Some standard content:
GB18171-2000
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. In terms of standard composition and writing format, this standard follows GB/T1.1-1993 "Guidelines for Standardization Work Unit 1: Rules for Drafting and Presentation of Standards Part 1: Basic Regulations for Standard Writing" and HG/T2467.5-1996 "Specifications for Writing Standards for Pesticide Aqueous Suspension Concentrates", and adopts FAO standards in terms of technical content. Appendix A of this standard is the appendix of the standard.
This standard is proposed by the State Administration of Petroleum and Chemical Industry of the People's Republic of China. This standard is technically managed by Shenyang Chemical Research Institute. This standard is interpreted by the Secretariat of the National Pesticide Standardization Technical Committee. The responsible drafting units of this standard are: Shenyang Chemical Research Institute, Jiangyin Ligang Fine Chemical Factory, Jiangsu Province. The main drafters of this standard are: Xing Hong, Miao Jinfeng, Wang Xiaojun, and Wang Yufan. 661
National Standard of the People's Republic of China
Chlorothalonil aqueous suspension concentratesOther names, structural formulas and basic physicochemical parameters of the active ingredient chlorothalonil in this product are as follows:ISO common name: Chlorothalonil
CIPAC digital code: 288
Chemical name: 2,4,5,6-tetrachloro-1,3-dicyanobenzeneStructural formula:
Empirical formula: C.Cl.Nz
Relative molecular mass: 265.91 (according to the 1997 international relative atomic mass)Biological activity: bactericidal
Melting point: 250℃~251℃| |tt||Boiling point: 350℃
Vapor pressure (40C): <1.33×10-3PaGB18171--2000
Solubility (g/L, 25℃): 6×10-4 in water, 80 in xylene, 2 in acetone, 30 in cyclohexanone, dimethylformamide, ≤10 in keroseneStability: Stable under normal storage conditions, stable to light, stable in weak acid and weak alkali media; decomposes in strong alkali media1Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of 40% chlorothalonil suspension. This standard is applicable to 40% chlorothalonil suspension made from chlorothalonil technical material, fillers and suitable additives that meet the standard GB9551.
2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard was published, the versions shown were all valid. All standards are subject to revision and parties using this standard should investigate the possibility of using the most recent versions of the following standards. GB/T1601—1993 Determination of pH value of pesticides GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605—1979 (1989) Sampling methods for commercial pesticides GB 3796--1999
9 General rules for pesticide packaging
GB 9551—1999
Chlorothalonil technical
3 Determination of suspension rate of wettable powders of pesticides GB/T 14825—1993
GB/T 16150---1995
Determination of fineness of pesticide powders and wettable powders Approved by the State Administration of Quality and Technical Supervision on July 31, 2000 662
Implemented on March 1, 2001
3 Requirements
GB 18171—2000
3.1 Appearance: It should be a flowing, easily measurable suspension liquid; during storage, precipitation may occur, but it should return to its original state after being shaken by hand; there should be no lumps.
3.240% chlorothalonil suspension concentrate should meet the requirements of Table 1. Table 1 Control Items and Indicators of Chlorothalonil Suspension Concentrate
Chlorothalonil content, %
Hexachlorobenzene content, %
pH range
Pourability
Suspension rate, %
Residue after pouring, %
Residue after washing, %
Sieve analysis (through 44 μm test sieve), %
Persistent foam volume (placed for 1 min), mL
Low temperature stability
Hot storage stability
1 Hexachlorobenzene and pourability are tested only once when the raw materials remain unchanged. 2 Under normal circumstances, the low temperature stability and heat storage stability tests shall be conducted at least once every three months. 4 Test methods
4.1 Sampling
The sampling method for emulsions and liquids in GB/T1605-1979 (1989) shall be followed. The sampling packages shall be determined by the random number table method; the final sampling volume shall be no less than 250 mL. 4.2 Identification test
Gas chromatography method The identification test can be conducted simultaneously with the determination of the content of chlorothalonil. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak of the sample solution and the retention time of the chlorothalonil chromatographic peak in the standard solution shall be within 1.5%. When there is doubt about the identification of the active ingredient using the above method, other effective methods can be used for identification. 4.3 Chlorothalonil Determination of the content of thiophanate-methyl
4.3.1 Method Summary
The sample is dissolved in xylene, and o-diphenylbenzene is used as the internal standard. A glass column (or stainless steel column) filled with 5% OV-17+1.1% OV-225/ChromosorbWAW-DMCS and a hydrogen flame ionization detector are used to separate and determine the thiophanate-methyl in the sample by gas chromatography.
