Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2201—91
Prometryn Technical
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
Prometryn Technical
1 Subject Content and Scope of Application
HG2201—91
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements for Prometryn Technical. This standard applies to Prometryn Technical.
Active ingredient: Promethazine
Chemical name: 4,6-diisopropylamino-2-methylthio-s-triazine Structural formula:
Molecular formula: C1oH1gNeS
NH-CH(CH3)2
CH(CH3)2
Relative molecular mass: 241.36 (according to the 1987 international relative atomic mass) 2 Reference standards
GB601 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB1605 Sampling method for commercial pesticides
GB37962
General rules for pesticide packaging
3 Technical requirements
3.1 Appearance: White to off-white or yellow powder, without visible foreign impurities. 3.2 Promethazine technical shall also meet the requirements of the following table. %(m/m)
Promethazine content
Heating loss
Sodium chloride content
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991Superior product
First-class product
Qualified product
Implemented on July 1, 1992
W.4 Test method
4.1 Determination of promethazine content (arbitration method)4.1.1 Summary of method
HG2201-91
The sample was dissolved in chloroform and triadimefon was used as the internal standard. Promethazine was separated and quantified on a chromatographic column filled with 3% polyethylene glycol 20000/GaschromQ. 4.1.2 Reagents and solutions
Trichloromethane (GB682);
Polyethylene glycol 20000 gas chromatography stationary phase; GaschromQ: 150~180um (80~100 mesh), carrier for gas chromatography; Internal standard solution: 20g/L triadimefon chloroform solution, Promethazine standard: known content, >99.0% (m/m); Triadimefon: content ≥95% (m/m), 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, 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 160mL beaker, add about 45mL chloroform (just enough to immerse the carrier), and 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. 4.1.4.2 Gas chromatograph operating conditions Temperature: Column chamber 200 ± 5 °C; Vaporization chamber 230 °C; Detector 230 °C. Gas flow rate: Carrier gas 80 mL/min; Hydrogen 40 mL/min; Air 400 mL/min. Sample volume: Wbzsoso, cO Retention time: Promethazine 13 min; Triadimefon 18 min. HG2201-91 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 test solution4.1.4.3.1 Standard solution
Weigh 0.10g of promethazine standard sample, accurate to 0.0001g, into a small glass bottle with a cover, add 5.0mL of internal standard solution with a pipette, and shake well.
4.1.4.3.2 Test solution
Weigh a sample containing about 0.10g of promethazine finely ground and mixed, accurate to 0.0001g, into a small glass bottle with a cover, 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 standard solution of promethazine until the relative deviation of the peak height ratio (or peak area ratio) of promethazine and the internal standard in two consecutive injections is less than 0.6%. Then inject and analyze in the following order: a. Standard solution;
b. Sample solution;
Sample solution;
Standard solution.
Ww.bzsoso：com4.1.4.5 Calculation
HG2201—91
According to the chromatograms of the four injections a, b, c, respectively, calculate the average values of the peak height ratios (or peak area ratios) of promethazine and the internal standard of ad, b, and c.
The mass percentage content of promethazine (X) is calculated according to formula (1): i·m·P
Wherein: 1——the average value of the peak height ratio (or peak area ratio) of promethazine and the internal standard substance in the sample solution injected twice in b and c; T2——the average value of the peak height ratio (or peak area ratio) of promethazine and the internal standard substance 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
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 exceed 1.5%. 4.2 Determination of heating loss
4.2.1 Apparatus
Weighing bottle: height 30mm, diameter 50mm;Www.bzxZ.net
Oven: 90±2℃
Dryer.
4.2.2 Operation steps
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 an oven. After drying for about 2 hours, cover them, take them out and place them in a dryer. Weigh them after cooling to room temperature. Repeat the drying until the difference between two consecutive weighings is less than 0.01g.
4.2.3 Calculation
The heating loss (X2) expressed as a mass percentage is calculated according to formula (2): me
Where: ms—the mass of the sample and weighing bottle before drying, g; m4
—the mass of the sample and weighing bottle after drying, g; —the mass of the weighed sample, 8.
