Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2202—91
Prometryn Wettable Powder
Issued on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
WChemical Industry Standard of the People's Republic of China
Prometryn Wettable Powder
1 Subject Content and Scope of Application
HG2202—91
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for 40% and 25% Prometryn Wettable Powders.
This standard applies to Prometryn Wettable Powders made from Prometryn technical material, fillers and adjuvants. Active ingredient: Promethazine
Chemical name: 4,6-diisopropylamino-2-methylthio-s-triazine Structural formula:
Molecular formula: CioHigN,S
CH(CH3）2
NH -CH(CH．)2
Relative molecular mass: 241.36 (according to the international relative atomic mass in 1987) 2 Reference standards
GB1601
GB1605
GB3796
GB5451
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 HG2-896 Method for determination of fineness of pesticide powders 3 Technical requirements
3.1 Appearance: Loose powder without visible foreign impurities. 3.2 Promethazine wettable powder should meet the requirements of the following table. Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991 and implemented on July 1, 1992
W/.bzsoso.cOm Item
Promethazine content, %(m/m)
Fineness (through 38um (325 mesh)), %(m/m)Wetting time, s
Suspension rate, %(m/m)
Hot storage stability1)
Note: 1) is a type inspection item.
4 Test method
4.1. Determination of promethazine content (arbitration method) 4.1.1 Summary of the method
HG2202-91
The sample was dissolved in chloroform, triadimefon was used as the internal standard, and 3% polyethylene glycol 20000/GaschromQ was used as the filling material of the chromatographic column to separate and quantify promethazine. 4.1.2 Reagents and solutions
Chloroform (GB682),
Polyethylene glycol 20000 gas chromatography stationary liquid; GaschromQ: 150~180um (80~100 days), gas chromatography carrier internal standard solution: 20g/L triadimefon chloroform solution; promethazine standard sample: known content, >99.0% (m/m); triadimefon: content ≥95% m/m). There were no impurities interfering with the analysis. 4.1.3 Instruments
Gas chromatograph: with flame ionization detector, chromatographic column: 1.8~2.0m long, 4mm inner diameter, stainless steel column filled with 3% polyethylene glycol 20000/GaschromQ (150~180um);
Carrier gas: nitrogen, nitrogen content greater than 99.99%, try to filter out oxygen and water in it, 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 polyethylene glycol 20000 in a 100mL beaker, add about 45mL chloroform (just enough to immerse the carrier). Stir to completely dissolve. Pour 15.0g of the weighed carrier into the beaker at once, place the beaker in a water bath at about 60℃, and shake the beaker gently from time to time to mix it evenly. When the solvent evaporates and is almost dry, place the beaker in a 100℃ oven and dry it for 1h. 4.1.4.1.2 Filling of the chromatographic column
Connect a small funnel to the inlet of the cleaned chromatographic column, wrap the outlet with gauze, and connect it to the vacuum pump with a rubber tube. Turn on the vacuum pump, pour the column filler in batches from the funnel, and tap the column wall continuously to make the filler fill the chromatographic column tightly and evenly, then insert a small ball of glass wool at each end of the column and press it appropriately. 4.1.4.1.3 Aging of the chromatographic column
Connect the inlet of the chromatographic column to the vaporization chamber, and do not connect the outlet to the detector for the time being. Raise the temperature to 210℃ in stages at a carrier gas flow rate of about 20mL/min, and age it at this temperature for at least 24h. 2
W.4.1.4.2 Gas chromatograph operating conditions
Temperature:
Column chamber 200±5℃;
Vaporization chamber 230℃;
Detector 230℃.
Gas flow rate:
Carrier gas 80mL/min
Hydrogen 40mL/min,
Air 400mL/min.
Injection volume:
Retention time:
Promethazine 13min;
Triadimefon 18min.
HG2202—91
The above gas chromatograph 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.
Gas chromatogram of promethazine
1—promethazine; 2—triadimefon
4.1.4.3 Preparation of standard solution and sample solution 3
W.4.1.4.3.1 Standard solution
HG2202—91
Weigh 0.10g of promethazine standard sample, accurate to 0.0001g, into a small glass bottle with a lid, add 5.0mL of internal standard solution with a pipette, and shake well.
