Some standard content:
GB 334--2001
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. Introduction
This standard is a revision of the mandatory national standard GB334-1981 (1989) "Trichlorfon Powder". The main differences between this standard and GB334-1981 (1989) are as follows: 1. In this revision, the original refined product is changed to superior product. Considering the actual domestic production and use situation, the original first-class product is temporarily retained as a qualified product.
2. The moisture index of superior product is changed from 0.4% to 0.3%. 3. The acidity index of qualified product is relaxed from 1.5% to 1.8%. 4. Add the moisture index of qualified product.
5. Add the index of acetone insoluble matter.
6. For the determination method of trichlorfon content, the original potentiometric titration method is deleted and high performance liquid chromatography is added as the arbitration method. 7. The warranty period has been added.
This standard replaces GB334-1981 (1989) from the date of entry into force. This standard is proposed by the State Bureau of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Technical Committee for Standardization of Pesticides. The responsible drafting unit of this standard is Shenyang Chemical Research Institute. The participating drafting units of this standard are Shandong Dacheng Pesticide Co., Ltd. and Hunan Nantian Industrial Co., Ltd. The main drafters of this standard are Ma Yaguang, Xing Jun, Wang Baojie, Xiao Dongliang and Xing Zhaowu. This standard was first issued in 1964 and revised for the first time in 1981. This standard is the second revision.
The Secretariat of the National Technical Committee for Standardization of Pesticides is entrusted with the responsibility for the interpretation of this standard. 470
National Standard of the People's Republic of China
Trichlorfon technical
Trichlorfon technical
Other names, structural formulas and basic physicochemical parameters of trichlorfon are as follows: ISO common name: Trichlorfon
CIPAC digital code: 68
Chemical name: 0,0-dimethyl-(2,2,2-trichloro-1-hydroxyethyl)phosphonate Structural formula:
Empirical formula: C,H.Cl,O,P
CHO O OH
CH-—CCl3
Relative molecular mass: 257.4 (according to the 1997 international relative atomic mass) Biological activity: insecticide
Melting point: 83℃~84℃
Vapor pressure: 0.21MPa (20℃)
GB334--2001
Replaces GB334—1981(1989)
Solubility (g/L, 20C): Solubility in water is 120, soluble in benzene, ethanol and most chlorinated hydrocarbons, insoluble in petroleum ether, slightly soluble in ether and carbon tetrachloride.
Stability: Stable in acidic medium; gradually converted into dichlorvos when pH is greater than 6; half-life (22℃): 510d for pH=4, 46h for pH=7, less than 30min for pH=9.
1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of trichlorfon technical. This standard applies to trichlorfon technical consisting of trichlorfon and impurities generated during production. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601—1988 Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents GB/T603-1988 Preparation of preparations and products used in test methods for chemical reagents Method for determination of moisture content in pesticides
GB/T 1600--2001
GB/T 1604--1995
Rules for acceptance of commercial pesticides
GB/T 1605--2001
Sampling methods for commercial pesticides
GB3796-1999 General rules for packaging of pesticides
Approved by the People's Republic of China on July 13, 2001
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
Implementation on February 1, 2002
3.1 Appearance
White solid.
Trichlorfon technical shall meet the requirements of Table 1
Trichlorfon
Acetone insolubles
GB 334—2001
Table 1 Control Items of Trichlorfon Technical
Superior Products
Note: Acetone insolubles shall be inspected once every three months. 4
Test Method
4.1 Sampling
% (mass fraction)
Qualified Products
Carry out according to the "technical drug sampling" method in GB/T1605--2001. The sampling packages shall be determined by the random number table method, and the final sampling volume shall be not less than 200g.
4.2 Identification Test
4.2.1 High Performance Liquid Chromatography: This identification test can be carried out simultaneously with the determination of trichlorfon content. Under the same chromatographic operating conditions, the relative difference between the retention time of the main chromatographic peak in the sample solution and the retention time of the trichlorfon chromatographic peak in the standard solution should be within 1.5%. 4.2.2 Infrared spectroscopy: There should be no significant difference in the infrared spectra of the sample and the standard sample in the wave number range of 4000cm-1-1400cm-1 (see Figure 1).
