Some standard content:
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended: Six standards, China Petrochemical Industry Association proposed the standard and issued the National Pesticide Standardization Technical CommitteeThe requirements of the emetic test method and its etiquette index requirements and FAOSpecttIclon5E/T5/S/Fi1994) can be obtained by the National Agricultural Standardization Technical ...
4.2 Identification test
For commercially available paraquat, this identification test can be carried out simultaneously with the determination of paraquat. Under the same chromatographic operating conditions, the retention time of a certain chromatographic peak of the test solution and that of the chromatographic peak of the standard sample should be within one week, that is, by comparison method 1. This identification test can be carried out in reverse order with the determination of paraquat. Under the same working conditions, the maximum absorption wavelength of the sample liquid should be consistent with that of the standard sample, both of which are Gnm. 4.3 Determination of herbicide content
|4.3.1 Dropwise chromatography (secondary method)
|4.3.1.1 Summary of the method
The sample is dissolved in hot water, and sodium fluoride-ethyl acetate is used as the active phase. The herbicide in the sample is subjected to liquid chromatography and detection by digital detector using reliPuk1HMGr as the raw material. 4.3.1.2 Reagents and solutions
Sodium carbonate: Chromatographically pure:
Ethyl acetate: Chromatographically purified water;
Natural water;
Hydroxide standard sample (preferably dried at 120°C or above before use): 1! Known mass fraction 8.0%. CB 19307-2003
Mobile phase: 3.5% hexane, dissolve in 9 ml water, add 15 ml diethyl ether, adjust to H2; then add 10 ml ethyl acetate, mix well, filter with C4r filter membrane: ultrasonic 1mim4.3.1.3 Instruments
Liquid chromatography equipment: with external variable length detector quantitative injection machine: data processor or chromatograph! Column: 2.G mm (r) × 250) mm stainless steel column, filled with C: pcllPak C-RMG, 1μm filler (or other reverse phase chromatographic equipment with the same column microconcentrator, cell membrane pore detection about 0.45mm
Micro-injector.F!.
4.3. t.4 Liquid phase chromatographic operation conditions
Mobile phase volume: 1.5mL, mia:
Injection temperature, chamber (humidity change should not be greater than 3)Detection length: 29..m
Inlet: 10L
Retention time: about 5.2mn.
The above-mentioned chromatographic operation conditions are typical operation parameters. The characteristics of the instrument can be summarized, and appropriate adjustments can be made for the given selection parameters in order to obtain the overall effect. The typical herbal drug precursor chromatogram is shown in Figure 1. H
1 Herbal drug separation chromatogram
4.3.1.5 Determination steps
4.3. 1. 5.1 Preparation of standard sample
Weigh 0.15% of the standard sample containing herbicide (accurate to 0.02%) and put it in a 5m2 volumetric flask, dissolve it with water and make up to volume, shake it and leave it in a 40ml volumetric plate, add water to make up to volume and shake well. 4.3.1.5.2 Preparation of test solution
Weigh 0.1% of the standard sample containing herbicide (accurate to 0.00025%) and put it in a 50m2 volumetric flask, add water and make up to volume, add 5m2 of the standard sample and make up to volume, shake well. Then, filter through a 0.45 μm filter membrane, and then, under the above chromatographic conditions, inject several standard sample solutions into the instrument continuously until the peak area difference between two adjacent samples is less than 1.0. Then, inject the standard sample solution, test solution, sample solution, and bridge sample solution in the following order. GA19307—2003
4.3.7.6 Analysis
Average the peak areas of the two tested sample solutions and the two subsequent standard sample solutions. The mass distribution of the monochloroethane in the sample is calculated by the formula (1): A, - the average value of the monochloroethane surface area in the standard solution: A: -- the average value of the monochloroethane surface area in the sample solution! 2 -- the mass of the standard sample m, in g)
the mass of the sample, in g (m):
the mass of the standard dichloride in the sample, in %: M, -: the mass of the standard sample, in g per coul (g/mul (M, = [8.3: M -- the mass of the molar mass of the dichloroethane of T-237.2) in g per coul (/n) (M, - 237.2): 4.3.1.7 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1%. The arithmetic mean value shall be taken as the determination result. 4.3.2 Colorimetric method
4. 3.2.1 Method Summary
Biotek uses a method to reduce the mechanical droplets to blue free radicals. This free radical can be used as a blue glass slide as a comparison. Its absorbance is measured at 600 nm. A standard curve is drawn with two bottles of chemical standard samples in the cabinet. The mass fraction of the sample in the test solution is calculated from this.