4.3.2 Reagents and solutions
a) Xylene: should not contain impurities that interfere with the analysis; b) Chlorothalonil standard sample: known content, ≥99.0%; c) Internal standard: o-diphenylbenzene, should not contain impurities that interfere with the analysis; d) Stationary liquid: Silicone OV-17, Silicone OV-225; e) Carrier: Chromosorb W AW-DMCS, 150 μm~180 μm; f) Internal standard solution: weigh 3.3 g of o-diphenylbenzene in a 1000 mL volumetric flask, dissolve it in xylene and dilute to the mark, shake well. 4.3.3 Instruments
GB 18171--2000
a) Gas chromatograph: with hydrogen flame ionization detector FID; b) Chromatographic data processor;
c) Chromatographic column: 4 mm (id) × 2 m glass column (or stainless steel column); d) Column filling: 5% OV-17 + 1.1% OV-225 coated on Chromosorb W AW-DMCS (150 μm-~180 μm), OV-17+OV-225+carrier=5.0+1.1+93.9; e) Micro syringe: 10μl.
4.3.4 Preparation of chromatographic column
4.3.4.1 Coating of stationary liquid
Weigh 1.25g OV-17 and 0.25g OV-225 in a 100mL beaker, add appropriate amount of acetone to completely dissolve. Weigh 23.5g Chromosorb W AW-DMCS (150 μm~180 um) into a beaker and shake it so that the solution just covers the carrier. Place the beaker in a 50℃ water bath to evaporate the solvent, then place the beaker in a 110℃ oven for 1h. 4.3.4.2 Filling of the 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 1.5cm 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 filled evenly and tightly. After filling, also plug a small ball of glass wool at the inlet end and press it appropriately to prevent the column filler from moving. 4.3.4.3 Aging of the chromatographic column
Connect the inlet of the chromatographic column to the vaporizer, and do not connect the outlet to the detector for the time being. Pass the carrier gas (N2) at a flow rate of 20mL/min, raise the temperature to 240℃ in stages, and age at this temperature for at least 48h. Then connect the outlet to the detector. 4.3.5 Gas chromatography operating conditions
a) Temperature (C): column temperature 195, vaporizer 280, detector chamber 280; b) Gas flow (mL/min): carrier gas (Nz) 50, hydrogen 50, air 600; c) Injection volume (μL): 2.0;
d) Relative retention value (min):
1) Thiophanate: 1.30;
2) Tetrachloroterephthalonitrile: 1.16;
3) o-diphenylbenzene: 1.00.
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. A typical gas chromatogram of 40% chlorothalonil suspension is shown in Figure 1. 1-o-diphenylbenzene; 2-tetrachloroterephthalonitrile; 3-chlorothalonil Figure 1 Gas chromatogram of chlorothalonil suspension
4.3.6 Determination steps
4.3.6.1 Preparation of standard solution
GB 18171--2000
Weigh 0.10g (accurate to 0.0002g) of chlorothalonil standard sample and place it in a stoppered glass bottle. Use a pipette to transfer 10mL of internal standard solution, then add appropriate amount of xylene to dissolve and dilute the chlorothalonil standard sample and shake well. 4.3.6.2 Preparation of sample solution
Weigh a sample containing 0.10g of chlorothalonil (accurate to 0.0002g) and place it in a stoppered glass bottle. Use the same pipette as in 4.3.6.1 to transfer 10mL of internal standard solution, then add an appropriate amount of xylene to dissolve and dilute the chlorothalonil standard sample, and shake to mix. 4.3.6.3 Determination
Under the above operating conditions, after the instrument is stable, continuously inject several injections of standard solution until the relative change of the ratio of the peak area of chlorothalonil to the peak area of the internal standard between two adjacent injections is less than 1.0%, and then analyze 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 chlorothalonil to the internal standard in the two injections of sample solution and the two injections of standard solution before and after the sample. The thiophanate-methyl content X, expressed as mass fraction (%), is calculated according to formula (1): Xi
wherein: Xi—the average value of the peak areas of thiophanate-methyl and internal standard in the standard solution; Y2—the average value of the peak areas of thiophanate-methyl and internal standard in the test solution; m—the mass of the standard sample, g;
the mass of the test sample, g;
P—the mass fraction of thiophanate-methyl in the standard sample, %. 4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 0.8%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of Hexachlorobenzene Content
4.4.1 High Performance Liquid Chromatography (Arbitration Method)4.4.1.1 Summary of Method
(1)
The sample was dissolved in acetonitrile, and methanol was used as the mobile phase. ODS (C18), 5μm stainless steel column as filler and UV detector (254nm) were used to separate and determine the hexachlorobenzene in the sample by reverse phase high performance liquid chromatography, and the external standard method was used for quantification. 4.4.1.2 Reagents and Solutions
a) Methanol: chromatographically pure;
b) Acetonitrile: chromatographically pure;
c) Mobile phase: Methanol was filtered through a 0.45μm pore size filter membrane, and degassed in an ultrasonic bath for 10 minutes, then sealed in a dark bottle and stored at low temperature.