Figure 1 Infrared spectrum of trichlorfon standard sample
4.3 Determination of trichlorfon content
4.3.1 High performance liquid chromatography (arbitration method)4.3.1.1 Method summary
GB334.2001
The sample is dissolved in acetonitrile, acetonitrile/water (water is adjusted to pH=3.0 with phosphoric acid) is used as the mobile phase, and a stainless steel column filled with Shimadzu vpODS and a UV detector are used to separate the trichlorfon in the sample by reverse phase high performance liquid chromatography and quantify it by external standard method. 4.3.1.2 Reagents and solutions
Acetonitrile: chromatographic grade;
Phosphoric acid,
Water: freshly distilled water;
Mobile phase: 4 (acetonitrile: water) = 15:85 (water adjusted to pH = 3.0 with phosphoric acid); Trichlorfon standard: known content, ≥99.0%. 4.3.1.3 Instruments
High performance liquid chromatograph: with variable wavelength UV detector; Chromatographic column: 150mm×4.6mm (id) stainless steel column, filled with Shimadzu-vpODS filler, particle size 5μm; Chromatographic data processor;
Ultrasonic cleaner;
Filter membrane: 0.45μm organic filter membrane;
Quantitative injection tube: 5uL;
Micro-injector. 50μ.
4.3.1.4 HPLC operating conditions
Mobile phase: acetonitrile: water) = 15:85 (water adjusted to pH = 3.0 with phosphoric acid); flow rate: 1.0mlL/min;
Column temperature: 30℃;
Detection wavelength: 200nm;
Injection volume: 5μL
Retention time: Trichlorfon 11.0min. bZxz.net
The above operating parameters are typical and can be appropriately adjusted according to the characteristics of different instruments in order to obtain the best results. Typical HPLC chromatogram of trichlorfon technical (see Figure 2). 0. 00 2. 00 4. 00 6. 00 8. 00 10. 00 12. 00 14. 00 minFig. 2 HPLC chromatogram of trichlorfon technical
4.3.1.5 Determination steps
a) Preparation of standard solution
GB 334—-2001
Weigh about 0.2g of trichlorfon standard sample, accurate to 0.0002g, put it into a 50mL volumetric flask, dissolve it in 10ml of acetonitrile, and then dilute it to the scale with acidic water (adjust pH=3.0 with phosphoric acid) and shake well. b) Preparation of sample solution
Weigh a sample containing about 0.2g of trichlorfon (accurate to 0.0002g), place it in a 50ml volumetric flask, dissolve it with 10ml of acetonitrile, dilute it to the scale with acidic water (adjust pH=3.0 with phosphoric acid), and shake it well. c) Determination
Under the operating conditions specified in 4.3.1.4, after the instrument baseline is stable, continuously inject several needles of standard solution. When the response value of two adjacent needles changes by less than 1.2%, determine in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.1.6 Calculation
Average the peak areas of trichlorfon in the two needles of sample solution and the two needles of standard solution before and after the sample. The mass fraction of trichlorfon in the sample, X (%), is calculated according to formula (1): Xi = Asmp
Where: A,
The average value of the trichlorfon peak area in the standard solution; -The average value of the trichlorfon peak area in the sample solution; A2—
The mass of the standard sample, g,
m2—-—~The mass of the sample, g;
p—The mass fraction of trichlorfon in the standard sample, %. 4.3.1.7 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.2%. The arithmetic mean value shall be taken as the determination result. 4.3.2 Alkaline hydrolysis chlorination method
4.3.2.1 Method summary
The sample undergoes alkaline hydrolysis to remove hydrogen chloride, and a certain amount (excess) of silver nitrate standard solution is added to convert Cl- into AgCI precipitation. The excess Ag+ is titrated with ammonium thiocyanate standard titration solution using ammonium ferric sulfate as an indicator until a light red color is obtained, which is the end point. 4.3.2.2 Reaction principle
2(CH:O),PCH(OH)CC13 +CO2---- 2(CH:O),P--C--CCl2 +2C1-+H2O+CO, Cl-+Ag *---AgCl +
Ag++CNS--AgCNS+
3CNS-→Fe3+Fe(CNS)3
4.3.2.3 Reagents and solutions
Dibutyl phthalate;
Nitric acid solution:y(HNO::H2O)=1:3; Sodium carbonate solution:c(
Na2CO,)-1. 0 mol/L;
Ethanol solution: (C2H.OH: H,O)=1:1;Silver nitrate standard solution: c(AgNO3)=0.05mol/L, prepared according to GB/T601;Ammonium thiocyanate standard titration solution: c(NH,CNS)=0.05mol/L, prepared according to GB/T601;Ammonium ferric sulfate solution: p[NH,Fe（SO4)]=100g/L, prepared according to GB/T603. 4.3.2.4 Apparatus
Constant temperature water bath: 30℃±0.5C;
Burette: 25mL, 50mL.