4.3.2.2 Reagents and solvents
Note:
C. mo.l sodium oxide solvent
The mass fraction is: %
Acid-free reagent: Use 1 ml/T sodium hydroxide to prepare a 1% mass dispersion of sulfoxide. Prepare it before use and keep it for no more than 1 hour. The sample contains chemical standard (must be stored for more than 12 hours before use): known mass fraction 98. (%: Recommended reagent: dichloromethane Standard sample (.17g (confirmed to, (2). 5, ml. volumetric bottle. Dissolved with water, fixed, and stored for 30 days and months. 4.3.2,3 Instrument
Spectrophotometer equipped with 1cm colorimetric cell, with fast blue glass filter (or - can produce about 1.5 warm light absorption at ionm long-term material such as natural change pond light said gold net placed on the cell stand, this stand and Li than the cell carefully connected: 4.3.2.4 Determination of step frequency
4.3.2.4.1 Drawing of calibration curve
Confirm the secret absorption of 3.00m, 13.00m1.00m: 2.30ml13.00m standard melt chain into the change 5 + 1mJ volume rent, dilute with water to ml. Take one of the volumetric bottles, add 11L mass fraction of 1 Sodium diisocyanate ether solution is obtained and diluted with water to the mark in the selected chamber, the air is adjusted tightly, and the container is inverted three times at a speed of rising from one end to the other (do not shake violently to avoid immediate color loss due to oxidation): immediately transfer the solution into a 1'm colorimetric solution and use a permanent magnetic plate as a reference. Measure the absorbance of the sample at 6J1>. Dissolve the solution in other containers in the same way, but only after completing a drop of absorption determination can sodium diisocyanate ether solution with a concentration of 1% be added for the next drop of determination. Draw the calibration curve with absorbance as the ordinate and mass standard (unit: 8/mL) as the coordinate: 4.3.2.4.2 Determination of sample
Weigh the sample with the highest content of 12 (accurate to 0.92) in 50L of water to make a fixed volume. GB19307—2003
Confirm the amount of 1u.00)ral double-sided 1CCmI tube volumetric condensate. Dilute with water to 80mT, add 1lm2 mass fraction of -% rapid-acting acid, dilute with water to the scale, add purple or glass, and use bubbles to rise from the soul of the mother to the other end. The volume should be stirred violently once a small amount to avoid oxidation and color disappearance). Then transfer this melt into a 1cm colorimetric cell and use a permanent multi-color film as a reference: measure the absorbance of the solution at 69nr. According to the absorbance of the sample solution, obtain the formula from the calibration and the mass increase before condensation. 4.3.2.5 Calculate the mass fraction of the sample
and the test herb mass fraction (Xing) according to formula (2): =01G×20x100
P "The mass concentration of the herb mass fraction in the test batch of the school engineering department is in grams per liter (g:m) (see the mass spectrometry of the single R).
4.3.2.6 Allow the difference between the two parallel passes to be 0, and take the arithmetic mean as the determination result. 4.4 Determination of pH value
Control GTT: 501.
4.5 Determination of the mass ratio of herb mass fraction and triazole 4.5.1 Summary of the method
The sample is stirred for 1 h, with methanol-water as the mobile phase, in a CPakCl8M.5m filler chromatographic sample UV variable wavelength detection volume, liquid chromatography separation and formulation of the selected diaminobenzene, call calculation of mountain herb production and triazinon rain quality ratio
4.5.2 Reagents and sources
Isopropyl alcohol: chromatographic pure:
Water: freshly distilled, secondary distilled retained water:
Triazinon case details: 1! Known mass fraction is 398.0% 4.5.3 Instrument
Liquid chromatography equipment: UV variable wavelength detector and quantitative injection valve 5 spectrum data processor or chromatography workstation
No increase, 4.tmmat)×2aum stainless steel brown, CapcellPakcBMG inside, 5am filler (or its position with phase effect and chromatograph
filter: DeTeng machine contains about c.15ml
microinjector 51,
4. 5. 4 Liquid chromatography operating conditions
Flow rate E: CH.: IO) = 55t5
Flow surface flow rate ..m..
Rod: Room temperature Yi stem change should not be more than 2): Detection wavelength: 39L
Injection volume is called!
Baoshi: Oh medicine 4.6:
The above color selection parameters are typical exploration parameters. According to different instrument points, the given operating parameters can be appropriately adjusted to obtain the best effect. The color map of the typical herbal medicine GB 19307-2003
[—"Zazolam" medical ketone
4. 5.5 Steps
4.5.5.1 Preparation of sample solution
Figure 2 Liquid chromatogram of triazole pyrimidone in paraquat parent drug. 1. 2) 100 ml of the sample was dissolved in a flask, and 1 l was drawn with a pipette, and the solution was added to a 50 mL volumetric flask. Then, the solution was added with water and the solution was added. 4.5.5.2 Preparation of sample solution
Take 1.2 g of the sample (accurate to 0.001000 mL) and put it into a 50 mL volumetric flask, dissolve it in water and discard it. Use 45 mL of diaphragm to ignite the flask,
4.5.5.3 Determination
Under the working condition, after the instrument is stable, continue to inject the standard sample solution until the area of the two adjacent samples of triazole pyrimidone is less than 3.0 5%, the standard sample melts, the sample is dissolved, the sample solution is filtered, and the standard sample is filtered for analysis. 4.5.6 Calculate the mass fraction of triazolopyrimidine in the two standard sample solutions before and after the test: The mass fraction of triazolopyrimidine in the solution is calculated by the following formula: × x
period = A1X%×100
The average of the triazolopyrimidine peaks in the solution is: The average of the triazolopyrimidine peaks in the sample solution is: .--· The mass of the standard sample is in grams (R) and the mass of the standard sample is in ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
Where: ||t t||Mass fraction of sample:
Mass fraction of azole ketone in the sample,
Determination of mass fraction of 4,64.4:-bipyridine 4.6.1 Summary of method
GB19307--2003
The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-bipyridine in the sample is analyzed and determined by a chromatograph with Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions
Methanol:
Ethylene glycol: pure;
Water: freshly steamed twice hot water
4,4-Bipyridine standard sample: has a mass fraction of 93.(%.) 4.6.3 Instrument
Phase chromatographic detection: with purple variable length and reliable sampling test: including chromatographic machine or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in CapeetlFC18MG5m filler (or other chromatographic column with the same effect!