d) Hexachlorobenzene standard: known content, ≥99.0%. 4.4.1.3 Instruments
a) HPLC: UV detector with wavelength of 254nm; b) Chromatographic column: 150mmX4.6mm(id) stainless steel column, filled with ODS(C18), particle size 5μm; c) Chromatographic data processor;
d) Injector: 50 μL;
e) Filter: pore size of filter membrane is about 0.45μm. 4.4.1.4 HPLC operating conditions
a) Mobile phase: methanol;
b) Flow rate: 1.5mL/min;
c) Column temperature: 20C～35℃ (temperature change should be less than 2℃); 665
d) Detection wavelength: 254nm;
e) Injection volume: 10 uL;
f) Retention time: 7.4min for hexachlorobenzene.
GB 18171—-2000
The above operating conditions are typical. According to the characteristics of different instruments, the chromatographic column (using C18 type liquid chromatography column) and the given operating conditions can be appropriately adjusted to obtain the best effect. The typical HPLC chromatogram of hexachlorobenzene in 40% chlorothalonil suspension is shown in Figure 2. 1—chlorothalonil; 2—hexachlorobenzene
Figure 2 HPLC chromatogram of hexachlorobenzene in chlorothalonil suspension 4.4.1.5 Determination steps
a) Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of hexachlorobenzene standard sample, place it in a 250mL clean and dry volumetric flask, dilute to the scale with acetonitrile, and shake well. Use a pipette to transfer 2mL to a 50mL volumetric flask and dilute to the scale with acetonitrile, shake well. Filter with a 0.45μm pore size filter membrane and store in a sealed container.
b) Preparation of sample solution
Weigh a sample containing 0.10g (accurate to 0.0002g) of thiophanate-methyl, dissolve it in acetonitrile and dilute it to the mark in a 10mL clean volumetric flask, shake it for 5min, and filter it with a 0.45μm pore size filter membrane. c) Determination
Under the above chromatographic operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the peak area change between two adjacent needles is less than 1.5%, and then determine it in the order of standard solution, sample solution, sample solution, and standard solution. d) Calculation
Average the peak areas of hexazobenzene in the two sample solutions and the two standard solutions before and after the sample. The content of hexachlorobenzene expressed as mass fraction X, (%) is calculated according to formula (2): AzmP
625XAjm2
Wherein: A——average value of hexachlorobenzene peak area in standard solution; A2-average value of hexachlorobenzene peak area in sample solution; 666
mass of hexachlorobenzene standard sample·g;
mass of sample, g;
GB 18171-2000
P-mass fraction of hexachlorobenzene in standard sample, %; 625——-ratio of dilution volume of standard solution to sample solution e) Allowable difference
The relative deviation of two parallel determination results shall not exceed ±20%. 4.4.2 Capillary gas chromatography
For capillary gas chromatography, see Appendix A (Standard Appendix). 4.5 Determination of pH value
Carry out according to GB/T1601.
4.6 Pourability Test
4.6.1 Method Summary
After placing the suspension sample in the container for a certain period of time, pour it according to the prescribed procedure and measure the amount of sample retained in the container; after washing the container with water, measure the amount of sample in the container again. 4.6.2 Instrument
Volume cylinder with ground stopper: 500mL±2mlL; the height of the volume cylinder is 39cm, and the distance between the upper and lower scales is 25cm (or other equivalent containers suitable for measuring pourability).
