GB/T 22173-2021_English: PDF (GB/T22173-2021)
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Oxadiazon technical material
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GB/T 22173-2021
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[GB/T 22173-2008] Oxadiazon technical
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| Standard ID | GB/T 22173-2021 (GB/T22173-2021) | | Description (Translated English) | Oxadiazon technical material | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 9,945 | | Date of Issue | 2021-12-31 | | Date of Implementation | 2022-07-01 | | Older Standard (superseded by this standard) | GB/T 22173-2008 | | Drafting Organization | Anhui Kelihua Chemical Co., Ltd. | | Administrative Organization | National Pesticide Standardization Technical Committee | | Regulation (derived from) | National Standard Announcement No. 17 of 2021 | | Proposing organization | China Petroleum and Chemical Industry Federation | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration | | Standard ID | GB 22173-2008 (GB22173-2008) | | Description (Translated English) | [GB/T 22173-2008] Oxadiazon technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 10,141 | | Date of Issue | 2008-07-11 | | Date of Implementation | 2009-01-01 | | Quoted Standard | GB/T 601-2002; GB/T 1600; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 | | Drafting Organization | Shenyang Institute of Chemical Industry | | Administrative Organization | National Standardization Technical Committee of pesticides | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 overall) | | Proposing organization | China Petroleum and Chemical Industry Association | | Issuing agency(ies) | Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China; Standardization Administration of China | | Summary | This Chinese standard specifies the original drug Oxadiazon requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to Oxadiazon and impurities generated in the production of Oxadiazon original drug. |
GB/T 22173-2021
Oxadiazon technical material
ICS 65:100:20
CCSG25
National Standards of People's Republic of China
Replacing GB/T 22173-2008
Oxadiazone original drug
Published on 2021-12-31
2022-07-01 Implementation
State Administration for Market Regulation
Released by the National Standardization Administration
foreword
This document is in accordance with the provisions of GB/T 1:1-2020 "Guidelines for Standardization Work Part 1: Structure and Drafting Rules of Standardization Documents"
drafted:
This document replaces GB/T 22173-2008 "Oxadiazone Technical Drugs", compared with GB/T 22173-2008, except for structural adjustment and editorial
In addition to the changes, the main technical changes are as follows:
--- Changed the index of oxadiazon mass fraction (see 4:2, 3:2 of the:2008 edition);
--- Changed the acetone insoluble matter index (see 4:2, 3:2 of the:2008 edition);
--- Changed the test method for acidity (see 5:8, 4:6 of the:2008 edition);
--- Deleted product inspection and acceptance (see 4:7 of the:2008 edition);
--- Delete the acceptance period (see 5:6 of the:2008 edition);
--- Added inspection rules (see Chapter 6);
--- Added other names, structural formulas and basic physicochemical parameters of oxadiazon (see Appendix A):
Please note that some content of this document may be patented: The issuing agency of this document assumes no responsibility for identifying patents:
This document is proposed by China Petroleum and Chemical Industry Federation:
This document is under the jurisdiction of the National Pesticide Standardization Technical Committee (SAC/TC133):
This document is drafted by: Anhui Kelihua Chemical Co:, Ltd:, Anhui Chemical Research Institute, Anhui Guangxin Agrochemical Co:, Ltd:, Hefei
Xingyu Chemical Co:, Ltd:, Shenyang Shenyang Institute of Chemical Technology Co:, Ltd:, Shenyang Chemical Research Institute Co:, Ltd:
The main drafters of this document: Ding Xiangdong, Liu Gailing, Yu Liang, Shen Long, Lei Shichao, Miao Li, Lin Xiang, Jiang Yan, Sun Hongfeng:
The previous versions of this document and its superseded documents are as follows:
---First published in:2008 as GB/T 22173-2008;
---This is the first revision:
Oxadiazone original drug
1 Scope
This document specifies the technical requirements, test methods, inspection rules, acceptance and quality assurance period of oxadiazon technical materials, as well as signs, labels, packaging