4.1.4.3.2 Sample solution
Weigh the sample containing about 0.10g of promethazine, accurate to 0.0001g, into a small glass bottle with a lid, add 5.0mL of internal standard solution with a pipette, shake well, let 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 promethazine standard solution until the relative deviation of the peak height ratio (or peak area ratio) of promethazine to the internal standard in two consecutive injections is less than 0.6%. Then inject and analyze in the following order: 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, and d, calculate the average values of the peak height ratio (or peak area ratio) of promethazine to the internal standard in a, d and b, c, respectively.
The mass percentage content of promethazine (X) is calculated according to formula (1): X
f2·m1
Wherein: i——the average value of the peak height ratio (or peak area ratio) of promethazine and internal standard substance in the sample solution injected twice in b and c; the average value of the peak height ratio (or peak area ratio) of promethazine and internal standard substance in the standard solution injected twice in a and d; 2
The mass of the sample, g;
The mass of the standard sample,;
P—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 should not be greater than 1.0%. 4.2 Determination of pH value
The pH meter method in GB1601 is used.
4.3 Determination of wetting time
The method in GB5451 is used.
4.4 Determination of fineness
According to the HG2-896 medium wet sieving method.
4.5 Determination of suspension rate
4.5.1 Summary of the method
Use standard hard water to prepare a suspension of known concentration in a measuring cylinder. Under the specified conditions, determine the content of promethazine in the bottom 1/10 suspension and sediment, and calculate its suspension rate. 4.5.2 Solution
Standard hard water: 342ppm. Prepared according to the method in GB5451; internal standard solution:
Solution A (for 40% wettable powder): 20g/L triadimefon chloroform solution; Solution B (for 25% wettable powder): 12g/L triadimefon chloroform solution. 4
W.4.5.3 Apparatus
HG2202-91
Measuring cylinder with stopper: 250mL, the distance between 0~250mL scale should be 20.0~21.5cm, the distance between 250mL scale and the bottom of the stopper should be 4~6cm,
Glass pipette: about 40cm long, the diameter of the hole at one end is 2~3mm, and the other end of the pipette is connected to the exhaust source; Constant temperature water bath: 30±1℃;
4.5.4 Determination steps
Weigh 1.0g of sample, accurate to 0.0001g, slowly put it into a 200mL beaker containing 50mL standard hard water (30±1℃), shake the beaker in a circular motion for 2min, 120 times per minute. Place the beaker in a 30±1℃ water bath for 13min, transfer the sample quantitatively to a 250mL stoppered measuring cylinder with 30±1℃ standard hard water, dilute to the scale, and cover with a stopper. Invert the measuring cylinder 30 times within 1min, and then place it vertically in a constant temperature water bath without vibration and direct sunlight. After placing it for 30min, use a glass pipette to suck out 9/10 of the suspension on the upper part of the measuring cylinder within 10-15s. When extracting liquid, the pipette should be attached to the wall of the cylinder, and 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 draw 1/10 (25mL) of the residue 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 and evaporate to dryness. Weigh 0.20g (for 40% wettable powder) or 0.12g (for 25% wettable powder) of the promethazine standard sample, accurate to 0.0001g, into a stoppered glass bottle, and use a pipette to transfer 10.0mL of the corresponding internal standard solution (liquid A or solution B) into the standard sample vial and the residue beaker respectively. Determine according to 4.1.4.3 and 4.1.4.4. 4.5.5 Calculation
First calculate the mass of promethazine contained in 1/10 of the residue according to formula (2), and then calculate the suspension rate of promethazine (X2) according to formula (3): ms=
m-mx111.1
Wherein: m4——the mass of promethazine in the sample used to prepare the suspension, g; m3
—the mass of promethazine in 1/10 of the residue + 8; 111.1——conversion coefficient.
4.5.6 Allowable error
The difference between the results of two parallel determinations of this method should not exceed 5%. 4.6 Thermal storage stability
4.6.1 Apparatus
Beaker: 250mL, inner diameter 6~6.5cm,
Metal ball: coated with plastic, diameter slightly smaller than the inner diameter of the beaker, weight to produce a pressure of 2450Pa on the bottom surface; Oven: 54±2℃;
Dryer: without desiccant.
4.6.2 Operating steps
(2)
(3)
Weigh 20g of sample into the beaker and spread it into a smooth and uniform layer of equal thickness without using pressure. Gently place the metal ball on the surface of the sample in the beaker. Place the beaker in an oven at 54±2℃ for 14 days. Take out the beaker, remove the ball, and place it in a dryer to cool to room temperature. Conduct the test within 24 hours according to the methods specified in Articles 4.1.4.3 and 4.4 of this standard. If the results meet the requirements of this standard, the hot storage stability of the sample is qualified.