4.6.3 Test Steps
Mix a sufficient amount of sample and promptly place a part of it in the weighed volume cylinder (including the stopper) to 8/10 of the volume of the volume cylinder, plug the ground stopper, weigh it, and leave it for 2h. Open the stopper, tilt the inverted measuring cylinder 45, pour it for 60s, and then invert it for 60s. Reweigh the volume cylinder and stopper. Pour water (20℃) equivalent to 80% of the volume of the measuring cylinder into the measuring cylinder, plug the ground stopper, turn the measuring cylinder upside down 10 times with the bottom of the measuring cylinder as the center, pour out the contents according to the above operation, and weigh the measuring cylinder and stopper again. 4.6.4 Calculate the residue X3-1 (%) after pouring and the residue X3-2 (%) after washing according to formula (3-1) and formula (3-2) respectively: mg = mo × 100
X3-1 (%) -
ms = mo × 100
X3-2 (%) =
Where: m is the mass of the measuring cylinder, ground stopper and sample, g; m2 is the mass of the measuring cylinder, ground stopper and residue after the first pouring, g; m3 is the mass of the measuring cylinder, ground stopper and residue after the second pouring (washing and pouring with water), g; m. -—The mass of the measuring cylinder and the ground stopper after constant weight, g. 4.7 Determination of suspension rate
4.7.1 Operation steps
(3-1)
Perform according to GB/T14825. (Weigh 2.0g of the sample, accurate to 0.0002g; transfer the remaining 1/10 suspension and sediment to a 100mL volumetric flask, wash the bottom of the measuring cylinder with 15mL water, and then use the same pipette used to prepare the standard sample to accurately add 10mL of internal standard solution, and then add 30mL of xylene, shake for 10min, let it stand, take the organic phase clear liquid, and determine the mass of thiophanate-methyl according to 4.3.6, and calculate its suspension rate.)
4.7.2 Allowable difference
The difference between the results of two parallel determinations should not be greater than 5%; take the arithmetic mean as the determination result. 4.8 Sieve analysis
Perform according to the wet sieving method in GB/T16150-1995. 667
4.9 Determination of persistent foam volume
4.9.1 Summary of method
GB 18171—2000
Mix the specified amount of sample with standard hard water, let it stand and record the foam volume. 4.9.2 Reagents
Standard hard water: p(Ca2++Mg2)342 mg/L, pH=6.0~～7.0. Prepared according to GB/T 14825. 4.9.3 Apparatus
Measuring cylinder with stopper: 250mL (division value 2mL, 0250mL scale line 20cm~21.5cm, 250mL scale line to the bottom of the stopper 4 cm~6 cm);
Industrial balance: sensitivity 0.1g, range 500g. 4.9.4 Determination steps
Add standard hard water to the 180mL scale line in the measuring cylinder, place the measuring cylinder on the balance, add 1.0g of the sample (accurate to 0.1g), and add hard water to the scale line 9cm away from the bottom of the measuring cylinder stopper. After the stopper is put on, turn the measuring cylinder upside down 30 times (2s each time) with the bottom of the measuring cylinder as the center. Let it stand on the test bench for 1min and record the foam volume.
4.10 Low temperature stability test
4.10.1 Method summary
Keep the sample at 0℃ for 1h, and observe whether the appearance changes. Continue to store at 0℃ for 7d, and test its physical properties. 4.10.2 Apparatus
Refrigerator: 0℃±1℃.
Beaker: 100mL.
4.10.3 Test steps
Put 80mL of the sample in a 100mL beaker, cool it to 0℃±1℃ in a refrigerator, and keep it for 1h. During this period, stir it once every 15min, each time for 15s, and observe whether the appearance changes. Put the beaker back into the refrigerator and continue to place it at 0℃±1℃ for 7d. After 7d, take out the beaker, return it to room temperature, and complete the determination of suspension rate and sieve analysis according to 4.7 and 4.8. The suspension rate and sieve analysis meet the standard requirements and are qualified. 4.11 Hot Storage Stability Test
4.11.1 Apparatus
Thermostatic box (or thermostatic water bath): 54℃±2℃; bottle (or glass bottle with stopper that can still be sealed at 54℃): 50mL; medical syringe: 50mL.
4.11.2 Test Procedure
Use a syringe to inject about 30mL of sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and seal it with a high-temperature flame. Seal at least 3 bottles, weigh them separately, place the sealed bottles in a metal container, and then place the metal container in a thermostatic box (thermostatic water bath) at 54℃±2℃ for 14 days. Take out the bottles, wipe the outside of the bottles clean, and weigh them separately. For the samples that have not changed in mass, complete the determination of appearance, effective content, suspension rate and sieve analysis according to 3.1, 4.3, 4.7, and 4.8 within 24 hours. If the test results and appearance meet the technical requirements of this standard, the heat storage stability of the sample is qualified.
4.12 Inspection and acceptance of products
It shall comply with the provisions of GB/T1604, and the limit value shall be processed by the rounded value comparison method. 5 Marking, labeling, packaging, transportation
5.1 The marking, labeling and packaging of chlorothalonil suspension shall comply with the provisions of GB3796. 5.2 Chlorothalonil suspension shall be packaged in well-sealed plastic bottles, and the net weight of each bottle is 100 kg. The outer packaging shall be corrugated paper boxes or calcium plastic boxes, and the net weight of each box shall not exceed 10 kg.