packaging and storage:
This document is applicable to the quality control of oxadiazon technical products, and can also be used as a guide for trade, conformity assessment and management activities between suppliers and buyers:
in accordance with:
Note: See Appendix A for other names, structural formulas and basic physicochemical parameters of oxadiazon:
2 Normative references
The contents of the following documents constitute essential provisions of this document through normative references in the text: Among them, dated citations
documents, only the version corresponding to that date applies to this document; for undated references, the latest edition (including all amendments) applies to
this document:
GB/T 1600-2021 Method for Determination of Moisture of Pesticide
GB/T 1604 Rules for the acceptance of commercial pesticides
GB/T 1605-2001 Sampling method for commercial pesticides
GB 3796 General Rules for Pesticide Packaging
GB/T 8170-2008 Numerical Rounding Rules and Representation and Judgment of Limit Values
GB/T 19138 Determination method of pesticide acetone insoluble matter
GB/T 28135-2011 Pesticide acid (alkali) degree determination method indicator method
3 Terms and Definitions
There are no terms and definitions that need to be defined in this document:
4 Technical requirements
4:1 Appearance
It is white to yellow solid powder:
4:2 Specifications
The original drug of oxadiazone should meet the requirements of Table 1:
......
GB 22173-2008
Oxadiazon technical
ICS 65.100.20
G25
National Standards of People's Republic of China
Grass-one original drug
Posted 2008-07-11
2009-01-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
The standard Chapter 3, Chapter 5 are mandatory, the rest are recommended.
Appendix A of this standard is the data appendix.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee on Pesticides (CSBTS/T C133) centralized.
This standard is drafted by. Shenyang Chemical Research Institute, Anhui Province Chemical Industry Research Institute.
Participated in the drafting of this standard. Anhui Branch Lihua Chemical Company.
The main drafters of this standard. Jiangmin Yi, Xing Jun, South Korea seek country, Jiang Hong, Wang redundant.
The standard commission Secretariat of National Pesticide Standardisation Technical Committee responsible for the interpretation.
Grass-one original drug
Other name, structural formula and basic physicochemical parameters of the active ingredients of the product mesotrione as follows.
ISO common name. oxadiazon
CAS Registry Number. 19666-30-9
CIPAC Numeric Code. 213
Chemical name. 5-tert-butyl-3- (2,4-dichloro-5-isopropoxyphenyl) -1,3,4-oxadiazol -2 (3H) - one
Structure.
Handkerchief
N
(CH3) 3
Normal Normal Normal Normal Normal Normal
Among Teachers
Division
C O
Cl
Cl
OCH (CH3) 2
Empirical formula. C15H18Cl2N2O3
Molecular Weight. 345.2 (according to 2005 international relative atomic mass)
Biological activity. weeding
Melting point. about 90 ℃
Vapor pressure. less than 0.133mPa (20 ℃)
Solubility (20 ℃). water 0.7mg/L; acetone, acetophenone, anisole 600g/L; benzene, toluene, chloroform, 1kg/L.
Stability. storage stability at room temperature. Soil DT50 about 90d.
1 Scope
This standard specifies the
Grass-one of the original drug requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the
Grass ketone impurity generated in the production and composition
Grass-one of the original drug.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
Preparation of GB/T 601-2002 Chemical Reagent standard titration solution
GB/T 1600 Determination of Water Pesticides
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB 3796 pesticide packaging General
GB/T 19138 Determination of acetone insoluble pesticide
3 Requirements
3.1 Appearance
White to tan solid, no visible foreign matter and filling the modifier.
3.2 grass-one of the original drug should be consistent with the requirements in Table 1.
Table 1 mesotrione original drug quality control program indicators
Item Index
Grass-one mass fraction /% ≥ 95.0
Moisture /% ≤ 0.5
Acetone insolubles a /% ≤ 0.5
Acidity (H2SO4 meter) /% ≤ 0.3
a substance insoluble in acetone, measurement at least once every three months.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 "on the original drug product sampling" approach. Determining sample package using a random number table method; the final sample size
Not less than 100g.