Ww.bzsoso：com5 Inspection rules
HG2202—91
5.1 Promethazine wettable powder shall be inspected by the quality supervision and inspection department of the manufacturer according to this standard. The manufacturer shall ensure that all Promethazine wettable powders shipped out of the factory meet the requirements of this standard. 5.2 The user has the right to inspect whether the quality of the Promethazine wettable powder received 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 the sampling method for wettable powders in 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, samples should be taken from twice the amount of packages for re-testing. If only one indicator does not meet the requirements of this standard, the whole batch of Promethazine WP is considered an unqualified product. 5.5 When there is a dispute between the supply and demand parties over quality, it 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 The marking and packaging of Promethazine WP shall comply with the relevant provisions of GB3796. 6.2 During storage and transportation, it should be strictly protected from moisture and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds and feed, and should avoid contact with the skin and prevent inhalation through the mouth and nose.
6.3 Under normal storage and transportation conditions, the Promethazine content should meet the requirements of this standard within two years from the date of leaving the factory. 6
W.bzsoso.cOmA1Method summary
HG2202—91
Appendix A
Gas chromatography determination method for promethazine content
(Supplement)
The sample was dissolved in dimethylformamide, di-n-pentyl phthalate was used as the internal standard, and the chromatographic column was filled with 5%XE-60/ChromosorbWAWDMCS to separate and quantify promethazine. Reagents and instruments
Dimethylformamide (Liao Q988-84)
Internal standard solution: 24g/dipentyl phthalate dimethylformamide solution; Promethazine standard sample: known content, >99.0% (m/m); internal standard: dipentyl phthalate, content 99%, no interference 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/chromosorbWAWDMCS150~180um filling material;
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:
Promethazine 5.5min,
Di-n-pentyl phthalate 9.5min.
The above gas chromatography 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
HG2202—91
Figure A1 Gas chromatogram of promethazine
1—promethazine; 2—di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the upper clear solution for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples are injected and analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard sample solution.
A6 Calculation
The mass percentage of promethazine (X3) is calculated according to formula (A1): 8
W.bzsoso,cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p—the purity of the standard, %(m/m).
Allowable difference
The difference between the results of two parallel determinations in this method should not be greater than 1.0%. Additional remarks:
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 technical supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry. Jilin Chemical Industry Company Pesticide Factory participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)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 Pesticide Factory of Jilin Chemical Industry Company participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)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 Pesticide Factory of Jilin Chemical Industry Company participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)12g (for 25% wettable powder) of promethazine standard sample, accurate to 0.0001g, is placed in a stoppered glass bottle. Use a pipette to transfer 10.0mL of the corresponding internal standard solution (solution A or solution B) to the standard sample bottle and the residue beaker respectively. Determine according to 4.1.4.3 and 4.1.4.4. 4.5.5 Calculation
First calculate the mass of promethazine in 1/10 of the residue according to formula (2), and then calculate the suspension rate of promethazine (X2) according to formula (3): ms=
m-mx111.1
Where: m4——the mass of promethazine in the sample used to prepare the suspension, g; m3
—the mass of promethazine in 1/10 of the residue + 8; 111.1——conversion factor.
4.5.6 Allowable error
The difference between the results of two parallel determinations of this method should not exceed 5%. 4.6 Thermal storage stability
4.6.1 Apparatus
Beaker: 250mL, inner diameter 6~6.5cm,
Metal ball: coated with plastic, diameter slightly smaller than the inner diameter of the beaker, weight to produce a pressure of 2450Pa on the bottom surface; Oven: 54±2℃;
Dryer: without desiccant.
4.6.2 Operating steps
(2)
(3)
Weigh 20g of sample into the beaker and spread it into a smooth and uniform layer of equal thickness without using pressure. Gently place the metal ball on the surface of the sample in the beaker. Place the beaker in an oven at 54±2℃ for 14 days. Take out the beaker, remove the ball, and place it in a dryer to cool to room temperature. Conduct the test within 24 hours according to the methods specified in Articles 4.1.4.3 and 4.4 of this standard. If the results meet the requirements of this standard, the hot storage stability of the sample is qualified.
