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GB 22618-2008: [GB/T 22618-2008] Fenoxaprop-P-ethyl emulsifiable concentrates
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[GB/T 22618-2008] Fenoxaprop-P-ethyl emulsifiable concentrates
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Basic data | Standard ID | GB 22618-2008 (GB22618-2008) | | Description (Translated English) | [GB/T 22618-2008] Fenoxaprop-P-ethyl emulsifiable concentrates | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 12,188 | | Date of Issue | 2008-12-17 | | Date of Implementation | 2009-06-01 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 21 of 2008 (No. 134 overall) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard specifies the Fenoxaprop EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to fenoxaprop original drug, security agent and emulsifier solution grass azole dissolved in a suitable solvent in the preparation of fenoxaprop EC. | GB 22618-2008: [GB/T 22618-2008] Fenoxaprop-P-ethyl emulsifiable concentrates---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Fenoxaprop-P-ethyl emulsifiable concentrates
ICS 65.100.20
G25
National Standards of People's Republic of China
Oxazole diclofop EC
Posted 2008-12-17
2009-06-01 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 an informative annex.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee on Pesticides (SAC/TC133) centralized.
This standard is drafted by. the Ministry of Agriculture.
Participated in the drafting of this standard. Jiangsu Rui Wo Chemical Co., Ltd., Anhui Fengle Agrochemical Co., Ltd., Zhejiang Hisun Chemical Company Limited
Division, Hangzhou Yulong Chemical Co., Ltd.
The main drafters of this standard. Jiang Yifei, the United Kingdom, in the wing, single-Wei force, Chentie Chun, Wang Qiang, Jin Jinsong, Wang Limin, Xu Liting.
Oxazole diclofop EC
Other name, structural formula and basic physicochemical parameters of the refined product azole active ingredients diclofop as follows.
ISO common name. fenoxaprop-P-ethyl
CIPAC digital code. 484
CA registration number. 71283-80-2
Chemical Name. (R) -2- [4- (6- chloro-1,3-benzoxazol-2-yloxy) phenoxy] propionate
Structure.
Empirical formula. C18H16ClNO5
Molecular Weight. 361.8 (according to 2007 international relative atomic mass)
Biological activity. weeding
Melting point. 89 ℃ ~ 91 ℃
Vapor pressure (20 ℃). 530nPa
Solubility (g/L, 20 ℃). water 7 × 10-4 (pH5.8), acetone 200, 200 of toluene, ethyl acetate > 200, about 24 ethanol
Stability. 50 ℃ stable 90d, a light-insensitive, met acid, alkali decomposition
This product safety agent fenchlorazole other name, structural formula and basic physicochemical parameters are as follows.
ISO common name. fenchlorazole-ethyl
CA registration number. 103112-35-2
Chemical name. 1- (2,4-dichlorophenyl) -5-trichloromethyl-1,2,4-triazole-3-carboxylic acid -1H ethyl
Structure.
Empirical formula. C12H8Cl5N3O2
Molecular Weight. 403.5 (according to 2007 international relative atomic mass)
Biological activity. safener
Melting point. 108 ℃ ~ 112 ℃
Vapor pressure (20 ℃). 890nPa
Solubility (g/L, 20 ℃). water 9 × 10-4 (pH4.5), 2.5 hexane, 27 methanol, toluene, 270, 360 as acetone, dichloromethane > 500
1 Scope
This standard specifies the fine
Oxazole diclofop EC requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the fine
Oxazole diclofop original drug, security agents fenchlorazole formulated with an emulsifier is dissolved in a suitable solvent from the fine
Oxazole diclofop EC.
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.
GB/T 1600 Determination of Water Pesticides
Determination of GB/T 1601 Pesticides pH value
GB/T 1603 Determination of emulsion stability of pesticide
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB/T 4472 chemical product density, relative density measurement General
GB 4838 EC pesticide packaging
GB/T 19136 Determination of Pesticide Thermal storage stability
GB/T 19137 Pesticide cryogenic stability Determination
3 Requirements
3.1 Composition and appearance. This product should be compliant oxazole diclofop fine original drug, fenchlorazole security agent and emulsifier dissolved in a suitable solvent
The preparation should be stable homogeneous liquid, free from visible suspended matter and sediment.
3.2 azole fine grasses Ling EC shall comply with the requirements of Table 1.
Table 1 fine azole diclofop EC Control Project Index
project
index
6.9% 80.5g/L 100g/L
Oxazole diclofop mass fraction a /%
Or concentration (20 ℃) / (g/L)
+ 0.7-0.7 0.8-0.8 6.9 8.4 + 10.4 + 1.0 to 1.0
- 100 + 80.5 + 8.0-8.0 10-10
Fenchlorazole mass fraction b /% ≥ declared value (accurate to 1 after the decimal point)
Moisture content /% ≤ 1.0
pH range of 5.0 to 9.0
Emulsion stability (diluted 200 times) Qualified
Low temperature stability Qualified c
Thermal storage stability c qualified
When a dispute occurs when the quality to fine oxazole diclofop mass fraction of arbitration.
b whether to add security agents decided by crop objects; allows the use of other security agents, the detection method and the corresponding indicators in the national pesticide requirements can be standardized technology
Committee was surgery.
C When normal production, low-temperature storage stability and thermal stability test, every three months, at least once.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 5.3.2 in "liquid formulation sampled" in. Determining sample package using a random number table method, the final sample
The amount of not less than 200mL.