Filter: membrane pore size about G.15uml
Micro injection: CK,
4.6.4 Liquid chromatography detection working conditions
Mobile phase: CHCl:H1;
Eluent phase: 1.tL/min
Temperature: room temperature, pressure does not change||2
Detection length: 2 nm
Sampling body: 101:
Retention time.1,4\-bipyridinium about 13.mia. The above chromatographic operation conditions are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted to obtain the desired effect. The typical 1-pyridamole standard is shown in the corresponding color chart. 4.6.5 Preparation of standard sample
4.6.5.1 Weigh 44-44 batches of standard sample: 2) Weigh 1 ml of solution in a bottle and pipette it according to the volume, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (0.0100 ml, 0.0200 ml, add 50 ml of solution, and mix well. Use 0.4 micron method
4.6.5.3 Preparation of sample slide
||After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the number of adjacent two, 4,4-bipyridine peak area scan of Anhua 3.0 tablets, or standard sample solution, the sample sequence, the test solution and the standard sample rate are carefully sampled. 4.6.6
The measured peak areas of 4,4-bipyridine in the two test limits and the standard sample solution before and after the test are averaged. The mass fraction of 2,4-bipyridine in the sample (A) is calculated according to formula (5): A,XP
74=A X:XTGG
B19307-2003
The average value of the peak area of 4,4-bipyridine in the liquid sample A.
The average of the peak area of 4,4-bipyridine in the liquid sample and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
The pure 4,4-bipyridine standard sample
1--4,1*-bipyridine
The quasi-phase chromatogram of the 4,4\-bipyridine standard sample 4.7 Determination of water-insoluble matter| |tt||4.7.1 Test and Instruments
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination Method
Weigh 20g of test sample (accurate to 0.01e) and put it in a 25mL cup, add 100mL of water and stir for 2in. Press the sample in the oven to a constant weight (accurate to .M0), and then use 9) [water to wash the beaker three times. Filter: Put the orange in the oven to dry for 1h, and cool it in the dryer to get the effect (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (le), according to the formula: -2max100
Where:
The total mass of the water-free substances on the non-scale after condensation, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world conforms to the current regulations of 1 movement, but the limit of condensation, adopts the method of about lower speed, 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of Paraquat masterbatch shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat masterbatch should be packaged in clean plastic barrels or plastic-lined iron barrels. Be careful not to let it come into direct contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.3 Instruments
Liquid chromatography equipment: UV variable wavelength detector and quantitative injection valve 5 spectrum data processor or chromatography workstation
no increase, 4.tmmat)×2aum stainless steel brown, CapcellPakcBMG inside, 5am filler (or its position with phase effect and chromatograph
filter: DeTeng machine contains about c.15ml
microinjector 51,
4. 5. 4 Liquid chromatography operating conditions
Flow rate: CH.: IO) = 55t5
Flow surface flow rate ..m..
rod: room temperature change should not be more than 2): detection wavelength: 39L
injection volume!
Baoshi: Oh medicine 4.6:
The above color selection parameters are typical exploration parameters. According to different instrument points, the given operating parameters can be appropriately adjusted to obtain the best effect. The color map of the typical herbal medicine GB 19307-2003
[—"Zazolam" medical ketone
4. 5.5 Steps
4.5.5.1 Preparation of sample solution
Figure 2 Liquid chromatogram of triazole pyrimidone in paraquat parent drug. 1. 2) 100 ml of the sample was dissolved in a flask, and 1 l was drawn with a pipette, and the solution was added to a 50 mL volumetric flask. Then, the solution was added with water and the solution was added. 4.5.5.2 Preparation of sample solution
Take 1.2 g of the sample (accurate to 0.001000 mL) and put it into a 50 mL volumetric flask, dissolve it in water and discard it. Use 45 mL of diaphragm to ignite the flask,
4.5.5.3 Determination
Under the working condition, after the instrument is stable, continue to inject the standard sample solution until the area of the two adjacent samples of triazole pyrimidone is less than 3.0 5%, the standard sample melts, the sample is dissolved, the sample solution is filtered, and the standard sample is filtered for analysis. 4.5.6 Calculate the mass fraction of triazolopyrimidine in the two standard sample solutions before and after the test: The mass fraction of triazolopyrimidine in the solution is calculated by the following formula: × x
period = A1X%×100
The average of the triazolopyrimidine peaks in the solution is: The average of the triazolopyrimidine peaks in the sample solution is: .--· The mass of the standard sample is in grams (R) and the mass of the standard sample is in ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
Where: ||t t||Mass fraction of sample:
Mass fraction of azole ketone in the sample,
Determination of mass fraction of 4,64.4:-bipyridine 4.6.1 Summary of method
GB19307--2003
The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-bipyridine in the sample is analyzed and determined by a chromatograph with Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions
Methanol:
Ethylene glycol: pure;
Water: freshly steamed twice hot water
4,4-Bipyridine standard sample: has a mass fraction of 93.(%.) 4.6.3 Instrument
Phase chromatographic detection: with purple variable length and reliable sampling test: including chromatographic machine or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in CapeetlFC18MG5m filler (or other chromatographic column with the same effect!
