Some standard content:
ICS65.100
Registration No.: 10931--2002
Chemical Industry Standard of the People's Republic of China
HG3701-2002
Trifluralin Technical
Published on September 28, 2002
Implemented on June 1, 2003
Published by the State Economic and Trade Commission of the People's Republic of China
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. HG3701--2002
This standard is modified and formulated based on the United Nations Food and Agriculture Organization (FAO) pesticide specification "Trifluralin Technical" standard FAOSpecification183/TC)S(1989)7.
The main difference between this standard and FAO Specification 183/TC/S (1989) is that the control items of acetone insoluble matter are added. This standard was proposed by the Policy and Regulations Department of the former State Bureau of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Pesticide Standardization Technical Committee (CSBTS/TC133). The responsible drafting unit of this standard is Shenyang Chemical Research Institute. The participating drafting unit of this standard is Dongyang Dongnong Chemical Co., Ltd. The main drafters of this standard are Zhang Pilong, Lou Shaowei, Xu Guoxin, Wu Hao. This standard is entrusted to the Secretariat of the National Pesticide Standardization Technical Committee for interpretation. 1
Trifluralin technical
Other names, structural formulas and basic physicochemical parameters of the active ingredient trifluralin of this product are as follows:ISO common name: Trifluralin
CIPAC digital code: 183
Chemical name: N,N-dipropyl-4-trifluoromethyl-2,6-dinitroanilineStructural formula:
Empirical formulaCaHeFN,O
NOCH.CHaCHs
CH.CHaCHa
Relative molecular mass: 335.3 (according to the 1997 international relative atomic mass)Biological activity: Herbicidal
Vapor pressure (25℃): 1.4×10-2Pa
Relative density (22℃): 1.36||tt| |Flash point (℃): 151 (closed cup)
Melting point (℃): 48.5~49.0
Boiling point (℃24Pa): 96~97
HG3701—2002
Solubility (g/L, 25℃): Water 1.84×10-4 (pH5) 2.21×10-4 (pH7) 1.88×10-4 (pH9), acetone 400, xylene 580, trifluoromethane, acetonitrile, toluene, ethyl acetate 1000, methanol 33~40, hexane 50~60Stability: Stable below 52℃, stable in aqueous medium with pH=3~9 (52℃), decomposes under ultraviolet light in the range of 1
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of trifluralin technical. This standard applies to trifluralin technical consisting of trifluralin and impurities generated during production. 2 Normative references
The clauses in the following documents become clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, the parties who reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version applies to this standard. GB/T1604 Acceptance Rules for Commercial Pesticides
GB/T1605 Sampling Methods for Commercial Pesticides
GB3796 General Rules for Pesticide Packaging
3 Requirements
3.1 Appearance: Yellow solid.
3.2 The control indicators of trifluralin technical shall meet the requirements of Table 1. HG3701~2002
Mass fraction of fluralin, %
Mass fraction of N,N-nitrosodipropylamine, mg/kgMass fraction of acetone insoluble matter, %
Table 1 Fluralin technical control item index
The test of acetone insoluble matter mass fraction is a random inspection item. Under normal production conditions, it shall be inspected at least once every three monthsa
4 Test method
4.1 Sampling
It shall be carried out in accordance with the method of "sampling of commercial technical materials" in GB/T1605. The sampling packages shall be determined by the random number table method, and the final sampling volume shall be not less than 100g.
4.2 Identification test
4.2.1 Gas chromatography: This identification test can be carried out simultaneously with the determination of the mass fraction of fluralin. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak in the sample solution and the retention time of the chromatographic peak of fluralin in the standard solution should be within 1.5%. 4.2.2 Infrared spectroscopy: There should be no obvious difference between the infrared spectra of the sample and the standard in the wavenumber range of 4000cm1~400cm-1. The infrared spectrum of the fluralin standard sample is shown in Figure 1. 4.000
4.3 Determination of the mass fraction of fluralin
4.3.1 Summary of the method
Figure 1 Infrared spectrum of the fluralin standard sample
The sample is dissolved in acetone, diisobutyl phthalate is used as the internal standard, a glass column with 5% DC-200 as the filling material and a hydrogen flame ionization detector are used to separate the fluralin in the sample by gas chromatography and quantify it by the internal standard method. 4.3.2 Reagents and solutions
Acetone.