Ww.bzsoso：com5 Inspection rules
HG2202—91
5.1 Promethazine wettable powder shall be inspected by the quality supervision and inspection department of the manufacturer according to this standard. The manufacturer shall ensure that all Promethazine wettable powders shipped out of the factory meet the requirements of this standard. 5.2 The user has the right to inspect whether the quality of the Promethazine wettable powder received 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 the sampling method for wettable powders in 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, samples should be taken from twice the amount of packages for re-testing. If only one indicator does not meet the requirements of this standard, the whole batch of Promethazine WP is considered an unqualified product. 5.5 When there is a dispute between the supply and demand parties over quality, it 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 The marking and packaging of Promethazine WP shall comply with the relevant provisions of GB3796. 6.2 During storage and transportation, it should be strictly protected from moisture and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds and feed, and should avoid contact with the skin and prevent inhalation through the mouth and nose.
6.3 Under normal storage and transportation conditions, the Promethazine content should meet the requirements of this standard within two years from the date of leaving the factory. 6
W.bzsoso.cOmA1Method summary
HG2202—91
Appendix A
Gas chromatography determination method for promethazine content
(Supplement)
The sample was dissolved in dimethylformamide, di-n-pentyl phthalate was used as the internal standard, and the chromatographic column was filled with 5%XE-60/ChromosorbWAWDMCS to separate and quantify promethazine. Reagents and instruments
Dimethylformamide (Liao Q988-84)
Internal standard solution: 24g/dipentyl phthalate dimethylformamide solution; Promethazine standard sample: known content, >99.0% (m/m); internal standard: dipentyl phthalate, content 99%, no interference 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/chromosorbWAWDMCS150~180um filling material;
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:
Promethazine 5.5min,
Di-n-pentyl phthalate 9.5min.
The above gas chromatography 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
HG2202—91
Figure A1 Gas chromatogram of promethazine
1—promethazine; 2—di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the upper clear solution for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples are injected and analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard sample solution.
A6 Calculation
The mass percentage of promethazine (X3) is calculated according to formula (A1): 8
W.bzsoso,cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p—the purity of the standard, %(m/m).
Allowable difference
The difference between the results of two parallel determinations in this method should not be greater than 1.0%. Additional remarks:
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 technical supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry. Jilin Chemical Industry Company Pesticide Factory participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)12g (for 25% wettable powder) of promethazine standard sample, accurate to 0.0001g, is placed in a stoppered glass bottle. Use a pipette to transfer 10.0mL of the corresponding internal standard solution (solution A or solution B) to the standard sample bottle and the residue beaker respectively. Determine according to 4.1.4.3 and 4.1.4.4. 4.5.5 Calculation
First calculate the mass of promethazine in 1/10 of the residue according to formula (2), and then calculate the suspension rate of promethazine (X2) according to formula (3): ms=
m-mx111.1
Where: m4——the mass of promethazine in the sample used to prepare the suspension, g; m3
—the mass of promethazine in 1/10 of the residue + 8; 111.1——conversion factor.
4.5.6 Allowable error
The difference between the results of two parallel determinations of this method should not exceed 5%. 4.6 Thermal storage stability
4.6.1 Apparatus
Beaker: 250mL, inner diameter 6~6.5cm,
Metal ball: coated with plastic, diameter slightly smaller than the inner diameter of the beaker, weight to produce a pressure of 2450Pa on the bottom surface; Oven: 54±2℃;
Desiccant: without desiccant.
4.6.2 Operating steps
(2)
(3)
Weigh 20g of sample into the beaker and spread it into a smooth and uniform layer of equal thickness without using pressure. Gently place the metal ball on the surface of the sample in the beaker. Place the beaker in an oven at 54±2℃ for 14 days. Take out the beaker, remove the ball, and place it in a desiccator to cool to room temperature. Conduct the test within 24 hours according to the methods specified in Articles 4.1.4.3 and 4.4 of this standard. If the results meet the requirements of this standard, the hot storage stability of the sample is qualified.
Ww.bzsoso：com5 Inspection rules
HG2202—91
5.1 Promethazine wettable powder shall be inspected by the quality supervision and inspection department of the manufacturer according to this standard. The manufacturer shall ensure that all Promethazine wettable powders shipped out of the factory meet the requirements of this standard. 5.2 The user has the right to inspect whether the quality of the Promethazine wettable powder received 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 the sampling method for wettable powders in 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, samples should be taken from twice the amount of packages for re-testing. If only one indicator does not meet the requirements of this standard, the whole batch of Promethazine WP is considered an unqualified product. 5.5 When there is a dispute between the supply and demand parties over quality, it 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 The marking and packaging of Promethazine WP shall comply with the relevant provisions of GB3796. 6.2 During storage and transportation, it should be strictly protected from moisture and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds and feed, and should avoid contact with the skin and prevent inhalation through the mouth and nose.
