gas chromatograph: with flame ionization detector; Chromatographic 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 (just enough to immerse the carrier), and stir to dissolve it completely. Weigh 15.0g of the carrier and pour it into the above beaker at one time. Put the beaker in a water bath of about 60℃ and shake the beaker gently from time to time to mix it evenly. When the solvent evaporates and is almost dry, put 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:bzxz.net
Carrier gas (N2) 80mL/minz
Hydrogen 40mL/min
Air 400mL/min.
Injection volume:
Retention time:
Rhizoctonia 11min;
Wbzsoso, cOtriazole 17min.
HG2204—91
The above gas chromatography 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.
Gas chromatogram of rhizoctonia
1—Rhizoctonia; 2
4.1.4.3 Preparation of standard solution and sample solution Triazole
Weigh the standard containing 0.10g of rhizoctonia and the well-shaken sample (accurate to 0.0001g) in a stoppered vial. Dry the sample vial in a 105℃ oven. 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. Centrifuge or filter if necessary.
4.1.4.4 Determination
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the atrazine standard solution until the relative deviation of the peak height ratio (or peak area ratio) of atrazine to triadimefon in two adjacent injections is less than 0.7%. Then inject in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard solution.
4.1.4.5 Calculation
Based on the chromatograms of the four injections a, b, c, calculate the average values of the peak height ratio (or peak area ratio) of atrazine to triadimefon in a, d and b, c respectively.
Ww.bzsoso：comHG2204—91
The mass percentage of chloranil (a) is calculated according to formula (1): Tr.m2-w
T2·m1
Wherein: ii——the average value of the peak height ratio (or peak area ratio) of chloranil 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 chloranil to triadimefon in the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard sample, g
w——the purity of the standard sample, %(m/m).
4.1.5 Allowable difference
The difference between the results of two parallel determinations in this method shall not exceed 1.0%. 4.2 Determination of suspension rate
4.2.1 Method summary
Weigh 1g of sample and prepare a suspension in a measuring cylinder with standard hard water. Under specified conditions, measure the amount of dezin in the bottom 1/10 suspension and precipitate and calculate the suspension rate.
4.2.2 Solution
Standard hard water: 342ppm, prepared according to the method in GB5451. Internal standard solution: 15g/L triadimefon chloroform solution. 4.2.3 Apparatus
Constant temperature water bath: 30±1℃
Graduated cylinder: with ground stopper, the distance between 0~250mL scale line is 20~21.5cm, and the distance between 250mL scale line and the bottom of the stopper is 4~6cm; Glass pipette: about 40cm long, 5mm inner diameter, with a 2~3mm hole at the tip, and the other end connected to the suction source. Measure 100mL of standard hard water into a 250mL graduated cylinder, and place the graduated cylinder in a water bath at 30±1℃. Weigh a sample containing 0.4g of chlorpheniramine (accurate to 0.0001g) in a 50mL beaker, transfer the sample quantitatively to the above-mentioned measuring cylinder with standard hard water (30±1℃), and dilute to 250mL. Insert the stopper, turn the measuring cylinder upside down 30 times at a speed of once every two seconds, and place it vertically in a water bath. The water surface should reach the neck of the measuring cylinder to prevent vibration. Keep it for 30 minutes. Then, draw out 9/10 of the suspension in the upper part of the measuring cylinder. When drawing liquid, the tip of the pipette should be kept a few millimeters below the liquid surface to minimize the agitation of the suspension. Use a long pipette to suck 1/10 of the residue in the measuring cylinder into a 50mL beaker, rinse the bottom of the measuring cylinder with 15mL of water three times (avoid washing the sticky materials on the upper wall of the measuring cylinder), and transfer them to the beaker. Place the beaker in a 100℃ water bath to evaporate to dryness. Weigh 0.07g of amantadine standard sample (accurate to 0.0001g) into a stoppered vial. Pipette 5.0mL of internal standard solution is placed in the standard sample vial and the residue beaker, and the determination is carried out according to 4.1.4.3 and 4.1.4.4. 4.2.5 Calculation
First calculate the mass of 1/10 residue containing chloramphenicol according to formula (2), and then calculate the suspension rate (α2) of chloramphenicol water suspension according to formula (3).
ji·m2·w
m-m3×111.1
: (2)
W.HG2204—91
Wherein: m3——the mass of chloramphenicol in 1/10 residue, m4——the mass of chloramphenicol in the sample weighed for preparing suspension, g; 111.1——conversion coefficient;
11, 72, w are the same as formula (1).