Fluralin standard sample: known mass fraction greater than or equal to 99.0%. Internal standard: diisobutyl phthalate, should be free of impurities that interfere with analysis. Stationary liquid: DC-200.
Carrier: Chromosorb W/AWDMCS (180μm~250μm). HG3701-2002
Internal standard solution: weigh 0.8g of diisobutyl phthalate, place in a 250mL volumetric flask, add appropriate amount of acetone to dissolve, dilute to scale, and shake to hook.
4.3.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic data processor.
Chromatographic column: 1.5m×3.2mmi.d.) glass column. Column filling: DC-200 coated on Chromosorb W/AWDMCS (180μm~250um), stationary liquid: (stationary liquid + carrier) = 5:100.
4.3.4 Preparation of chromatographic columns
4.3.4.1 Application of stationary liquid
Accurately weigh 0.5g DC-200 stationary liquid into a 250mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of acetone to completely dissolve it: Pour 9.5g of the carrier, shake gently to mix well and evaporate the solvent to dryness, then put the beaker into an oven at 80℃ to dry for 2h, take it out and cool it to room temperature in a desiccator.
4.3.4.2 Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, and fill the prepared filler into the column in batches, while constantly tapping the column wall until it is filled to 0.5cm from the column outlet. Move the funnel to the inlet of the chromatographic column, plug a small ball of silanized glass wool at the outlet, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, continue to slowly add the filler, and constantly tap the column wall to make it evenly and tightly filled. After filling, also plug a small ball of glass wool at the inlet end and press it appropriately to keep the filler in the column from moving. 4.3.4.3 Aging of chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, do not connect the outlet end to the detector for the time being, pass the carrier gas (Nz) at a flow rate of 15mL/min, raise the temperature to 230℃ in stages, and age at this temperature for 24h. 4.3.5 Gas chromatography operating conditions
Temperature (℃): column chamber 174, vaporization chamber 205, detection chamber 275. Gas flow rate (mL/min), carrier gas (N.) 50, hydrogen 35, air 350. Injection volume (uL): 1.0.
Retention time (min): trifluralin 5.7, internal standard 11.4. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of trifluralin original drug is shown in Figure 2. (101)
HG37012002
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
1 dose, 2-fluralin, 3-internal standard
Figure 2 Gas chromatogram of fluralin original drug
Weigh 0.05g of fluralin standard sample (accurate to 0.0002g), place it in a stoppered glass bottle, add 10mL of internal standard solution accurately with a pipette, and shake well.
4.3.6.2 Preparation of sample solution
Weigh about 0.05g of sample containing fluralin (accurate to 0.0002g), place it in a stoppered glass bottle, and mix with 4.3.6.Accurately add 10mL of internal standard solution to the same pipette used in 1 and shake well. 4.3.6.3 Determination
Under the above operating conditions, after the baseline of the instrument is stable, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and when the relative response value of two adjacent needles changes by less than 1%, measure in the order of standard solution, sample solution, sample solution, and standard solution.
4.3.7 Calculation
Average the ratio of the peak area of trifluralin to the internal standard in the two needles of sample solution and the two needles of standard solution before and after the sample. The mass fraction W (%) of fluramide is calculated according to formula (1): ramP
Wherein:
-The average value of the peak area ratio of fluramide to the internal standard in the standard solution; r2--The average value of the peak area ratio of fluramide to the internal standard in the sample solution: mi~The mass of the standard sample, in grams (g); m2The mass of the sample, in grams (g);
PThe mass fraction of fluramide in the standard sample, expressed in %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1.5%. Take the arithmetic mean as the determination result. 4.4 Determination of the mass fraction of N,N-di-n-propylnitrosamine 4.4.1 Summary of the method
Note: N,N-di-n-propylnitrosamine is a potent carcinogen. Avoid contact during operation! 4
HG3701-2002
The sample is dissolved in n-hexane, placed in a silica gel column and eluted with toluene to separate trifluralin, and then N, N-di-n-propylnitrosamine is eluted with isopropanol. The N, N-di-n-propylnitrosamine in the isopropanol eluent is separated by gas chromatography using a capillary column and a nitrogen-phosphorus detector, and quantified by the external standard method.