Filter: membrane pore size about G.15uml
Micro injection: CK,
4.6.4 Liquid chromatography detection working conditions
Mobile phase: CHCl:H1;
Eluent phase: 1.tL/min
Temperature: room temperature, pressure does not change||2
Detection length: 2 nm
Sampling body: 101:
Retention time.1,4\-bipyridinium about 13.mia. The above chromatographic operation conditions are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted to obtain the desired effect. The typical 1-pyridamole standard is shown in the corresponding color chart. 4.6.5 Preparation of standard sample
4.6.5.1 Weigh 44-44 batches of standard sample: 2) Weigh 1 ml of solution in a bottle and pipette it according to the volume, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (0.0100 ml, 0.0200 ml, add 50 ml of solution, and mix well. Use 0.4 micron method
4.6.5.3 Preparation of sample slide
||After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the number of adjacent two, 4,4-bipyridine peak area scan of Anhua 3.0 tablets, or standard sample solution, the sample sequence, the test solution and the standard sample rate are carefully sampled. 4.6.6
The measured peak areas of 4,4-bipyridine in the two test limits and the standard sample solution before and after the test are averaged. The mass fraction of 2,4-bipyridine in the sample (A) is calculated according to formula (5): A,XP
74=A X:XTGG
B19307-2003
The average value of the peak area of 4,4-bipyridine in the liquid sample A.
The average of the peak area of 4,4-bipyridine in the liquid sample and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
The pure 4,4-bipyridine standard sample
1--4,1*-bipyridine
The quasi-phase chromatogram of the 4,4\-bipyridine standard sample 4.7 Determination of water-insoluble matter| |tt||4.7.1 Test and Instruments
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination Method
Weigh 20g of test sample (accurate to 0.01e) and put it in a 25mL cup, add 100mL of water and stir for 2in. Press the sample in the oven to a constant weight (accurate to .M0), and then use 9) [water to wash the beaker three times. Filter: Put the orange in the oven to dry for 1h, and cool it in the dryer to get the effect (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (le), according to the formula: -2max100
Where:
The total mass of the water-free substances on the non-scale after condensation, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world conforms to the current regulations of 1 movement, but the limit of condensation, adopts the method of about lower speed, 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of Paraquat masterbatch shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat masterbatch should be packaged in clean plastic barrels or plastic-lined iron barrels. Be careful not to let it come into direct contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.3 Instruments
Liquid chromatography equipment: UV variable wavelength detector and quantitative injection valve 5 spectrum data processor or chromatography workstation
no increase, 4.tmmat)×2aum stainless steel brown, CapcellPakcBMG inside, 5am filler (or its position with phase effect and chromatograph
filter: DeTeng machine contains about c.15ml
microinjector 51,
4. 5. 4 Liquid chromatography operating conditions
Flow rate: CH.: IO) = 55t5
Flow surface flow rate ..m..
rod: room temperature change should not be more than 2): detection wavelength: 39L
injection volume!
Baoshi: Oh medicine 4.6:
The above color selection parameters are typical exploration parameters. According to different instrument points, the given operating parameters can be appropriately adjusted to obtain the best effect. The color map of the typical herbal medicine GB 19307-2003
[—"Zazolam" medical ketone
4. 5.5 Steps
4.5.5.1 Preparation of sample solution
Figure 2 Liquid chromatogram of triazole pyrimidone in paraquat parent drug. 1. 2) 100 ml of the sample was dissolved in a flask, and 1 l was drawn with a pipette, and the solution was added to a 50 mL volumetric flask. Then, the solution was added with water and the solution was added. 4.5.5.2 Preparation of sample solution
Take 1.2 g of the sample (accurate to 0.001000 mL) and put it into a 50 mL volumetric flask, dissolve it in water and discard it. Use 45 mL of diaphragm to ignite the flask,
4.5.5.3 Determination
Under the working condition, after the instrument is stable, continue to inject the standard sample solution until the area of the two adjacent samples of triazole pyrimidone is less than 3.0 5%, the standard sample melts, the sample is dissolved, the sample solution is filtered, and the standard sample is filtered for analysis. 4.5.6 Calculate the mass fraction of triazolopyrimidine in the two standard sample solutions before and after the test: The mass fraction of triazolopyrimidine in the solution is calculated by the following formula: × x
period = A1X%×100
The average of the triazolopyrimidine peaks in the solution is: The average of the triazolopyrimidine peaks in the sample solution is: .--· The mass of the standard sample is in grams (R) and the mass of the standard sample is in ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
Where: ||t t||Mass fraction of sample:
Mass fraction of azole ketone in the sample,
Determination of mass fraction of 4,64.4:-bipyridine 4.6.1 Summary of method
GB19307--2003
The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-bipyridine in the sample is analyzed and determined by a chromatograph with Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions
Methanol:
Ethylene glycol: pure;
Water: freshly steamed twice hot water
4,4-Bipyridine standard sample: has a mass fraction of 93.(%.) 4.6.3 Instrument
Phase chromatographic detection: with purple variable length and reliable sampling test: including chromatographic machine or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in CapeetlFC18MG5m filler (or other chromatographic column with the same effect!
Filter: membrane pore size about G.15uml
Micro injection: CK,
4.6.4 Liquid chromatography detection working conditions
Mobile phase: CHCl:H1;
Eluent phase: 1.tL/min
Temperature: room temperature, pressure does not change||2
Detection length: 2 nm
Sampling body: 101:
Retention time.1,4\-bipyridinium about 13.mia. The above chromatographic operation conditions are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted to obtain the desired effect. The typical 1-pyridamole standard is shown in the corresponding color chart. 4.6.5 Preparation of standard sample
4.6.5.1 Weigh 44-44 batches of standard sample: 2) Weigh 1 ml of solution in a bottle and pipette it according to the volume, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (0.0100 ml, 0.0200 ml, add 50 ml of solution, and mix well. Use 0.4 micron method
4.6.5.3 Preparation of sample slide
||After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the number of adjacent two, 4,4-bipyridine peak area scan of Anhua 3.0 tablets, or standard sample solution, the sample sequence, the test solution and the standard sample rate are carefully sampled. 4.6.6
The measured peak areas of 4,4-bipyridine in the two test limits and the standard sample solution before and after the test are averaged. The mass fraction of 2,4-bipyridine in the sample (A) is calculated according to formula (5): A,XP
74=A X:XTGG
B19307-2003
The average value of the peak area of 4,4-bipyridine in the liquid sample A.