4.3.2.5 Determination steps
GB 334--2001
Weigh 0.3g0.4g sample (accurate to 0.0002g), place in a 250ml conical flask, add 50mL ethanol solution, after the sample is dissolved, place in a constant temperature water bath at 30℃±0.5℃, let stand for 10min to allow the solution temperature to reach equilibrium with the bath temperature, add 5mL sodium carbonate solution, and immediately and slowly add 5mL nitric acid solution after 10min, take out the conical flask from the constant temperature water bath, add 20mL water, 35mL silver nitrate standard solution, 3mL ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to completely condense the silver fluoride precipitate; titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. Blank determination: Weigh 0.3g0.4g sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50ml ethanol solution, after the sample is dissolved, add 7mL nitric acid solution, slowly add 5mL sodium carbonate solution, maintain in a constant temperature water bath for 10min, take out the conical flask, add 40mL water, 10mL silver nitrate standard solution, 3ml ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to make the silver chloride precipitate completely condense, and titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. 4.3.3 Calculation: The mass fraction of trichlorfon X, (%), is calculated according to formula (2): (cVi-cV? --- GV3 -c,V4)
Wherein: c
concentration of silver nitrate standard solution, mol/L; ~concentration of ammonium thiocyanate standard titration solution, mol/L; X 0.257 4X1.01 X100
The volume of silver nitrate standard solution added when titrating the sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the sample, mL; The volume of silver nitrate standard solution added when titrating the blank sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the blank sample, mL; The mass of the sample, g;
—The mass of the blank sample, g;
The mass of trichlorfon in grams equivalent to 1.00mL of silver nitrate standard solution [EcAgNO:)=1.000mol/L];
Correction coefficient.
4.3.4 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.0%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of moisture
Carry out according to the "Karl Fischer method" in GB/T1600-2001. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH) = 0.02 mol/L, prepared according to GB/T601; methyl red ethanol solution: p(methyl red) = 1 g/L. 4.5.2 Determination steps
Weigh 1g~2g of the sample (accurate to 0.002g), place it in a 250mL conical flask, add 50mL of water, wait for the sample to dissolve, add 3 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution. At the same time, perform a blank determination. 4.5.3 Calculation
The acidity of the sample expressed as mass fraction X: (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-Volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--Volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m——Sample mass·g;
GB 334--2001
0.049---With 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L] is equivalent to the mass of sulfuric acid expressed in grams.
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter bottle: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and place it in an oven to dry for 30min. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo× 100
Where: mo-
Mass of the sand core crucible after constant weight,;
-Total mass of the crucible and acetone insoluble matter after constant weight, g; Mass of the sample, g.
4.7 Inspection and acceptance of products
shall comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. ·(4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they shall comply with the provisions of GB3796. 5.3 Packages should be stored in a ventilated and dry warehouse. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash immediately with soap and water. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. The trichlorfon content within two years should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,2 Reaction principle
2(CH:O),PCH(OH)CC13 +CO2---- 2(CH:O),P--C--CCl2 +2C1-+H2O+CO, Cl-+Ag *---AgCl +
Ag++CNS--AgCNS+
3CNS-→Fe3+Fe(CNS)3
4.3.2.3 Reagents and solutions
Dibutyl phthalate;
Nitric acid solution:y(HNO::H2O)=1:3;Sodium carbonate solution:c(
Na2CO,)-1. 0 mol/L;
Ethanol solution: (C2H.OH: H,O)=1:1;Silver nitrate standard solution: c(AgNO3)=0.05mol/L, prepared according to GB/T601;Ammonium thiocyanate standard titration solution: c(NH,CNS)=0.05mol/L, prepared according to GB/T601;Ammonium ferric sulfate solution: p[NH,Fe（SO4)]=100g/L, prepared according to GB/T603. 4.3.2.4 Apparatus
Constant temperature water bath: 30℃±0.5C;
Burette: 25mL, 50mL.