4.4.2 Reagents and solutions
N-hexane.
Toluene.
Isopropanol.
Absolute ethanol.
N, N-di-n-propylnitrosamine standard sample: known mass fraction greater than or equal to 90%. Capillary quartz column: MEGABORECARBOWAX, 30mX0.53mm(id), film thickness 1.2μm. Silica gel cartridge: WATERS51900.
4.4.3 Instruments
Gas chromatograph: with nitrogen-phosphorus detector.
Chromatographic data processor.
Glass concentrator: 10mL with scale.
KD steaming flask: 500mL
Glass syringe: 10mL with scale.
Condenser: spherical distillation column.
Constant temperature water bath.
4.4.4 Gas chromatographic operating conditions
Temperature (℃): Column chamber 140 for 8min and then increase to 230 at 40/min, vaporization chamber 200, detector chamber 200. Gas flow rate (mL/min): carrier gas (Hea) 20, hydrogen 50, air 500. Current (pA): 30~40.
Injection volume (uL): 1.0.
Retention time (min), N,N-nitrosodipropylamine 4.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of N,N-nitrosodipropylamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then extract for 5 more minutes. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.7 Calculation
Average the ratio of the peak area of trifluralin to the internal standard in the two sample solutions and the two standard solutions before and after the sample. The mass fraction of trifluralin W (%) is calculated according to formula (1):ramP
Where:
--the average value of the peak area ratio of trifluralin to the internal standard in the standard solution;r2--the average value of the peak area ratio of trifluralin to the internal standard in the sample solution:mi~the mass of the standard sample, in grams (g);m2the mass of the sample, in grams (g);
Pthe mass fraction of trifluralin in the standard sample, expressed in %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.5%. Take the arithmetic mean as the determination result. 4.4 Determination of mass fraction of N,N-nitrosodipropylamine 4.4.1 Summary of the method
Note: N,N-nitrosodipropylamine is a potent carcinogen. Avoid contact during operation! 4
HG3701-2002
The sample is dissolved in n-hexane, placed in a silica gel column and eluted with toluene to separate trifluralin. N,N-nitrosodipropylamine is then eluted with isopropanol. The N,N-nitrosodipropylamine in the isopropanol eluent is separated by gas chromatography using a capillary column and a nitrogen-phosphorus detector, and quantified by the external standard method.
4.4.2 Reagents and solutions
N-hexane.
Toluene.
Isopropanol.
Anhydrous ethanol.
N,N-nitrosodipropylamine standard sample: known mass fraction greater than or equal to 90%. Capillary quartz column: MEGABORECARBOWAX, 30mX0.53mm(id), film thickness 1.2μm. Silica gel cartridge: WATERS51900.
4.4.3 Apparatus
Gas chromatograph: with nitrogen-phosphorus detector.
Chromatographic data processor.
Glass concentrator: 10mL with scale.
KD steaming flask: 500mL
Glass syringe: 10mL with scale.
Condenser: spherical distillation column.
Constant temperature water bath.
4.4.4 Gas chromatographic operating conditions
Temperature (℃): Column chamber 140℃ for 8min, then heated to 230℃ at 40/min, vaporization chamber 200℃, detector chamber 200℃. Gas flow rate (mL/min): carrier gas (Hea) 20, hydrogen 50, air 500. Current (pA): 30~40.
Injection volume (uL): 1.0.