The average of the peak area of 4,4-bipyridine in the liquid sample and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
The pure 4,4-bipyridine standard sample
1--4,1*-bipyridine
The quasi-phase chromatogram of the 4,4\-bipyridine standard sample 4.7 Determination of water-insoluble matter| |tt||4.7.1 Test and Instruments
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination Method
Weigh 20g of test sample (accurate to 0.01e) and put it in a 25mL cup, add 100mL of water and stir for 2in. Press the sample in the oven to a constant weight (accurate to .M0), and then use 9) [water to wash the beaker three times. Filter: Put the orange in the oven to dry for 1h, and cool it in the dryer to get the effect (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (le), according to the formula: -2max100
Where:
The total mass of the water-free substances on the non-scale after condensation, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world conforms to the current regulations of 1 movement, but the limit of condensation, adopts the method of about lower speed, 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of Paraquat masterbatch shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat masterbatch should be packaged in clean plastic barrels or plastic-lined iron barrels. Be careful not to let it come into direct contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.
Stem: Room temperature change should not be greater than 2): Detection wavelength: 39L
Input sample volume!
Time: Medicine 4.6:
The above chromatographic parameters are typical detection parameters. According to different instrument points, the given operating parameters can be appropriately adjusted to obtain the effective results. The chromatographic diagram of a typical herbal medicine is GB 19307-2003
[—"Xinazole"
4. 5.5 Steps
4.5.5.1 Preparation of sample solution
Figure 2 Liquid chromatogram of triazole pyrimidone in paraquat parent drug. 1. 2) 100 ml of the sample was dissolved in a flask, and 1 l was drawn with a pipette, and the solution was added to a 50 mL volumetric flask. Then, the solution was added with water and the solution was added. 4.5.5.2 Preparation of sample solution
Take 1.2 g of the sample (accurate to 0.001000 mL) and put it into a 50 mL volumetric flask, dissolve it in water and discard it. Use 45 mL of diaphragm to ignite the flask,
4.5.5.3 Determination
Under the working condition, after the instrument is stable, continue to inject the standard sample solution until the area of the two adjacent samples of triazole pyrimidone is less than 3.0 5%, the standard sample melts, the sample is dissolved, the sample solution is filtered, and the standard sample is filtered for analysis. 4.5.6 Calculate the mass fraction of triazolopyrimidine in the two standard sample solutions before and after the test: The mass fraction of triazolopyrimidine in the solution is calculated by the following formula: × x
period = A1X%×100
The average of the triazolopyrimidine peaks in the solution is: The average of the triazolopyrimidine peaks in the sample solution is: .--· The mass of the standard sample is in grams (R) and the mass of the standard sample is in ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
Where: ||t t||Mass fraction of sample:
Mass fraction of azole ketone in the sample,
Determination of mass fraction of 4,64.4:-bipyridine 4.6.1 Summary of method
GB19307--2003
The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-bipyridine in the sample is analyzed and determined by a chromatograph with Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions
Methanol:
Ethylene glycol: pure;
Water: freshly steamed twice hot water
4,4-Bipyridine standard sample: has a mass fraction of 93.(%.) 4.6.3 Instrument
Phase chromatographic detection: with purple variable length and reliable sampling test: including chromatographic machine or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in CapeetlFC18MG5m filler (or other chromatographic column with the same effect!
Filter: membrane pore size about G.15uml
Micro injection: CK,
4.6.4 Liquid chromatography detection working conditions
Mobile phase: CHCl:H1;
Eluent phase: 1.tL/min
Temperature: room temperature, pressure does not change||2
Detection length: 2 nm
Sampling body: 101:
Retention time.1,4\-bipyridinium about 13.mia. The above chromatographic operation conditions are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted to obtain the desired effect. The typical 1-pyridamole standard is shown in the corresponding color chart. 4.6.5 Preparation of standard sample
4.6.5.1 Weigh 44-44 batches of standard sample: 2) Weigh 1 ml of solution in a bottle and pipette it according to the volume, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (0.0100 ml, 0.0200 ml, add 50 ml of solution, and mix well. Use 0.4 micron method
4.6.5.3 Preparation of sample slide
||After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the number of adjacent two, 4,4-bipyridine peak area scan of Anhua 3.0 tablets, or standard sample solution, the sample sequence, the test solution and the standard sample rate are carefully sampled. 4.6.6
The measured peak areas of 4,4-bipyridine in the two test limits and the standard sample solution before and after the test are averaged. The mass fraction of 2,4-bipyridine in the sample (A) is calculated according to formula (5): A,XP
74=A X:XTGG
B19307-2003wwW.bzxz.Net
The average value of the peak area of 4,4-bipyridine in the liquid sample A.