5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the provisions of GB3796. 5.4 Chlorothalonil suspension packages shall be stored in ventilated and dry warehouses. 668
GB18171—2000
5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: This product is a low-toxic preparation and is irritating to the eyes and skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash it with soap and water immediately. If poisoning occurs, ask a doctor to take rescue measures. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of 40% chlorothalonil suspension is 2 years from the date of production. 669
A1 Method Summary
GB 18171—2000
Appendix A
(Standard Appendix)
Determination of hexachlorobenzene in chlorothalonil by capillary gas chromatography The sample was dissolved in xylene, and the hexachlorobenzene in the sample was separated and determined using a 30m×0.53mm (id) capillary column coated with 1.2μm SE-54 and a hydrogen flame ionization detector. A2 Reagents and Solutions
Toluene: does not contain impurities that interfere with analysis; Hexachlorobenzene standard: known content, ≥99%; Stationary liquid: SE-54.
A2.1 Instruments
Gas chromatograph: Capillary chromatographic column can be used, with splitter, hydrogen flame ionization detector and data processor; Capillary chromatographic column: 30m×0.53mm(id) wall coated with SE-54, liquid film thickness 1.2um; Micro syringe: 5μuL.
A2.2 Gas chromatograph operating conditions
a) Temperature (℃): Detection chamber: 300; Vaporization chamber: 300; Column chamber: 200. b) Gas (kPa): Carrier gas (high purity nitrogen): 40; Air: 50; Hydrogen: 60. c) Split ratio: 70:1.
d) Range: 102.
e) Injection volume: lμL.
f) Retention time (min): Hexachlorobenzene: 8.98; Chlorothalonil: 12.58. The typical chromatogram of the sample under the above gas chromatography operating conditions is shown in Figure A1. 1 Hexachlorobenzene; 2-Chlorothalonil
Gas chromatogram of hexafluorobenzene in chlororothalonil sample The above gas chromatography operating conditions are typical. The given operating parameters can be appropriately adjusted according to the characteristics of different instruments and the requirements of their own conditions in order to obtain the best results. A3 Determination steps
A3.1 Solution preparation
A3.1.1 Hexachlorobenzene standard solution
GB 18171—2000
Accurately weigh 0.05g (accurate to 0.0002g) of hexachlorobenzene standard in a 250mL clean and dry volumetric flask, dissolve it with toluene and dilute it to the scale, and shake it. Take 5ml of the solution in a 100mL volumetric flask, dilute it to the scale with toluene, and shake it. A3.1.2 Sample solution
Accurately weigh 0.45g of sample (accurate to 0.0002g) in a 10mL volumetric flask, dissolve it with toluene and dilute to the mark, shake well. A3.2 Determination
Under the above gas chromatographic operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the peak area change between two adjacent needles is less than 1.5%, and then determine in the order of standard solution, sample solution, sample solution, and standard solution. A3.3 Calculation
Average the peak areas of hexachlorobenzene in the two sample solutions and the two standard solutions before and after the sample. The mass fraction X (%) of hexachlorobenzene is calculated according to formula (A1):
A,m2× 500
Wherein: Awww.bzxz.net
The average value of the peak area of hexachlorobenzene in the standard solution; The average value of the peak area of hexachlorobenzene in the sample solution; The mass of the hexachlorobenzene standard, g;
m2-The mass of the sample, g;
P—The mass fraction of hexafluorobenzene in the standard sample, %; 500—The ratio of the dilution volume of the standard solution to the sample solution. A3.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed ±20%. (Al)8Complete the determination of suspension rate and sieve analysis. Suspension rate and sieve analysis meet the standard requirements and are qualified. 4.11 Hot storage stability test
4.11.1 Apparatus
Constant temperature box (or constant temperature water bath): 54℃±2℃; bottle (or glass bottle with stopper that can still be sealed at 54C): 50mL; medical syringe: 50mL.
4.11.2 Test steps
Use a syringe to inject about 30mL of sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice salt bath to cool, and seal it with a high-temperature flame. Seal at least 3 bottles, weigh them separately, place the sealed ones in a metal container, and then place the metal container in a constant temperature box (constant temperature water bath) at 54℃±2℃ for 14 days. Take out the sample, wipe the outside and weigh it separately. For the sample with no change in mass, complete the test of appearance, effective content, suspension rate and sieve analysis according to 3.1, 4.3, 4.7 and 4.8 within 24 hours. If the test results and appearance meet the technical requirements of this standard, the thermal storage stability of the sample is qualified.