Retention time (min), N,N-di-n-propylnitrosamine 4.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of N,N-di-n-propylnitrosamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then extract for 5 more minutes. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.7 Calculation
Average the ratio of the peak area of trifluralin to the internal standard in the two sample solutions and the two standard solutions before and after the sample. The mass fraction of trifluralin W (%) is calculated according to formula (1):ramP
Wherein:
--the average value of the peak area ratio of trifluralin to the internal standard in the standard solution;r2--the average value of the peak area ratio of trifluralin to the internal standard in the sample solution:mi~the mass of the standard sample, in grams (g);m2the mass of the sample, in grams (g);
Pthe mass fraction of trifluralin in the standard sample, expressed in %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.5%. Take the arithmetic mean as the determination result. 4.4 Determination of mass fraction of N,N-nitrosodipropylamine 4.4.1 Summary of the method
Note: N,N-nitrosodipropylamine is a potent carcinogen. Avoid contact during operation! 4
HG3701-2002
The sample is dissolved in n-hexane, placed in a silica gel column and eluted with toluene to separate trifluralin. N,N-nitrosodipropylamine is then eluted with isopropanol. The N,N-nitrosodipropylamine in the isopropanol eluent is separated by gas chromatography using a capillary column and a nitrogen-phosphorus detector, and quantified by the external standard method.
4.4.2 Reagents and solutions
N-hexane.
Toluene.
Isopropanol.
Anhydrous ethanol.
N,N-nitrosodipropylamine standard sample: known mass fraction greater than or equal to 90%. Capillary quartz column: MEGABORECARBOWAX, 30mX0.53mm(id), film thickness 1.2μm. Silica gel cartridge: WATERS51900.
4.4.3 Apparatus
Gas chromatograph: with nitrogen-phosphorus detector.
Chromatographic data processor.
Glass concentrator: 10mL with scale.
KD steaming flask: 500mL
Glass syringe: 10mL with scale.
Condenser: spherical distillation column.
Constant temperature water bath.
4.4.4 Gas chromatographic operating conditions
Temperature (℃): Column chamber 140 for 8min, then heated to 230 at 40/min, vaporization chamber 200, detector chamber 200. Gas flow rate (mL/min): carrier gas (Hea) 20, hydrogen 50, air 500. Current (pA): 30~40.
Injection volume (uL): 1.0.
Retention time (min), N,N-di-n-propylnitrosamine 4.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of N,N-di-n-propylnitrosamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes by less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then add 5 minutes more. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.N-nitrosodipropylamine is a potent tumorigenic substance. Avoid contact during operation! 4
HG3701-2002
The sample is dissolved in n-hexane, placed in a silica gel column and eluted with toluene to separate trifluralin, and then N, N-nitrosodipropylamine is eluted with isopropanol. The N, N-nitrosodipropylamine in the isopropanol eluent is separated by gas chromatography using a capillary column and a nitrogen-phosphorus detector, and quantified by the external standard method.
4.4.2 Reagents and solutions
N-nitrosodipropylamine.
Toluene.
Isopropanol.
Absolute ethanol.
Standard sample of N, N-nitrosodipropylamine: known mass fraction greater than or equal to 90%. Capillary quartz column: MEGABORECARBOWAX, 30mX0.53mm(id), film thickness 1.2μm. Silica gel cartridge: WATERS51900.
4.4.3 Instruments
Gas chromatograph: with nitrogen-phosphorus detector.
Chromatographic data processor.
Glass concentrator: 10mL with scale.
KD steaming flask: 500mL
Glass syringe: 10mL with scale.
Condenser: spherical distillation column.
Constant temperature water bath.
4.4.4 Gas chromatography operating conditions
Temperature (℃): Column chamber 140, maintained for 8min, then heated to 230 at 40/min, vaporization chamber 200, detector chamber 200. Gas flow rate (mL/min): carrier gas (Hea) 20, hydrogen 50, air 500. Current (pA): 30~40.
Injection volume (uL): 1.0.