4.2 Identification Test
Infrared spectroscopy --- sample and standard samples at 4000cm-1 ~ 400cm-1 range of the infrared absorption spectrum should be no significant difference. Mark
Like infrared spectrum is shown in Figure 1.
Figure 1 mesotrione standard infrared spectra
Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of the grass one. Under the same chromatographic operating conditions, the test
The retention time of the sample solution and the standard solution in a chromatographic peak
Mesotrione retention time peaks, the relative difference should be 1.5%
Fewer.
4.3 Determination of the mass fraction of mesotrione
4.3.1 Method summary
Sample was dissolved in chloroform to tetracosane as internal standard, using a HP-5 (5% phenyl methyl silicone) fused silica capillary column coated walls, and
Flame ionization detector, the sample
Grass-one capillary gas chromatography and determination. This method of arbitration law, may also be used
Packed column gas chromatography, chromatographic operating conditions, see Appendix A.
4.3.2 Reagents and solutions
Chloroform;
Grass-one standard. a known mass fraction, ≥99.0%;
Tetracosane. Do not interfere with the analysis of impurities;
Internal standard solution. Weigh 5.0g of tetracosane, in 1000mL volumetric flask, dissolved with chloroform, constant volume, shake.
4.3.3 Instruments
Gas chromatograph. with flame ionization detector;
Column. 30m × 0.32mm (. I.d) quartz capillary column, wall coated HP-5 (5% phenyl methyl silicone), film thickness 0.25μm;
Chromatographic data processor or chromatography workstation.
4.3.4 GC operating conditions
Temperature (℃). Room 210 column, the gasification chamber 250, detection chamber 260;
Gas flow rate (mL/min). carrier gas (N2) 1.8, the compensation gas (N2) 25, hydrogen gas 40, air 400;
Split ratio. 40.1;
Injection volume. 1.0μL;
keep time.
Grass-one. about 6.5min, internal standard. about 10.8min.
GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate,
In order to obtain the best results. typical
Grass-one drug and the internal standard gas chromatography is shown in Figure 2.
1 --- grass ketone;
2 --- internal standard.
FIG. 2 mesotrione original drug and the internal standard gas chromatograph
4.3.5 measuring step
4.3.5.1 preparation of standard solution
Weigh
Grass-one standard 0.05g (accurate to 0.00002g), placed in a glass bottle stopper, with a pipette accurately added 5mL internal standard
Solution, shake.
4.3.5.2 preparation of the sample solution
Weigh the sample 0.05g (accurate to 0.00002g), placed in a glass bottle stopper, using the same and 4.3.5.1 used a pipette
Tube accurately added internal standard solution 5mL, shake.
4.3.5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles
Grass-one with internal standard
After the change of the relative peak area ratio of less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution
Determination.
4.3.6 Calculation
The measured before and after the two-needle sample solution and two doses of the standard sample solution
Peak area ratio of mesotrione and the internal standard were averaged.
Specimen
Grass-one mass fraction of 1 (%) according to equation (1).
(1)
Where.
γ1 --- standard solution mean grass ketone and the internal standard peak area ratio;
γ2 --- the average of the sample solution and grass-one internal standard peak area ratio;
--- Standard in-one grass mass fraction, expressed as a percentage.
4.3.7 allowable difference
The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.
4.4 Determination of Moisture
According to GB/T 1600 the "Karl Fischer method".
4.5 Determination of acetone insolubles
According to GB/T 19138 performed.
4.6 Determination of acidity
4.6.1 Reagents and solutions
95% ethanol;
Sodium hydroxide standard titration solution c (NaOH) = 0.02mol/L, according to GB/T 601-2002 4.1 preparation and calibration;
Methyl red. 2g/L ethanol solution;
Bromocresol green. 1g/L ethanol solution;
Mixed indicator. Take 1mL methyl red ethanol solution and 3mL bromocresol green ethanol solution, and mix well.