4.12 Inspection and acceptance of products
Should comply with the provisions of GB/T1604, limit numerical processing, and rounded value comparison method. 5 Marking, labeling, packaging, transportation
5.1 The marking, labeling and packaging of chlorothalonil suspension concentrate shall comply with the provisions of GB3796. 5.2 Chlorothalonil suspension concentrate shall be packaged in well-sealed plastic bottles, and the net mass of each bottle is 100 kg. The outer packaging shall be made of corrugated paper boxes or calcium plastic boxes, and the net mass of each box shall not exceed 10 kg.
5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 The packages of chlorothalonil suspension should be stored in a ventilated and dry warehouse. 668
GB18171—2000
5.5 During storage and transportation, strictly 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: This product is a low-toxic preparation and is irritating to the eyes and skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash with soap and water immediately. If poisoning occurs, ask a doctor to take rescue measures. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of 40% chlorothalonil suspension is 2 years from the date of production. 669
A1 Method Summary
GB 18171—2000
Appendix A
(Standard Appendix)
Determination of hexachlorobenzene in chlorothalonil by capillary gas chromatography The sample was dissolved in xylene, and the hexachlorobenzene in the sample was separated and determined using a 30m×0.53mm (id) capillary column coated with 1.2μm SE-54 and a hydrogen flame ionization detector. A2 Reagents and Solutions
Toluene: does not contain impurities that interfere with analysis; Hexachlorobenzene standard: known content, ≥99%; Stationary liquid: SE-54.
A2.1 Instruments
Gas chromatograph: Capillary chromatographic column can be used, with splitter, hydrogen flame ionization detector and data processor; Capillary chromatographic column: 30m×0.53mm(id) wall coated with SE-54, liquid film thickness 1.2um; Micro syringe: 5μuL.
A2.2 Gas chromatograph operating conditions
a) Temperature (℃): Detection chamber: 300; Vaporization chamber: 300; Column chamber: 200. b) Gas (kPa): Carrier gas (high purity nitrogen): 40; Air: 50; Hydrogen: 60. c) Split ratio: 70:1.
d) Range: 102.
e) Injection volume: lμL.
f) Retention time (min): Hexachlorobenzene: 8.98; Chlorothalonil: 12.58. The typical chromatogram of the sample under the above gas chromatography operating conditions is shown in Figure A1. 1 Hexachlorobenzene; 2-Chlorothalonil
Gas chromatogram of hexafluorobenzene in chlororothalonil sample The above gas chromatography operating conditions are typical. The given operating parameters can be appropriately adjusted according to the characteristics of different instruments and the requirements of their own conditions in order to obtain the best results. A3 Determination steps
A3.1 Solution preparation
A3.1.1 Hexachlorobenzene standard solution
GB 18171—2000
Accurately weigh 0.05g (accurate to 0.0002g) of hexachlorobenzene standard in a 250mL clean and dry volumetric flask, dissolve it with toluene and dilute it to the scale, and shake it. Take 5ml of the solution in a 100mL volumetric flask, dilute it to the scale with toluene, and shake it. A3.1.2 Sample solution
Accurately weigh 0.45g of sample (accurate to 0.0002g) in a 10mL volumetric flask, dissolve it with toluene and dilute to the mark, shake well. A3.2 Determination
Under the above gas chromatographic operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the peak area change between two adjacent needles is less than 1.5%, and then determine in the order of standard solution, sample solution, sample solution, and standard solution. A3.3 Calculation
Average the peak areas of hexachlorobenzene in the two sample solutions and the two standard solutions before and after the sample. The mass fraction X (%) of hexachlorobenzene is calculated according to formula (A1):
A,m2× 500
Wherein: A
The average value of the peak area of hexachlorobenzene in the standard solution; The average value of the peak area of hexachlorobenzene in the sample solution; The mass of the hexachlorobenzene standard, g;
m2-The mass of the sample, g;
P—The mass fraction of hexafluorobenzene in the standard sample, %; 500—The ratio of the dilution volume of the standard solution to the sample solution. A3.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed ±20%. (Al)8Complete the determination of suspension rate and sieve analysis. Suspension rate and sieve analysis meet the standard requirements and are qualified. 4.11 Hot storage stability test
4.11.1 Apparatus
Constant temperature box (or constant temperature water bath): 54℃±2℃; bottle (or glass bottle with stopper that can still be sealed at 54C): 50mL; medical syringe: 50mL.