4.2.6 Allowable error
The difference between the results of two parallel determinations of this method should not be greater than 2%. 4.3 Determination of pH value
Weigh 0.5g of sample and add 50mL of water. The rest is carried out according to the pH meter method in GB1601. 4.4 Thermal storage stability
4.4.1 Apparatus
Oven: 54±2℃;
An: capacity is 50mL, neck length is about 5mm.
4.4.2 Operating steps
Pull about 30mL of sample into the annulus, and do not let the sample touch the neck of the annulus. Heat the neck of the annulus to melt and seal it. Place it in an oven at 54±2℃ and store for 14d. Then take out the annulus and cool it naturally to room temperature. Within 24h, measure according to 4.1, 4.2, and 4.3. If the test results and appearance meet the technical requirements of this standard, the heat storage stability of the sample is qualified. 5 Inspection rules
5.1 The quality supervision and inspection department of the production unit shall inspect the water suspension concentrate of the desulphuric acid. The production unit shall ensure that all the water suspension concentrates of the desulphuric acid that leave the factory meet the requirements of this standard. 5.2 The operating unit and the user unit have the right to inspect whether the water suspension concentrates of the desulphuric acid received meet 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 inspection results, when there are indicators that do not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. In the results of the re-inspection, if even one indicator does not meet the requirements of this standard, the entire batch of water suspension concentrates of the desulphuric acid is an unqualified product. 5.5 When a dispute arises between the supply and demand parties over product quality, it can be resolved through negotiation between the two parties, or by a legal inspection agency that conducts arbitration analysis in accordance with the inspection methods specified in this standard.
5.6 Under normal circumstances, the inspection cycle for type inspection items shall not exceed one quarter. 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 protected from sunlight, and should not be mixed with food, seeds and feed, and should avoid contact with the skin and inhalation through the mouth and nose. 6.3 The warranty period for this product is 2 years. That is, under normal packaging and storage conditions, all indicators should meet the technical requirements of this standard within two years from the date of leaving the factory.
WA1 Method Summary
HG2204—91
Appendix A
Gas chromatography determination method for amantadine content
(Supplement)
The sample was dissolved in dimethylformamide, and simetropium was used as the internal standard. Amantadine was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS chromatographic column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 66g/L simetholine dimethylformamide solution; Phenylthiocyanate standard sample: known content, >99% (m/m); simethoine: 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) 20mL/min;
Hydrogen 30mL/min;
Air 500mL/min.
Injection volume:
luL.
Retention time:
Trazine 7min;
Simethicone 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.
W.bzsoso, cOnA4 Preparation of standard solution and sample solution
HG2204-91
Figure A1 Gas chromatogram of quinoline
1-quinoline; 2-sicazoline
Weigh the standard sample containing about 0.08g of quinoline and the well-shaken sample (accurate to 0.0001g), and place them in stoppered vials respectively. Place the test vials in an oven at 105℃ to dry, 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 sampling and filter if necessary.
A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the quinoline standard solution until the relative deviation of the peak height ratio of quinoline and sicazoline in two consecutive injections is less than 0.7%. Then, inject the standard solution in the following order;
b. Sample solution,
c. Sample solution,
d. Standard solution.
A6 Calculation
The mass percentage of quinolones (a4) is calculated according to formula (A1):_13·m2·w
Wherein: 3——the average value of the peak height ratio of quinolones to quinolones in the sample solution injected twice in b and c; i4——the average value of the peak height ratio of quinolones to quinolones in the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
w——the purity of the standard, % (m/m).
W.A7
Allowable difference
HG2204—91
The difference between the results of two parallel determinations in this method should not exceed 1.0%. Additional Notes:
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision 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.4 In the test results, when there are indicators that do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. In the re-test results, even if one indicator does not meet the requirements of this standard, the entire batch of Motujin aqueous suspension is an unqualified product. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation between the two parties, or the statutory inspection agency can conduct arbitration analysis according to the inspection methods specified in this standard.
5.6 Under normal circumstances, the inspection cycle of type inspection items shall not exceed one quarter. 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 protected from sunlight, not mixed with food, seeds and feed, avoid contact with skin, and prevent inhalation through the mouth and nose. 6.3 The warranty period of this product is 2 years. That is, under normal packaging and storage conditions, all indicators should meet the technical requirements of this standard within two years from the date of leaving the factory.