Retention time (min), N,N-nitrosodipropylamine 4.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of N,N-nitrosodipropylamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes by less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then add 5 minutes more. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.N-nitrosodipropylamine is a potent tumorigenic substance. Avoid contact during operation! 4
HG3701-2002
The sample is dissolved in n-hexane, placed in a silica gel column and eluted with toluene to separate trifluralin, and then N, N-nitrosodipropylamine is eluted with isopropanol. The N, N-nitrosodipropylamine in the isopropanol eluent is separated by gas chromatography using a capillary column and a nitrogen-phosphorus detector, and quantified by the external standard method.
4.4.2 Reagents and solutions
N-nitrosodipropylamine.
Toluene.
Isopropanol.
Absolute ethanol.
Standard sample of N, N-nitrosodipropylamine: known mass fraction greater than or equal to 90%. Capillary quartz column: MEGABORECARBOWAX, 30mX0.53mm(id), film thickness 1.2μm. Silica gel cartridge: WATERS51900.
4.4.3 Instruments
Gas chromatograph: with nitrogen-phosphorus detector.
Chromatographic data processor.
Glass concentrator: 10mL with scale.
KD steaming flask: 500mL
Glass syringe: 10mL with scale.
Condenser: spherical distillation column.
Constant temperature water bath.
4.4.4 Gas chromatography operating conditions
Temperature (℃): Column chamber 140, maintained for 8min, then heated to 230 at 40/min, vaporization chamber 200, detector chamber 200. Gas flow rate (mL/min): carrier gas (Hea) 20, hydrogen 50, air 500. Current (pA): 30~40.
Injection volume (uL): 1.0.
Retention time (min), N,N-nitrosodipropylamine 4.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of N,N-nitrosodipropylamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes by less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then extract for 5 more minutes. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The gas chromatogram of N,N-di-n-propylnitrosamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then extract for 5 more minutes. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.2. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best results. The gas chromatogram of N,N-di-n-propylnitrosamine is shown in Figure 3. The KD concentrator device diagram is shown in Figure 4. 1—Solvent; 2—N,N-di-n-propylnitrosamine; 3—Impurity Figure 3 Gas chromatogram of N,N-di-n-propylnitrosamine (103)
HG3701—2002
4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
1—Condenser tube: 2—Dimensional flask: 3—Constant temperature water bath: 4—KD steaming flask Figure 4 KD concentrator device diagram
Weigh 0.005g (accurate to 0.00002g) of N,N-di-n-propylnitrosamine standard sample, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. Use a pipette to transfer 2mL of the above solution, place it in a 100mL volumetric flask, dilute it to the mark with ethanol, and shake it well. 4.4.5.2 Preparation of sample solution
Connect the silica gel column to a 10mL glass syringe, fix the glass syringe on a burette stand, and use 15mL of n-hexane to elute and balance the silica gel column. Weigh 0.5g of the sample (accurate to 0.0002g), place it in a small beaker, add 10mL of n-hexane to dissolve it, transfer it to the syringe, pressurize the solution to pass through the silica gel column at a flow rate of 1mL/min to 2mL/min, and discard the effluent. Rinse the inner wall and syringe plug of the syringe with 2×2mL of n-hexane, wash and press out the silica gel column, add 7mL of toluene and filter at the same speed. When halfway through, rinse the trifluralin outside the silica gel column with 1mL of toluene, and discard the effluent. Add 5mL of isopropanol at the same speed, pass through the silica gel column, collect the N,N-di-n-propyl nitrosamine isopropanol solution into a graduated concentrator tube pre-added with 20mL of ethanol, add two pieces of zeolite into the graduated concentrator tube, connect it to the KD flask glass concentrator, connect the exhaust device, concentrate it to about 9mL in an 85℃ water bath, cool it to room temperature, add 10mL, and mix it evenly. 4.4.5.3 Determination
Under the above operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution, calculate the repeatability of the corresponding value of each needle, and when the relative response value of two adjacent needles changes by less than 10%, determine it in the order of standard solution, sample solution, sample solution, and standard solution.