4.3.2.5 Determination steps
GB 334--2001
Weigh 0.3g0.4g sample (accurate to 0.0002g), place in a 250ml conical flask, add 50mL ethanol solution, after the sample is dissolved, place in a constant temperature water bath at 30℃±0.5℃, let stand for 10min to allow the solution temperature to reach equilibrium with the bath temperature, add 5mL sodium carbonate solution, and immediately and slowly add 5mL nitric acid solution after 10min, take out the conical flask from the constant temperature water bath, add 20mL water, 35mL silver nitrate standard solution, 3mL ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to completely condense the silver fluoride precipitate; titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. Blank determination: Weigh 0.3g0.4g sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50ml ethanol solution, after the sample is dissolved, add 7mL nitric acid solution, slowly add 5mL sodium carbonate solution, maintain in a constant temperature water bath for 10min, take out the conical flask, add 40mL water, 10mL silver nitrate standard solution, 3ml ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to make the silver chloride precipitate completely condense, and titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. 4.3.3 Calculation: The mass fraction of trichlorfon X, (%), is calculated according to formula (2): (cVi-cV? --- GV3 -c,V4)
Wherein: c
concentration of silver nitrate standard solution, mol/L; ~concentration of ammonium thiocyanate standard titration solution, mol/L; X 0.257 4X1.01 X100
The volume of silver nitrate standard solution added when titrating the sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the sample, mL; The volume of silver nitrate standard solution added when titrating the blank sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the blank sample, mL; The mass of the sample, g;
—The mass of the blank sample, g;
The mass of trichlorfon in grams equivalent to 1.00mL of silver nitrate standard solution [EcAgNO:)=1.000mol/L];
Correction coefficient.
4.3.4 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.0%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of moisture
Carry out according to the "Karl Fischer method" in GB/T1600-2001. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH) = 0.02 mol/L, prepared according to GB/T601; methyl red ethanol solution: p(methyl red) = 1 g/L. 4.5.2 Determination steps
Weigh 1g~2g of the sample (accurate to 0.002g), place it in a 250mL conical flask, add 50mL of water, wait for the sample to dissolve, add 3 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution. At the same time, perform a blank determination. 4.5.3 Calculation
The acidity of the sample expressed as mass fraction X: (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-Volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--Volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m——Sample mass·g;
GB 334--2001
0.049---With 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L] is equivalent to the mass of sulfuric acid expressed in grams.
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter bottle: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and place it in an oven to dry for 30min. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo× 100
Where: mo-
Mass of the sand core crucible after constant weight,;
-Total mass of the crucible and acetone insoluble matter after constant weight, g; Mass of the sample, g.
4.7 Inspection and acceptance of products
shall comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. ·(4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they shall comply with the provisions of GB3796. 5.3 Packages should be stored in a ventilated and dry warehouse. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash immediately with soap and water. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. The trichlorfon content within two years should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,2 Reaction principle
2(CH:O),PCH(OH)CC13 +CO2---- 2(CH:O),P--C--CCl2 +2C1-+H2O+CO, Cl-+Ag *---AgCl +
Ag++CNS--AgCNS+
3CNS-→Fe3+Fe(CNS)3
4.3.2.3 Reagents and solutions
Dibutyl phthalate;
Nitric acid solution:y(HNO::H2O)=1:3;Sodium carbonate solution:c(
Na2CO,)-1. 0 mol/L;
Ethanol solution: (C2H.OH: H,O)=1:1;Silver nitrate standard solution: c(AgNO3)=0.05mol/L, prepared according to GB/T601;Ammonium thiocyanate standard titration solution: c(NH,CNS)=0.05mol/L, prepared according to GB/T601;Ammonium ferric sulfate solution: p[NH,Fe（SO4)]=100g/L, prepared according to GB/T603. 4.3.2.4 Apparatus
Constant temperature water bath: 30℃±0.5C;
Burette: 25mL, 50mL.