The average of the peak area of 4,4-bipyridine in the liquid sample and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
The pure 4,4-bipyridine standard sample
1--4,1*-bipyridine
The quasi-phase chromatogram of the 4,4\-bipyridine standard sample 4.7 Determination of water-insoluble matter| |tt||4.7.1 Test and Instruments
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination Method
Weigh 20g of test sample (accurate to 0.01e) and put it in a 25mL cup, add 100mL of water and stir for 2in. Press the sample in the oven to a constant weight (accurate to .M0), and then use 9) [water to wash the beaker three times. Filter: Put the orange in the oven to dry for 1h, and cool it in the dryer to get the effect (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (le), according to the formula: -2max100
Where:
The total mass of the water-free substances on the non-scale after condensation, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world conforms to the current regulations of 1 movement, but the limit of condensation, adopts the method of about lower speed, 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of Paraquat masterbatch shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat masterbatch should be packaged in clean plastic barrels or plastic-lined iron barrels. Be careful not to let it come into direct contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.
Stem: Room temperature change should not be greater than 2): Detection wavelength: 39L
Input sample volume!
Time: Medicine 4.6:
The above chromatographic parameters are typical detection parameters. According to different instrument points, the given operating parameters can be appropriately adjusted to obtain the effective results. The chromatographic diagram of a typical herbal medicine is GB 19307-2003
[—"Xinazole"
4. 5.5 Steps
4.5.5.1 Preparation of sample solution
Figure 2 Liquid chromatogram of triazole pyrimidone in paraquat parent drug. 1. 2) 100 ml of the sample was dissolved in a flask, and 1 l was drawn with a pipette, and the solution was added to a 50 mL volumetric flask. Then, the solution was added with water and the solution was added. 4.5.5.2 Preparation of sample solution
Take 1.2 g of the sample (accurate to 0.001000 mL) and put it into a 50 mL volumetric flask, dissolve it in water and discard it. Use 45 mL of diaphragm to ignite the flask,
4.5.5.3 Determination
Under the working condition, after the instrument is stable, continue to inject the standard sample solution until the area of the two adjacent samples of triazole pyrimidone is less than 3.0 5%, the standard sample melts, the sample is dissolved, the sample solution is filtered, and the standard sample is filtered for analysis. 4.5.6 Calculate the mass fraction of triazolopyrimidine in the two standard sample solutions before and after the test: The mass fraction of triazolopyrimidine in the solution is calculated by the following formula: × x
period = A1X%×100
The average of the triazolopyrimidine peaks in the solution is: The average of the triazolopyrimidine peaks in the sample solution is: .--· The mass of the standard sample is in grams (R) and the mass of the standard sample is in ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
Where: ||t t||Mass fraction of sample:
Mass fraction of azole ketone in the sample,
Determination of mass fraction of 4,64.4:-bipyridine 4.6.1 Summary of method
GB19307--2003
The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-bipyridine in the sample is analyzed and determined by a chromatograph with Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions
Methanol:
Ethylene glycol: pure;
Water: freshly steamed twice hot water
4,4-Bipyridine standard sample: has a mass fraction of 93.(%.) 4.6.3 Instrument
Phase chromatographic detection: with purple variable length and reliable sampling test: including chromatographic machine or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in CapeetlFC18MG5m filler (or other chromatographic column with the same effect!
Filter: membrane pore size about G.15uml
Micro injection: CK,
4.6.4 Liquid chromatography detection working conditions
Mobile phase: CHCl:H1;
Eluent phase: 1.tL/min
Temperature: room temperature, pressure does not change||2
Detection length: 2 nm
Sampling body: 101:
Retention time.1,4\-bipyridinium about 13.mia. The above chromatographic operation conditions are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted to obtain the desired effect. The typical 1-pyridamole standard is shown in the corresponding color chart. 4.6.5 Preparation of standard sample
4.6.5.1 Weigh 44-44 batches of standard sample: 2) Weigh 1 ml of solution in a bottle and pipette it according to the volume, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (0.0100 ml, 0.0200 ml, add 50 ml of solution, and mix well. Use 0.4 micron method
4.6.5.3 Preparation of sample slide
||After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the number of adjacent two, 4,4-bipyridine peak area scan of Anhua 3.0 tablets, or standard sample solution, the sample sequence, the test solution and the standard sample rate are carefully sampled. 4.6.6
The measured peak areas of 4,4-bipyridine in the two test limits and the standard sample solution before and after the test are averaged. The mass fraction of 2,4-bipyridine in the sample (A) is calculated according to formula (5): A,XP
74=A X:XTGG
B19307-2003
The average value of the peak area of 4,4-bipyridine in the liquid sample A.