4.11.2 Test steps
Use a syringe to inject about 30mL of sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice salt bath to cool, and seal it with a high-temperature flame. Seal at least 3 bottles, weigh them separately, place the sealed ones in a metal container, and then place the metal container in a constant temperature box (constant temperature water bath) at 54℃±2℃ for 14 days. Take out the sample, wipe the outside and weigh it separately. For the sample with no change in mass, complete the test of appearance, effective content, suspension rate and sieve analysis according to 3.1, 4.3, 4.7 and 4.8 within 24 hours. If the test results and appearance meet the technical requirements of this standard, the thermal storage stability of the sample is qualified.
4.12 Inspection and acceptance of products
Should comply with the provisions of GB/T1604, limit numerical processing, and rounded value comparison method. 5 Marking, labeling, packaging, transportation
5.1 The marking, labeling and packaging of chlorothalonil suspension concentrate shall comply with the provisions of GB3796. 5.2 Chlorothalonil suspension concentrate shall be packaged in well-sealed plastic bottles, and the net mass of each bottle is 100 kg. The outer packaging shall be made of corrugated paper boxes or calcium plastic boxes, and the net mass of each box shall not exceed 10 kg.
5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 The packages of chlorothalonil suspension should be stored in a ventilated and dry warehouse. 668
GB18171—2000
5.5 During storage and transportation, strictly 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: This product is a low-toxic preparation and is irritating to the eyes and skin. When using this product, you should wear protective gloves, masks, and clean protective clothing. After use, wash with soap and water immediately. If poisoning occurs, ask a doctor to take rescue measures. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of 40% chlorothalonil suspension is 2 years from the date of production. 669
A1 Method Summary
GB 18171—2000
Appendix A
(Standard Appendix)
Determination of hexachlorobenzene in chlorothalonil by capillary gas chromatography The sample was dissolved in xylene, and the hexachlorobenzene in the sample was separated and determined using a 30m×0.53mm (id) capillary column coated with 1.2μm SE-54 and a hydrogen flame ionization detector. A2 Reagents and Solutions
Toluene: does not contain impurities that interfere with analysis; Hexachlorobenzene standard: known content, ≥99%; Stationary liquid: SE-54.
A2.1 Instruments
Gas chromatograph: Capillary chromatographic column can be used, with splitter, hydrogen flame ionization detector and data processor; Capillary chromatographic column: 30m×0.53mm(id) wall coated with SE-54, liquid film thickness 1.2um; Micro syringe: 5μuL.
A2.2 Gas chromatograph operating conditions
a) Temperature (℃): Detection chamber: 300; Vaporization chamber: 300; Column chamber: 200. b) Gas (kPa): Carrier gas (high purity nitrogen): 40; Air: 50; Hydrogen: 60. c) Split ratio: 70:1.
d) Range: 102.
e) Injection volume: lμL.
f) Retention time (min): Hexachlorobenzene: 8.98; Chlorothalonil: 12.58. The typical chromatogram of the sample under the above gas chromatography operating conditions is shown in Figure A1. 1 Hexachlorobenzene; 2-Chlorothalonil
Gas chromatogram of hexafluorobenzene in chlororothalonil sample The above gas chromatography operating conditions are typical. The given operating parameters can be appropriately adjusted according to the characteristics of different instruments and the requirements of their own conditions in order to obtain the best results. A3 Determination steps
A3.1 Solution preparation
A3.1.1 Hexachlorobenzene standard solution
GB 18171—2000
Accurately weigh 0.05g (accurate to 0.0002g) of hexachlorobenzene standard in a 250mL clean and dry volumetric flask, dissolve it with toluene and dilute it to the scale, and shake it. Take 5ml of the solution in a 100mL volumetric flask, dilute it to the scale with toluene, and shake it. A3.1.2 Sample solution
Accurately weigh 0.45g of sample (accurate to 0.0002g) in a 10mL volumetric flask, dissolve it with toluene and dilute to the mark, shake well. A3.2 Determination
Under the above gas chromatographic operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the peak area change between two adjacent needles is less than 1.5%, and then determine in the order of standard solution, sample solution, sample solution, and standard solution. A3.3 Calculation
Average the peak areas of hexachlorobenzene in the two sample solutions and the two standard solutions before and after the sample. The mass fraction X (%) of hexachlorobenzene is calculated according to formula (A1):
A,m2× 500
Wherein: A
The average value of the peak area of hexachlorobenzene in the standard solution; The average value of the peak area of hexachlorobenzene in the sample solution; The mass of the hexachlorobenzene standard, g;
m2-The mass of the sample, g;
P—The mass fraction of hexafluorobenzene in the standard sample, %; 500—The ratio of the dilution volume of the standard solution to the sample solution. A3.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed ±20%. (Al)2 Gas chromatograph operating conditions
a) Temperature (℃): detection chamber: 300; vaporization chamber: 300; column chamber: 200. b) Gas (kPa): carrier gas (high purity nitrogen): 40; air: 50; hydrogen: 60. c) Split ratio: 70:1.