4.3.2.5 Determination steps
GB 334--2001
Weigh 0.3g0.4g sample (accurate to 0.0002g), place in a 250ml conical flask, add 50mL ethanol solution, after the sample is dissolved, place in a constant temperature water bath at 30℃±0.5℃, let stand for 10min to allow the solution temperature to reach equilibrium with the bath temperature, add 5mL sodium carbonate solution, and immediately and slowly add 5mL nitric acid solution after 10min, take out the conical flask from the constant temperature water bath, add 20mL water, 35mL silver nitrate standard solution, 3mL ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to completely condense the silver fluoride precipitate; titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. Blank determination: Weigh 0.3g0.4g sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50ml ethanol solution, after the sample is dissolved, add 7mL nitric acid solution, slowly add 5mL sodium carbonate solution, maintain in a constant temperature water bath for 10min, take out the conical flask, add 40mL water, 10mL silver nitrate standard solution, 3ml ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to make the silver chloride precipitate completely condense, and titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. 4.3.3 Calculation: The mass fraction of trichlorfon X, (%), is calculated according to formula (2): (cVi-cV? --- GV3 -c,V4)
Wherein: c
concentration of silver nitrate standard solution, mol/L; ~concentration of ammonium thiocyanate standard titration solution, mol/L; X 0.257 4X1.01 X100
The volume of silver nitrate standard solution added when titrating the sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the sample, mL; The volume of silver nitrate standard solution added when titrating the blank sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the blank sample, mL; The mass of the sample, g;
—The mass of the blank sample, g;
The mass of trichlorfon in grams equivalent to 1.00mL of silver nitrate standard solution [EcAgNO:)=1.000mol/L];
Correction coefficient.
4.3.4 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.0%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of moisture
Carry out according to the "Karl Fischer method" in GB/T1600-2001. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH) = 0.02 mol/L, prepared according to GB/T601; methyl red ethanol solution: p(methyl red) = 1 g/L. 4.5.2 Determination steps
Weigh 1g~2g of the sample (accurate to 0.002g), place it in a 250mL conical flask, add 50mL of water, wait for the sample to dissolve, add 3 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution. At the same time, perform a blank determination. 4.5.3 Calculation
The acidity of the sample expressed as mass fraction X: (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-Volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--Volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m——Sample mass·g;
GB 334--2001
0.049---With 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L] is equivalent to the mass of sulfuric acid expressed in grams.
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter bottle: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and place it in an oven to dry for 30min. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo× 100
Where: mo-
Mass of the sand core crucible after constant weight,;
-Total mass of the crucible and acetone insoluble matter after constant weight, g; Mass of the sample, g.
4.7 Inspection and acceptance of products
shall comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. ·(4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they shall comply with the provisions of GB3796. 5.3 Packages should be stored in a ventilated and dry warehouse. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash immediately with soap and water. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. The trichlorfon content within two years should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,Add 50mL of ethanol solution to a conical flask. After the sample is dissolved, place it in a constant temperature water bath at 30°C ± 0.5°C and let it stand for 10 minutes to allow the solution temperature to reach equilibrium with the bath temperature. Add 5mL of sodium carbonate solution. After 10 minutes, immediately and slowly add 5mL of nitric acid solution. Take out the conical flask from the constant temperature water bath, add 20mL of water, 35mL of silver nitrate standard solution, 3mL of ammonium ferric sulfate solution and 3mL of dibutyl phthalate, and shake it thoroughly to completely condense the silver fluoride precipitate. Titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. Blank determination: Weigh 0.3g0.4g sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50ml ethanol solution, after the sample is dissolved, add 7mL nitric acid solution, slowly add 5mL sodium carbonate solution, maintain in a constant temperature water bath for 10min, take out the conical flask, add 40mL water, 10mL silver nitrate standard solution, 3ml ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to make the silver chloride precipitate completely condense, and titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. 4.3.3 Calculation: The mass fraction of trichlorfon X, (%), is calculated according to formula (2): (cVi-cV? --- GV3 -c,V4)
Wherein: c
concentration of silver nitrate standard solution, mol/L; ~concentration of ammonium thiocyanate standard titration solution, mol/L; X 0.257 4X1.01 X100
The volume of silver nitrate standard solution added when titrating the sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the sample, mL; The volume of silver nitrate standard solution added when titrating the blank sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the blank sample, mL; The mass of the sample, g;
—The mass of the blank sample, g;
The mass of trichlorfon in grams equivalent to 1.00mL of silver nitrate standard solution [EcAgNO:)=1.000mol/L];
Correction coefficient.