6.3 Under normal storage and transportation conditions, the Promethazine content should meet the requirements of this standard within two years from the date of leaving the factory. 6
W.bzsoso.cOmA1Method summary
HG2202—91
Appendix A
Gas chromatography determination method for promethazine content
(Supplement)
The sample was dissolved in dimethylformamide, di-n-pentyl phthalate was used as the internal standard, and the chromatographic column was filled with 5%XE-60/ChromosorbWAWDMCS to separate and quantify promethazine. Reagents and instruments
Dimethylformamide (Liao Q988-84)
Internal standard solution: 24g/dipentyl phthalate dimethylformamide solution; Promethazine standard sample: known content, >99.0% (m/m); internal standard: dipentyl phthalate, content 99%, no interference 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/chromosorbWAWDMCS150~180um filling material;
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:
Promethazine 5.5min,
Di-n-pentyl phthalate 9.5min.
The above gas chromatography 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
HG2202—91
Figure A1 Gas chromatogram of promethazine
1—promethazine; 2—di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the upper clear liquid for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples are injected and analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard sample solution.
A6 Calculation
The mass percentage of promethazine (X3) is calculated according to formula (A1): 8
W.bzsoso,cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p—the purity of the standard, %(m/m).
Allowable difference
The difference between the results of two parallel determinations in this method should not be greater than 1.0%. Additional remarks:
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 technical supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry. Jilin Chemical Industry Company Pesticide Factory participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)4. If the test result meets the requirements of this standard, the hot storage stability of the sample is qualified.
Ww.bzsoso：com5 Inspection rules
HG2202—91
5.1 Promethazine wettable powder shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with this standard. The manufacturer shall ensure that all Promethazine wettable powders shipped out of the factory meet the requirements of this standard. 5.2 The user has the right to inspect the quality of the Promethazine wettable powder received 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 the sampling method for wettable powders in 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, if any index does not meet the requirements of this standard, re-sampling shall be conducted from twice the amount of packaging. If the result of the re-inspection is that only one index does not meet the requirements of this standard, the entire batch of Promethazine WP is an unqualified product. 5.5 When the supply and demand parties have a dispute over quality, it 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 The marking and packaging of Promethazine WP shall comply with the relevant provisions of GB3796. 6.2 During storage and transportation, it should be strictly prevented from moisture and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds and feed, avoid contact with skin, and prevent inhalation through the mouth and nose.
6.3 Under normal storage and transportation conditions, the Promethazine content shall meet the requirements of this standard within two years from the date of leaving the factory. 6
W.bzsoso.cOmA1Method summary
HG2202—91
Appendix A
Gas chromatography determination method for promethazine contentwwW.bzxz.Net
(Supplement)
The sample was dissolved in dimethylformamide, di-n-pentyl phthalate was used as the internal standard, and the chromatographic column was filled with 5%XE-60/ChromosorbWAWDMCS to separate and quantify promethazine. Reagents and instruments
Dimethylformamide (Liao Q988-84)
Internal standard solution: 24g/dipentyl phthalate dimethylformamide solution; Promethazine standard sample: known content, >99.0% (m/m); internal standard: dipentyl phthalate, content 99%, no interference 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/chromosorbWAWDMCS150~180um filling material;
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:
Promethazine 5.5min,
Di-n-pentyl phthalate 9.5min.
The above gas chromatography 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
HG2202—91
Figure A1 Gas chromatogram of promethazine
1—promethazine; 2—di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the upper clear solution for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples are injected and analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard sample solution.
A6 Calculation
The mass percentage of promethazine (X3) is calculated according to formula (A1): 8
W.bzsoso,cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p—the purity of the standard, %(m/m).
Allowable difference
The difference between the results of two parallel determinations in this method should not be greater than 1.0%. Additional remarks:
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 technical supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry. Jilin Chemical Industry Company Pesticide Factory participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)4. If the test result meets the requirements of this standard, the hot storage stability of the sample is qualified.