4.3 Determination of sodium chloride content
4.3.1 Reagents and solutions
Acetone (GB686);
Sulfuric acid solution: about 50% (V/V)
Hydrochloric acid standard solution, c(HC1)=0.1mol/L, prepared and calibrated according to Article 4.2 of GB601, silver nitrate standard titration solution, c(AgNO3)=0.1mol/L, prepared and calibrated according to Article 4.2.1 of GB601. 4.3.2 Instruments
Potentiometric titrator: reading accurate to 2mV;
Electrode: silver-217 type calomel electrode with potassium nitrate salt bridge. 4.3.3 Analysis steps
W.HG2201—91
Weigh 2.0g of sample, accurate to 0.0001g, dissolve in 50mL acetone in a 400mL beaker, add 200mL water, acidify the solution to pH 12 with sulfuric acid, accurately add about 2mL of hydrochloric acid standard solution, and perform potentiometric titration with silver nitrate standard titration solution. 4.3.4 Calculation
The percentage content of sodium chloride (X) is calculated according to formula (3): 0.0585(ViC1-V2c2)X100
5.85(Vic1-V2c2)
Wherein: ci is the actual concentration of the silver nitrate standard titration solution, mol/L; 2
is the actual concentration of the hydrochloric acid standard solution, mol/L; Vi is the volume of the silver nitrate standard titration solution consumed during titration, mL; V2
is the actual volume of the hydrochloric acid standard solution added to the sample solution, mL; the mass of the sample, 8;
0.0585 is the mass of sodium chloride (NaCl) expressed in grams, which is equivalent to 1.00mL of the silver nitrate standard titration solution Lc (AgNO3) = 1.000mol/L.
5 Inspection rules
5.1 Prometryn technical shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with this standard. The manufacturer shall ensure that all Prometryn technical shipped from the factory meet the requirements of this standard.
5.2 The user has the right to inspect the quality of the Prometryn technical 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 in accordance with the technical sampling method 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, when any index does not meet the requirements of this standard, re-sampling shall be conducted from twice the amount of packaging. If the re-inspection results show that even if only one index does not meet the requirements of this standard, the entire batch of Prometryn technical shall be deemed as an unqualified product. 5.5 When a dispute arises between the supply and demand parties over quality, it may be resolved through negotiation between the two parties, or by arbitration analysis by a legal inspection agency in accordance with the inspection method specified in this standard.
6 Marking, packaging, transportation and storage
6.1 The marking and packaging of promethazine technical shall comply with the relevant provisions of GB3796. 6.2 During storage and transportation, it shall be strictly protected from moisture and sunlight, maintained with good ventilation, and shall not be mixed with food, seeds and feed, and shall avoid contact with skin and inhalation through the mouth and nose.
Ww.bzsoso：comA1 Method Summary
HG2201—91
Appendix A
Gas chromatography determination method for promethazine content
(Supplement)
The sample was dissolved in dimethylformamide, and promethazine was separated and quantified using a chromatographic column with di-n-pentyl phthalate as the internal standard and 5% XE-60/chromosorbWAWDMCS as the filler. 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
HG2201—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 finely ground and 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 well, and let it stand. Take the upper clear solution for sampling and filter 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, inject and analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution,
d. Standard solution.
A6 Calculation
The mass percentage of promethazine (X) is calculated according to formula (A1): 7
W.bzsoso, cOnHG2201-91
rg·m·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 of this method should not exceed 1.5%. 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)bzsoso:comA1 Method summary
HG2201—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
HG2201—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 finely ground and 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 well, and let it stand. Take the upper clear solution for sampling and filter 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, inject and analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution,
d. Standard solution.
A6 Calculation
The mass percentage of promethazine (X) is calculated according to formula (A1): 7
W.bzsoso, cOnHG2201-91
rg·m·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 of this method should not exceed 1.5%. 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)bzsoso:comA1 Method summary
HG2201—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
HG2201—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 finely ground and 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 well, and let it stand. Take the upper clear solution for sampling and filter 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, inject and analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution,
d. Standard solution.
A6 Calculation
The mass percentage of promethazine (X) is calculated according to formula (A1): 7
W.bzsoso, cOnHG2201-91
rg·m·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 of this method should not exceed 1.5%. 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)
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