WA1 Method Summary
HG2204—91
Appendix A
Gas chromatography determination method for amantadine content
(Supplement)
The sample was dissolved in dimethylformamide, and simetropium was used as the internal standard. Amantadine was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS chromatographic column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 66g/L simetholine dimethylformamide solution; Phenylthiocyanate standard sample: known content, >99% (m/m); simethoine: 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) 20mL/min;
Hydrogen 30mL/min;
Air 500mL/min.
Injection volume:
luL.
Retention time:
Trazine 7min;
Simethicone 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.
W.bzsoso, cOnA4 Preparation of standard solution and sample solution
HG2204-91
Figure A1 Gas chromatogram of quinoline
1-quinoline; 2-sicazoline
Weigh the standard sample containing about 0.08g of quinoline and the well-shaken sample (accurate to 0.0001g), and place them in stoppered vials respectively. Place the test vials in an oven at 105℃ to dry, 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 sampling and filter if necessary.
A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the quinoline standard solution until the relative deviation of the peak height ratio of quinoline and sicazoline in two consecutive injections is less than 0.7%. Then, inject the standard solution in the following order;
b. Sample solution,
c. Sample solution,
d. Standard solution.
A6 Calculation
The mass percentage of quinolones (a4) is calculated according to formula (A1):_13·m2·w
Wherein: 3——the average value of the peak height ratio of quinolones to quinolones in the sample solution injected twice in b and c; i4——the average value of the peak height ratio of quinolones to quinolones in the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
w——the purity of the standard, % (m/m).
W.A7
Allowable difference
HG2204—91
The difference between the results of two parallel determinations in this method should not exceed 1.0%. Additional Notes:
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision 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.4 In the test results, when there are indicators that do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. In the re-test results, even if one indicator does not meet the requirements of this standard, the entire batch of Motujin aqueous suspension is an unqualified product. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation between the two parties, or the statutory inspection agency can conduct arbitration analysis according to the inspection methods specified in this standard.
5.6 Under normal circumstances, the inspection cycle of type inspection items shall not exceed one quarter. 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 protected from sunlight, not mixed with food, seeds and feed, avoid contact with skin, and prevent inhalation through the mouth and nose. 6.3 The warranty period of this product is 2 years. That is, under normal packaging and storage conditions, all indicators should meet the technical requirements of this standard within two years from the date of leaving the factory.
WA1 Method Summary
HG2204—91
Appendix A
Gas chromatography determination method for amantadine content
(Supplement)
The sample was dissolved in dimethylformamide, and simetropium was used as the internal standard. Amantadine was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS chromatographic column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 66g/L simetholine dimethylformamide solution; Phenylthiocyanate standard sample: known content, >99% (m/m); simethoine: 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) 20mL/min;
Hydrogen 30mL/min;
Air 500mL/min.
Injection volume:
luL.
Retention time:
Trazine 7min;
Simethicone 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.
W.bzsoso, cOnA4 Preparation of standard solution and sample solution
HG2204-91
Figure A1 Gas chromatogram of quinoline
1-quinoline; 2-sicazoline
Weigh the standard sample containing about 0.08g of quinoline and the well-shaken sample (accurate to 0.0001g), and place them in stoppered vials respectively. Place the test vials in an oven at 105℃ to dry, 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 sampling and filter if necessary.
A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the quinoline standard solution until the relative deviation of the peak height ratio of quinoline and sicazoline in two consecutive injections is less than 0.7%. Then, inject the standard solution in the following order;
b. Sample solution,
c. Sample solution,
d. Standard solution.
A6 Calculation
The mass percentage of quinolones (a4) is calculated according to formula (A1):_13·m2·w
Wherein: 3——the average value of the peak height ratio of quinolones to quinolones in the sample solution injected twice in b and c; i4——the average value of the peak height ratio of quinolones to quinolones in the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard sample, g,
w——the purity of the standard sample, % (m/m).
W.A7
Allowable difference
HG2204—91
The difference between the results of two parallel determinations in this method should not be greater than 1.0%. Additional Notes:
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision 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.0%. Additional remarks:
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision 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.0%. Additional remarks:
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision 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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