4.6.2 measuring step
Weigh the sample 2g (accurate to 0.002g), placed in a 250mL Erlenmeyer flask, add 95% ethanol 50mL, shake the sample solution
solution. Add 8 drops of mixed indicator, with 0.02mol/L sodium hydroxide standard titration solution titration, the solution changed from red to green light is final
point. Meanwhile blank determination.
4.6.3 Calculation
Acidity 2 (%) of the sample, according to equation (2).
Ba 2 =
(Vp Vp 1- 0) × M
100 (2)
Where.
Ba --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L);
Vp 1 --- titration of the sample solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);
V0 --- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);
--- The M values of the molar mass of sulfuric acid, in units of grams per mole (g/mol), M 12
(H2SO4) = 49g/[] mol.
4.7 product testing and acceptance
Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 mesotrione original drug marking, labeling and packaging should comply with the provisions of GB 3796.
5.2 mesotrione original drug use clean plastic bag lined woven bag or cardboard drum lined with clean plastic bag, barrel a net content
Generally from 25kg or 40kg. Also available upon request or order agreement, the use of other forms of packaging, subject to the provisions of GB 3796.
5.3 mesotrione original drug package should be stored in well-ventilated, dry coffers.
5.4 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.5 Security. This is a low toxicity herbicides, are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product
Wear the necessary protective clothing. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. Coverage should be immediately sent to hospital symptomatic
treatment.
5.6 of acceptance. Acceptance of grass-one of the original drug for a month. From the date of delivery, product quality inspection completed within a month, its
Indicators should meet the standards.
Appendix A
(Informative)
Grass-one packed column gas chromatography analysis conditions
A. 1 Method summary
Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using the 5% OV-210/ChromosorbW AW-
DMCS (180μm ~ 250μm) as a filler stainless steel column and flame ionization detector, one was on the grass and Gas Chromatography
Determination.
A. 2 Reagents and solutions
Chloroform;
Grass-one standard. a known mass fraction ≥99.0%;
Internal standard. dicyclohexyl phthalate esters should not interfere with the analysis of impurities.
A. 3 instruments and reagents
Gas chromatograph. with flame ionization detector;
Chromatographic data processor;
Column. 1m × 3mm (i.d.) Stainless steel column;
Column packing. OV-210 coated in ChromosorbW AW-DMCS vector (180μm ~ 250μm), the fixative. (fixed
+ Liquid carrier) = 5.100.
A. 4 chromatographic operating conditions
Temperature (℃).200 column temperature, the gasification chamber 250, the detector 260;
Flow rate (mL/min). carrier gas (N2 of) 30, hydrogen gas 30, air 300;
Injection volume. 1.0μL;
Retention time (min). grass-one about 8.9; internal standard 15.8.
A. 5 measuring step
A. 5.1 Preparation of standard solution
Weigh
Grass-one standard 0.05g (accurate to 0.00002g), placed in a stoppered glass bottle with a pipette accurately added 5mL within
Standard solution, shake.
A. 5.2 Preparation of sample solution
Weigh containing
Mesotrione sample of approximately 0.05g (accurate to 0.00002g), placed in a glass bottle stopper, with the A. 5.1 Use
With a pipette accurately added internal standard solution 5mL, shake.
A. 5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles
Peak area of grass ketone and the internal standard
After the change in volume of less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured. See the typical patterns
Figure A. 1.
1 --- grass ketone;
2 --- internal standard.
Figure A. Figure 1 mesotrione GC internal standard is
A. 6 Calculation
The measured before and after the two-needle sample solution and two doses of the standard sample solution
Grass-one ratio and the internal standard peak area were averaged.
Specimen
Grass-one mass fraction of 1 (%) according to equation (A.1) Calculated.
(A.1)
Where.
γ1 --- standard solution mean grass ketone and the internal standard peak area ratio;
γ2 --- the average of the sample solution and grass-one internal standard peak area ratio;
--- Standard in-one grass mass fraction, expressed as a percentage.
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