4.3.4 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.0%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of moisture
Carry out according to the "Karl Fischer method" in GB/T1600-2001. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH) = 0.02 mol/L, prepared according to GB/T601; methyl red ethanol solution: p(methyl red) = 1 g/L. 4.5.2 Determination steps
Weigh 1g~2g of the sample (accurate to 0.002g), place it in a 250mL conical flask, add 50mL of water, wait for the sample to dissolve, add 3 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution. At the same time, perform a blank determination. 4.5.3 Calculation
The acidity of the sample expressed as mass fraction X: (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-Volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--Volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m——Sample mass·g;
GB 334--2001
0.049---With 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L] is equivalent to the mass of sulfuric acid expressed in grams.
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter bottle: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and place it in an oven to dry for 30min. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo× 100
Where: mo-
Mass of the sand core crucible after constant weight,;
-Total mass of the crucible and acetone insoluble matter after constant weight, g; Mass of the sample, g.
4.7 Inspection and acceptance of products
shall comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. ·(4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they shall comply with the provisions of GB3796. 5.3 Packages should be stored in a ventilated and dry warehouse. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash immediately with soap and water. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. The trichlorfon content within two years should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,Add 50mL of ethanol solution to a conical flask. After the sample is dissolved, place it in a constant temperature water bath at 30°C ± 0.5°C and let it stand for 10 minutes to allow the solution temperature to reach equilibrium with the bath temperature. Add 5mL of sodium carbonate solution. After 10 minutes, immediately and slowly add 5mL of nitric acid solution. Take out the conical flask from the constant temperature water bath, add 20mL of water, 35mL of silver nitrate standard solution, 3mL of ammonium ferric sulfate solution and 3mL of dibutyl phthalate, and shake it thoroughly to completely condense the silver fluoride precipitate. Titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. Blank determination: Weigh 0.3g0.4g sample (accurate to 0.0002g), place it in a 250mL conical flask, add 50ml ethanol solution, after the sample is dissolved, add 7mL nitric acid solution, slowly add 5mL sodium carbonate solution, maintain in a constant temperature water bath for 10min, take out the conical flask, add 40mL water, 10mL silver nitrate standard solution, 3ml ammonium ferric sulfate solution and 3mL dibutyl phthalate, shake thoroughly to make the silver chloride precipitate completely condense, and titrate with ammonium thiocyanate standard titration solution until the solution becomes a relatively stable light red color as the end point. 4.3.3 Calculation: The mass fraction of trichlorfon X, (%), is calculated according to formula (2): (cVi-cV? --- GV3 -c,V4)
Wherein: c
concentration of silver nitrate standard solution, mol/L; ~concentration of ammonium thiocyanate standard titration solution, mol/L; X 0.257 4X1.01 X100
The volume of silver nitrate standard solution added when titrating the sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the sample, mL; The volume of silver nitrate standard solution added when titrating the blank sample, mL; The volume of ammonium thiocyanate standard solution consumed when titrating the blank sample, mL; The mass of the sample, g;
—The mass of the blank sample, g;
The mass of trichlorfon in grams equivalent to 1.00mL of silver nitrate standard solution [EcAgNO:)=1.000mol/L];
Correction coefficient.
4.3.4 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 1.0%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of moisture
Carry out according to the "Karl Fischer method" in GB/T1600-2001. 4.5 Determination of acidity
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution: c(NaOH) = 0.02 mol/L, prepared according to GB/T601; methyl red ethanol solution: p(methyl red) = 1 g/L. 4.5.2 Determination steps
Weigh 1g~2g of the sample (accurate to 0.002g), place it in a 250mL conical flask, add 50mL of water, wait for the sample to dissolve, add 3 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution. At the same time, perform a blank determination. 4.5.3 Calculation
The acidity of the sample expressed as mass fraction X: (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-Volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--Volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m——Sample mass·g;
GB 334--2001
0.049---With 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L] is equivalent to the mass of sulfuric acid expressed in grams.