Ww.bzsoso：com5 Inspection rules
HG2202—91
5.1 Promethazine wettable powder shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with this standard. The manufacturer shall ensure that all Promethazine wettable powders shipped out of the factory meet the requirements of this standard. 5.2 The user has the right to inspect the quality of the Promethazine wettable powder received 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 the sampling method for wettable powders in 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, if any index does not meet the requirements of this standard, re-sampling shall be conducted from twice the amount of packaging. If the result of the re-inspection is that only one index does not meet the requirements of this standard, the entire batch of Promethazine WP is an unqualified product. 5.5 When the supply and demand parties have a dispute over quality, it 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 The marking and packaging of Promethazine WP shall comply with the relevant provisions of GB3796. 6.2 During storage and transportation, it should be strictly prevented from moisture and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds and feed, avoid contact with skin, and prevent inhalation through the mouth and nose.
6.3 Under normal storage and transportation conditions, the Promethazine content shall meet the requirements of this standard within two years from the date of leaving the factory. 6
W.bzsoso.cOmA1Method summary
HG2202—91
Appendix A
Gas chromatography determination method for promethazine content
(Supplement)
The sample was dissolved in dimethylformamide, di-n-pentyl phthalate was used as the internal standard, and the chromatographic column was filled with 5%XE-60/ChromosorbWAWDMCS to separate and quantify promethazine. Reagents and instruments
Dimethylformamide (Liao Q988-84)
Internal standard solution: 24g/dipentyl phthalate dimethylformamide solution; Promethazine standard sample: known content, >99.0% (m/m); internal standard: dipentyl phthalate, content 99%, no interference 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/chromosorbWAWDMCS150~180um filling material;
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:
Promethazine 5.5min,
Di-n-pentyl phthalate 9.5min.
The above gas chromatography 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
HG2202—91
Figure A1 Gas chromatogram of promethazine
1—promethazine; 2—di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the upper clear solution for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples are injected and analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard sample solution.
A6 Calculation
The mass percentage of promethazine (X3) is calculated according to formula (A1): 8
W.bzsoso,cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p—the purity of the standard, %(m/m).
Allowable difference
The difference between the results of two parallel determinations in this method should not be greater than 1.0%. Additional remarks:
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 technical supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry. Jilin Chemical Industry Company Pesticide Factory participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)5min.
The above gas chromatography operating conditions are typical operating parameters. The operating parameters can be adjusted appropriately according to the characteristics of the instrument to obtain the best effect.
W.bzsoso,conA4 Preparation of standard solution and sample solution
HG2202-91
Figure A1 Gas chromatogram of promethazine
1-Promethazine; 2-di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the supernatant for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples were analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of promethazine (X3) was calculated according to formula (A1): 8
W.bzsoso, cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p——the purity of the standard, % (m/m).
Allowable error
The difference between the results of two parallel determinations of this method should not exceed 1.0%. Additional remarks:
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 Shenyang Chemical Research Institute of the Ministry of Chemical Industry. The Pesticide Factory of Jilin Chemical Industry Company participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)5min.
The above gas chromatography operating conditions are typical operating parameters. The operating parameters can be adjusted appropriately according to the characteristics of the instrument to obtain the best effect.
W.bzsoso,conA4 Preparation of standard solution and sample solution
HG2202-91
Figure A1 Gas chromatogram of promethazine
1-Promethazine; 2-di-n-pentyl phthalate Weigh the standard sample containing about 0.10g of promethazine and the mixed sample to an accuracy of 0.0001g, and place them in small glass bottles with lids. Use a pipette to add 5.0mL of internal standard solution to each bottle, shake it thoroughly, and let it stand. Take the upper clear liquid for sampling and filter it if necessary. A5 Determination steps
Under the selected conditions, after the instrument is stable, repeat the injection of the standard solution until the relative deviation of the peak height ratio of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then, the samples were analyzed in the following order: a. Standard solution;
b. Sample solution,
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of promethazine (X3) was calculated according to formula (A1): 8
W.bzsoso, cOnHG2202—91
13·m2·P
Wherein: r3——the average value of the peak height ratio of promethazine to the internal standard of the sample solution injected twice in b and c; i——the average value of the peak height ratio of promethazine to the internal standard of the standard solution injected twice in a and d; m1——the mass of the sample, g;
m2——the mass of the standard, g,
p——the purity of the standard, % (m/m).
Allowable error
The difference between the results of two parallel determinations of this method should not exceed 1.0%. Additional remarks:
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 Shenyang Chemical Research Institute of the Ministry of Chemical Industry. The Pesticide Factory of Jilin Chemical Industry Company participated in the drafting. The main drafters of this standard are Wu Qi, Wang Yufan, Zhang Xuebing, Wang Shiyan, Wang Fengqin, and Zheng Taiyong. (A1)
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