4.4.6 Calculation
Average the peak areas of N,N-di-n-propyl nitrosamine in the two needles of sample solution and the two needles of standard solution before and after the sample.
The mass fraction of NN-nitrosodipropylamine wz (mg/kg) is calculated according to formula (2): AgmP×20
Wherein:
A The average value of the peak area of NN-nitrosodipropylamine in the standard solution; A2--The average value of the peak area of N,N-nitrosodipropylamine in the sample solution; mN,N-nitrosodipropylamine standard sample mass, in grams (g); m2--The mass of the sample, in grams (g); P The mass fraction of N,N-nitrosodipropylamine in the standard sample, expressed in % 20-Conversion factor.
4.5 Determination of the mass fraction of acetone insoluble matter
4.5.1 Instruments and reagents
Acetone.
Glass sand core crucible: G3.
Suction filter bottle: 500mL.
Thermostatic oven: 105℃±2℃.
4.5.2 Determination steps
HG3701-2002
Wash and dry the G3 glass crucible to constant weight (accurate to 0.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix evenly, transfer all to a vacuum filter, wash the crucible with 60mL acetone three times, and then add 5 minutes more. Remove and place in a thermostatic oven to dry to constant weight (accurate to 0.0002g). 4.5.3 Calculate
The mass fraction (%) of acetone insoluble matter shall be calculated according to formula (3): Us
Wherein:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of trifluralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical should be packaged in clean, dry, solid steel drums with protective coating. The net content of each drum is 50kg, 100kg or 200kg.5.3 Other forms of packaging can be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold occurs, seek medical treatment in time. 5.7 Acceptance period: Acceptance should be completed within one month from the date of delivery.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix well, transfer all to a beaker, filter under vacuum, wash the crucible with 60mL acetone three times, and then filter for 5 more minutes. Remove and place in a constant temperature oven to dry until constant weight (accurate to 0.0002g). 4.5.3 Calculate the mass fraction (%) of acetone insoluble matter, according to formula (3): Us
Where:
m-mox100wwW.bzxz.Net
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of the acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of Fluoralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical shall be packaged in clean, dry, solid steel drums with protective coating inside, with net content of 50kg, 100kg and 200kg per drum5.3 Other forms of packaging may be used according to user requirements or ordering agreement, but they shall comply with the provisions of GB3796. 5.4 Packages shall be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight, do not mix with food, seeds and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold is found, consult a doctor in time. 5.7 Acceptance period: Acceptance shall be completed within one month from the date of delivery.0002g), weigh 10g (accurate to 0.1g) of sample in a beaker, add 50mL acetone, mix well, transfer all to a beaker, filter under vacuum, wash the crucible with 60mL acetone three times, and then filter for 5 more minutes. Remove and place in a constant temperature oven to dry until constant weight (accurate to 0.0002g). 4.5.3 Calculate the mass fraction (%) of acetone insoluble matter, according to formula (3): Us
Where:
m-mox100
The mass of the sand core crucible after constant weight, in grams (g), mi—--The mass of the acetone insoluble matter after constant weight, in grams (g); m—The mass of the sample, in grams (g). 4.6 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of Fluoralin technical shall comply with the provisions of GB3796. (3)
5.2 Fluoralin technical shall be packaged in clean, dry, solid steel drums with protective coating inside, with net content of 50kg, 100kg and 200kg per drum5.3 Other forms of packaging may be used according to user requirements or ordering agreement, but they shall comply with the provisions of GB3796. 5.4 Packages shall be stored in ventilated and dry warehouses. 5.5 During storage and transportation, prevent moisture and sunlight, do not mix with food, seeds and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Fluoralin is of low toxicity. Wear protective gloves when using this product. Prevent inhalation through the mouth and nose. After the skin or exposed parts of the body come into contact with this product, they should be washed with soap and water in time. If mold is found, consult a doctor in time. 5.7 Acceptance period: Acceptance shall be completed within one month from the date of delivery.
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