The average of the peak area of 4,4-bipyridine in the liquid sample and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
The pure 4,4-bipyridine standard sample
1--4,1*-bipyridine
The quasi-phase chromatogram of the 4,4\-bipyridine standard sample 4.7 Determination of water-insoluble matter| |tt||4.7.1 Test and Instruments
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination Method
Weigh 20g of test sample (accurate to 0.01e) and put it in a 25mL cup, add 100mL of water and stir for 2in. Press the sample in the oven to a constant weight (accurate to .M0), and then use 9) [water to wash the beaker three times. Filter: Put the orange in the oven to dry for 1h, and cool it in the dryer to get the effect (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (le), according to the formula: -2max100
Where:
The total mass of the water-free substances on the non-scale after condensation, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world conforms to the current regulations of 1 movement, but the limit of condensation, adopts the method of about lower speed, 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of Paraquat masterbatch shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat masterbatch should be packaged in clean plastic barrels or plastic-lined iron barrels. Be careful not to let it come into direct contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.6. The area of the two needle test samples before and after the actual measurement is used to calculate the average of the triazole pyrimidine ketone content in the test solution: The mass fraction of the triazole pyrimidine ketone in the solution is calculated by the following formula: (Calculation formula: × x
period=A1X%×100
The average of the triazole pyrimidine ketone peaks in the test solution: The average of the triazole pyrimidine ketone peaks in the test solution is:.—·The mass of the standard sample is in grams (R). The mass unit is ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
In this formula:
The mass fraction of the sample is:
The mass fraction of the triazole pyrimidine ketone in the sample is,
4,64.4:- Determination of mass fraction of pyridine 4.6.1 Summary of the method GB19307--2003 The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-pyridine in the sample is separated and determined by a chromatograph with a UV variable length detector and Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions Methanol: Ethylene glycol: ergonomically pure; Water: freshly distilled twice hot water 4,4-pyridine standard sample: has a mass fraction of 93.(%. 4.6.3 Apparatus Phase chromatography: with UV variable length detector and fixed sample injection measurement: including chromatographic workstation or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in Capee FC18MG5m filling material (or other materials with the same effect) chromatographic column
filter: membrane pore size about G.15uml
microinjection: CK,
4.6.4 Liquid chromatography operating conditions
mobile phase: CHC:H1;
washing phase: 1.tL/min
temperature: room temperature, no pressure change
detection length: 2 nm
injection volume: 101:
retention time. 1,4\-bipyridinium about 13.mia. The above chromatographic operation requirements are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted appropriately to obtain the desired effect. The typical chromatographic diagram of 1,4\-bipyridinium benchmark is shown in 4.6.5 Preparation of standard sample
4.6.5.1 Preparation of standard sample
Weigh 44-44 batches of standard sample: Detailed information: 2) 1m. solution in a bottle and determine the value. Pipette liquid according to the volume plate, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (car 0, n002, 50l. In the amount of 50l., add the solution of this paint to the solution, and use the 0,4 method in the method 4.6.5.3. After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the margin, and then scan the 3.0-dipyridyl peak area of the two adjacent test samples or standard sample solution, and carefully separate the sample sequence and the test solution and standard sample rate. 4.6.6. The measured peak areas of 4,4-dipyridyl in the two test limits and the standard sample solution before and after the test are averaged respectively. The mass fraction of 2,4-pyrrolidone in the sample (in grams) is calculated according to formula (5): A,XP
74=AX:XTGG
B19307-2003
The average value A of the peak area of 4,4-pyrrolidone in the sample liquid.
The average value of the peak area of 2,4-pyrrolidone in the sample liquid and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
4,4.-Quick precipitate standard sample pure anhydrous
1--4,1*-bipyridine
34,4\-bipyridine standard sample quasi-phase chromatogram 4.7 Determination of water insoluble matter
4.7.1 Test and instrument
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination method
Weigh 20g of test solution (accurate to 0.01e) and put it in a 25mL cup, add 100mL water and stir for 2in. Press in the oven to constant weight (accurate to .M0) and then use 9) [water to wash the beaker three times. Filter: Dry the citrus in the oven for 1h, and cool it to dryness (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (music), according to the formula: -2max100
Where:
The total mass of the non-water-free substances after grinding, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass range of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world meets the current requirements of 1 dynamic, the limit of condensation, but the method of adopting the method of about lower than 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of the herbal medicine shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat herbal medicine should be packaged in clean plastic barrels or plastic-lined iron barrels, and be careful not to make it directly contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.6. The area of the two needle test samples before and after the actual measurement is used to calculate the average of the triazole pyrimidine ketone content in the test solution: The mass fraction of the triazole pyrimidine ketone in the solution is calculated by the following formula: (Calculation formula: × x
period=A1X%×100
The average of the triazole pyrimidine ketone peaks in the test solution: The average of the triazole pyrimidine ketone peaks in the test solution is:.—·The mass of the standard sample is in grams (R). The mass unit is ratio (g):
The purity of the standard sample is calculated by the mass ratio of the sample to the sample mass ratio according to formula (4): w
In this formula:
The mass fraction of the sample is:
The mass fraction of the triazole pyrimidine ketone in the sample is,
4,64.4:- Determination of mass fraction of pyridine 4.6.1 Summary of the method GB19307--2003 The test column is dissolved in water, acetonitrile is used as the mobile phase, and the 4,4-pyridine in the sample is separated and determined by a chromatograph with a UV variable length detector and Capcell Pakt&M,5m as the material. 4.6.2 Reagents and solutions Methanol: Ethylene glycol: ergonomically pure; Water: freshly distilled twice hot water 4,4-pyridine standard sample: has a mass fraction of 93.(%. 4.6.3 Apparatus Phase chromatography: with UV variable length detector and fixed sample injection measurement: including chromatographic workstation or chromatographic workstation; chromatographic 4.bmd×25um stainless valve, built-in Capee FC18MG5m filling material (or other materials with the same effect) chromatographic column
filter: membrane pore size about G.15uml
microinjection: CK,
4.6.4 Liquid chromatography operating conditions
mobile phase: CHC:H1;
washing phase: 1.tL/min
temperature: room temperature, no pressure change
detection length: 2 nm
injection volume: 101:
retention time. 1,4\-bipyridinium about 13.mia. The above chromatographic operation requirements are typical operating parameters. According to the characteristics of different equipment, the given operating parameters should be adjusted appropriately to obtain the desired effect. The typical chromatographic diagram of 1,4\-bipyridinium benchmark is shown in 4.6.5 Preparation of standard sample
4.6.5.1 Preparation of standard sample
Weigh 44-44 batches of standard sample: Detailed information: 2) 1m. solution in a bottle and determine the value. Pipette liquid according to the volume plate, add water and shake well. 4.6.5.2 Preparation of sample slide
Weigh 200 ml of sample (car 0, n002, 50l. In the amount of 50l., add the solution of this paint to the solution, and use the 0,4 method in the method 4.6.5.3. After the above conditions are met, wait for the instrument to be set, and then continue to inject the needle to indicate the margin, and then scan the 3.0-dipyridyl peak area of the two adjacent test samples or standard sample solution, and carefully separate the sample sequence and the test solution and standard sample rate. 4.6.6. The measured peak areas of 4,4-dipyridyl in the two test limits and the standard sample solution before and after the test are averaged respectively. The mass fraction of 2,4-pyrrolidone in the sample (in grams) is calculated according to formula (5): A,XP
74=AX:XTGG
B19307-2003
The average value A of the peak area of 4,4-pyrrolidone in the sample liquid.