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter bottle: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and place it in an oven to dry for 30min. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo× 100
Where: mo-
Mass of the sand core crucible after constant weight,;
-Total mass of the crucible and acetone insoluble matter after constant weight, g; Mass of the sample, g.
4.7 Inspection and acceptance of products
shall comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. ·(4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they shall comply with the provisions of GB3796. 5.3 Packages should be stored in a ventilated and dry warehouse. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash immediately with soap and water. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. The trichlorfon content within two years should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,3 Calculation
The acidity X of the sample expressed as mass fraction (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-The volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--The volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m--Sample mass·g;
GB 334--2001
0.049---The mass of sulfuric acid in grams equivalent to 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L].
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter flask: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and put it in an oven to dry for 30 minutes. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo × 100
Wherein: mo-
The mass of the sand core crucible after constant weight, g;
-The total mass of the crucible and acetone insoluble matter after constant weight, g; The mass of the sample, g.
4.7 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604. The rounded value comparison method is used for the processing of limit values. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. · (4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they must comply with the provisions of GB3796. 5.3 Packages should be stored in ventilated and dry warehouses. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash immediately with soap and water. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. Within two years, the trichlorfon content should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,3 Calculation
The acidity X of the sample expressed as mass fraction (%), calculated according to formula (3): X = cV/- V2) × 0. 049
Wherein: ℃Concentration of standard sodium hydroxide titration solution, mol/L; × 100
-The volume of standard sodium hydroxide titration solution consumed in titrating the sample solution, mL; V_
V--The volume of standard sodium hydroxide titration solution consumed in titrating the blank solution, mL, (3)
m--Sample mass·g;
GB 334--2001
0.049---The mass of sulfuric acid in grams equivalent to 1.00 mL of standard sodium hydroxide titration solution [c(NaOH)=1.000 mol/L].
4.6 Determination of acetone insoluble matter
4.6.1 Instruments and reagents
Acetone: dried over anhydrous sodium sulfate;
Glass sand core crucible: G3;
Suction filter flask: 500mL;
Oven: 110℃;
4.6.2 Determination steps
Weigh 10g of the sample (accurate to 0.01g), put it in a conical flask, add 50mL of acetone, and shake until all soluble matter is dissolved. Filter with a constant weight crucible, then wash the conical flask with 60mL of acetone three times, and filter it by suction. Remove it and put it in an oven to dry for 30 minutes. The mass fraction of acetone insoluble matter in the sample, X, (%), is calculated according to formula (4): X, = ml = mo × 100
Wherein: mo-
The mass of the sand core crucible after constant weight, g;
-The total mass of the crucible and acetone insoluble matter after constant weight, g; The mass of the sample, g.
4.7 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604. The rounded value comparison method is used for the processing of limit values. 5 Marking, labeling, packaging and storage and transportation
5.1 Marking, labeling and packaging shall comply with the provisions of GB3796. · (4)
5.2 The inner packaging of trichlorfon technical is plastic bottle packaging, and the outer packaging is paper corrugated box, with a net content of 10kg per box. Other types of packaging can also be adopted according to user requirements or ordering agreements, but they must comply with the provisions of GB3796. 5.3 Packages should be stored in ventilated and dry warehouses. 5.4 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. 5.5 Safety: This product is an organophosphorus pesticide with moderate toxicity. Wear protective gloves, gas masks, and clean protective clothing when applying the pesticide. After application, wash with soap and water immediately. If poisoning occurs, use atropine or pralidoxime for detoxification under the guidance of a doctor. 5.6 Warranty period: Under the prescribed storage and transportation conditions, the warranty period of trichlorfon technical is two years from the date of production. Within two years, the trichlorfon content should not be less than 95% of the labeled content; acidity: superior products should not be higher than 0.5%, and qualified products should not be higher than 2.5%; moisture: superior products should not be higher than 0.4%, and qualified products should not be higher than 1.0%,
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