d) Range: 102.
e) Injection volume: lμL.
f) Retention time (min): hexachlorobenzene: 8.98; chlorothalonil: 12.58. The typical chromatogram of the sample under the above gas chromatographic operating conditions is shown in Figure A1. 1 Hexachlorobenzene; 2-chlorothalonil
Gas chromatogram of hexafluorobenzene in chlorothalonil sample The above gas chromatographic operating conditions are typical. The given operating parameters can be appropriately adjusted according to the characteristics of different instruments and the requirements of their own conditions in order to obtain the best results. A3 Determination steps
A3.1 Solution preparation
A3.1.1 Hexachlorobenzene standard solution
GB 18171—2000
Accurately weigh 0.05g (accurate to 0.0002g) of hexachlorobenzene standard in a 250mL clean and dry volumetric flask, dissolve and dilute to the mark with toluene, and shake to hook. Take 5ml of the solution in a 100mL volumetric flask, dilute to the mark with toluene, and shake to hook. A3.1.2 Sample solution
Accurately weigh 0.45g of sample (accurate to 0.0002g) in a 10mL volumetric flask, dissolve and dilute to the mark with toluene, and shake to mix. A3.2 Determination
Under the above gas chromatography operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the peak area change between two adjacent needles is less than 1.5%, and then determine in the order of standard solution, sample solution, sample solution, and standard solution. A3.3 Calculation
Average the peak areas of hexachlorobenzene in the two sample solutions and the two standard solutions before and after the sample. The mass fraction X (%) of hexachlorobenzene is calculated according to formula (A1):
A,m2× 500
Where: A
The average value of the peak area of hexachlorobenzene in the standard solution; The average value of the peak area of hexachlorobenzene in the sample solution; The mass of the hexachlorobenzene standard, g;
m2-The mass of the sample, g;
P-The mass fraction of hexafluorobenzene in the standard sample, %; 500-The ratio of the dilution volume of the standard solution to the sample solution. A3.4 Allowable difference
The relative deviation of two parallel determination results should not exceed ±20%. (Al)2 Gas chromatograph operating conditions
a) Temperature (℃): detection chamber: 300; vaporization chamber: 300; column chamber: 200. b) Gas (kPa): carrier gas (high purity nitrogen): 40; air: 50; hydrogen: 60. c) Split ratio: 70:1.
d) Range: 102.
e) Injection volume: lμL.
f) Retention time (min): hexachlorobenzene: 8.98; chlorothalonil: 12.58. The typical chromatogram of the sample under the above gas chromatographic operating conditions is shown in Figure A1. 1 Hexachlorobenzene; 2-chlorothalonil
Gas chromatogram of hexafluorobenzene in chlorothalonil sample The above gas chromatographic operating conditions are typical. The given operating parameters can be appropriately adjusted according to the characteristics of different instruments and the requirements of their own conditions in order to obtain the best results. A3 Determination steps
A3.1 Solution preparation
A3.1.1 Hexachlorobenzene standard solution
GB 18171—2000
Accurately weigh 0.05g (accurate to 0.0002g) of hexachlorobenzene standard in a 250mL clean and dry volumetric flask, dissolve and dilute to the mark with toluene, and shake to hook. Take 5ml of the solution in a 100mL volumetric flask, dilute to the mark with toluene, and shake to hook. A3.1.2 Sample solution
Accurately weigh 0.45g of sample (accurate to 0.0002g) in a 10mL volumetric flask, dissolve and dilute to the mark with toluene, and shake to mix. A3.2 Determination
Under the above gas chromatography operating conditions, after the instrument baseline is stable, continuously inject several needles of standard solution until the peak area change between two adjacent needles is less than 1.5%, and then determine in the order of standard solution, sample solution, sample solution, and standard solution. A3.3 Calculation
Average the peak areas of hexachlorobenzene in the two sample solutions and the two standard solutions before and after the sample. The mass fraction X (%) of hexachlorobenzene is calculated according to formula (A1):
A,m2× 500
Where: A
The average value of the peak area of hexachlorobenzene in the standard solution; The average value of the peak area of hexachlorobenzene in the sample solution; The mass of the hexachlorobenzene standard, g;
m2-The mass of the sample, g;
P-The mass fraction of hexafluorobenzene in the standard sample, %; 500-The ratio of the dilution volume of the standard solution to the sample solution. A3.4 Allowable difference
The relative deviation of two parallel determination results should not exceed ±20%. (Al)
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