The average value of the peak area of 2,4-pyrrolidone in the sample liquid and the mass of the sample, in grams ():
The mass of the sample, in grams ()!
4,4.-Quick precipitate standard sample pure anhydrous
1--4,1*-bipyridine
34,4\-bipyridine standard sample quasi-phase chromatogram 4.7 Determination of water insoluble matter
4.7.1 Test and instrument
Oven: 105-2℃
Suction filter bottle 0um1
4.7.2 Determination method
Weigh 20g of test solution (accurate to 0.01e) and put it in a 25mL cup, add 100mL water and stir for 2in. Press in the oven to constant weight (accurate to .M0) and then use 9) [water to wash the beaker three times. Filter: Dry the citrus in the oven for 1h, and cool it to dryness (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (music), according to the formula: -2max100
Where:
The total mass of the non-water-free substances after grinding, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass range of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world meets the current requirements of 1 dynamic, the limit of condensation, but the method of adopting the method of about lower than 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of the herbal medicine shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat herbal medicine should be packaged in clean plastic barrels or plastic-lined iron barrels, and be careful not to make it directly contact with gold. Net content per handle: 2001. or 200. Other forms of packaging can also be used according to user requirements or order agreements, but they must meet the requirements of (33796). 5.3 Paraquat mother drug packaging should be stored in a ventilated and dry warehouse. 6.4 During storage and transportation, the product should be kept away from moisture and sunlight and should not be placed with food, seeds, and other materials. Avoid contact with skin and eyes. Prevent inhalation through the mouth. 5.5 Safety: This product is moderately toxic and has an irritating effect on eye fat. It can cause temporary damage to nails. When using this product, it is necessary to provide protective glasses and glue Leather gloves, if accidentally dropped into the eyes, immediately open the eye gel, use water to run 15min, then seek medical treatment, if the skin is stained with this product, immediately wash with clean water, if taken by mistake, immediately induce vomiting, and seek medical attention in time. Use 1L pressure-benefit fraction of 15% test white or mass fraction of ?% moist soil or activated carbon total suspension, and take it at the same time, wear other suitable pollutants. 5.6 Acceptance period: The acceptance period of paraquat mother drug is 1 month. From the date of delivery, the quality acceptance of the product shall be completed within 1 month, and all indicators shall meet the standard requirements.5.2 Preparation of sample slide
Weigh the sample (0.2g of car, n002, 50l of world ten). Add the solution of this paint to the sample. Use 0.4 method to prepare the sample.
4.6.5.3 Just set
Put the above conditions in place, wait for the instrument to be set, and then continue to inject the needle to reduce the margin. Scan the peak area of 3.0-dipyridyl tablets of Anhua, or take standard solution. Sample sequence, test solution standard sample 4.6.6 The average of the peak areas of 4,4-bipyrrolidone in the two test samples and the standard sample solution before and after the test is calculated. The mass fraction of 2,4-bipyrrolidone in the sample (A) is calculated according to formula (5): A,XP
74=AX:XTGG
B19307-2003
The average value of the peak area of 4,4-bipyrrolidone in the standard sample solution A
The average of the peak area of 4-bipyridine in the sample solution and the mass of the detection column, in grams ():
The mass of the sample, in grams ()!
The pure 4,4.-bipyridine standard sample
1--4,1*-bipyridine
The quasi-phase chromatogram of 4,4\-bipyridine standard sample 4.7 Determination of water-insoluble matter
4.7.1 Identification and instrument
Oven: 1 05-2℃
Suction filter bottle oum1
4.7.2 Determination method
Weigh 20g of test push (accurate to 0.01e) and put it in a 25mL cup, add 100mL of water and stir for 2in. Press the garbage in the oven to constant weight (accurate to .M0), and then use 9) [water, wash the beaker three times. Filter: Put the orange in the oven to dry for 1h, and cool it in the dryer to get the effect (accurate to 0.0002g). The water-free substances in the test column are recorded as 12 (le), according to the formula: -2max100
Where:
The total mass of the water-free substances on the non-scale after condensation, the unit is point ()! The mass of the constant disease, the single signature is grams:
The mass of the sample, the unit is grams,
4.8 Inspection and acceptance of products
The world conforms to the current regulations of 1 movement, but the limit of condensation, adopts the method of about lower speed, 8
5 Marking, labeling, packaging and storage and transportation
The marking, labeling and packaging of Paraquat masterbatch shall comply with the provisions of GB3/U6, E
tn9307-2c03
5.2 Paraquat masterbatch should be packaged in clean plastic barrels or plastic-lined iron barrels. Be careful not to let it come into direct contact with gold. Net content per handle: 2001. or 200. Other forms of packaging
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.