4.2 Identification Test
HPLC --- The identification test with fine
Determination oxazole diclofop content simultaneously. In the same chromatographic operation
Under the conditions, the sample solution is a two peak retention time
Azole grasses standard solution for the retention time of the two peaks of enantiomers relative
Of the difference should be less than 1.5%.
4.3 Determination of fine azole diclofop, fenchlorazole mass fraction
Determination 4.3.1 oxazole diclofop, fenchlorazole mass fraction
4.3.1.1 Method summary
Sample dissolved in mobile phase, n-hexane and isopropanol as the mobile phase, use ZORBAXSIL as filling a stainless steel column and variable wave
Long UV detector, of the sample
Oxazole diclofop, fenchlorazole normal phase HPLC separation and determination, external standard. also may
Using capillary gas chromatography
Oxazole diclofop mass fraction, chromatographic operating conditions given in Appendix A.
4.3.1.2 Reagents and solutions
Hexane. chromatography;
Isopropanol. chromatography;
Oxazole diclofop standard. a known mass fraction ≥99.0%;
Fenchlorazole standard. a known mass fraction ≥99.0%.
4.3.1.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column. 250mm × 4.6mm (i.d.) Stainless steel column, built ZORBAXSIL, 5μm particle size of the filler;
Filter. filter pore size of about 0.45μm;
Micro injector. 100μL;
Quantitative sample line. 10μL;
Ultrasonic cleaner.
4.3.1.4 HPLC operating conditions
Mobile phase. [Psi] (n-hexane. isopropanol) = 90.10;
Flow rate. 0.8mL/min;
Column temperature. room temperature;
Detection wavelength. 230nm;
Injection volume. 10μL;
keep time.
Oxazole diclofop 4.8min, fenchlorazole 5.5min.
The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to
To obtain the best results. typical
Oxazole diclofop EC HPLC is shown in Figure 1.
1 --- oxazole diclofop;
2 --- fenchlorazole.
Figure 1 EC fine azole diclofop HPLC Fig.
4.3.1.5 Measurement procedure
4.3.1.5.1 Preparation of standard solution
Weigh
Oxazole diclofop standard 0.05g, fenchlorazole standard 0.03g (accurate to 0.0002g), placed in 100mL volumetric flask.
80mL mobile phase in an ultrasonic bath shaking 5min make sample dissolution, removed after cooling to room temperature, dilute to the mark with the mobile phase,
Shake well.
4.3.1.5.2 Preparation of sample solution
Weigh containing
0.05g oxazole diclofop sample (accurate to 0.0002g), placed in 100mL flask, add 80mL mobile phase
In the ultrasonic bath shaking 5min make sample dissolution, removed after cooling to room temperature, mobile phase and dilute to the mark, shake, filtration.
4.3.1.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles
Lingfeng grass area with azole
After the change of less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.3.1.6 Calculation
The measured before and after the two-needle sample solution and two doses of the standard sample solution
Oxazole diclofop (fenchlorazole) peak areas are averaged.
Specimen
(1) Calculation azole diclofop (fenchlorazole) mass fraction of 1 (%) according to formula (2) to calculate the concentration of ρ1 (g/L) by the formula.
(1)
ρ1 =
Where.
A1 --- the standard solution, the average oxazole diclofop (fenchlorazole) peak area;
A2 --- sample solution, the average azole diclofop (fenchlorazole) peak area;
--- Standard samples azole diclofop (fenchlorazole) mass fraction,%;
4.3.1.7 allowable difference
Two parallel determination results relative error should not exceed 5% of the arithmetic mean as a measurement result.
4.3.2 R- enantiomer ratio of measurement
4.3.2.1 Method summary
Sample dissolved in mobile phase, n-hexane and ethanol as the mobile phase, use a stainless steel ChiralcelOK as filler chiral column and variable wave
Long UV detector, of the sample
Oxazole diclofop R- enantiomer normal phase high performance liquid separation and determination of the spectrum, phase separation may also be used
Other chiral column or flow when the phase.
4.3.2.2 Reagents and solutions
Hexane. chromatography;
Ethanol. chromatography;
Oxazole diclofop standard. a known mass fraction ≥99.0%.
4.3.2.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column. 250mm × 4.6mm (i.d.) Stainless steel chiral column, built ChiralcelOK, filler particle size of 10μm;
Filter. filter pore size of about 0.45μm;
Micro injector. 100μL;
Quantitative sample line. 20μL;
Ultrasonic cleaner.
4.3.2.4 HPLC operating conditions
Mobile phase. [Psi] (n-hexane. ethanol) = 50.50;
Flow rate. 1.3mL/min;
Column temperature. room temperature;
Detection wavelength. 280nm;
Injection volume. 20μL;
Retention time. R- enantiomer (fine azole diclofop) 8.4min, S- enantiomer 14.5min.
The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to
To obtain the best results. Typical fine
Oxazole diclofop EC HPLC is shown in Figure 2.
1 --- R- enantiomer (fine azole diclofop);
2 --- S- enantiomer.
Figure 2 Fine oxazole diclofop EC HPLC diagram
4.3.2.5 Measurement procedure
4.3.2.5.1 Preparation of standard solution
Weigh
Oxazole diclofop standard of about 0.05g, placed in 100mL volumetric flask, dissolved in mobile phase and dilute to the mark.
4.3.2.5.2 Preparation of sample solution
Weigh about containing fine
0.05g oxazole diclofop sample, placed in 100mL volumetric flask, dissolved in mobile phase and dilute to volume, shake,
filter.
4.3.2.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles
Oxazole diclofop R- enantiomers,
S- enantiomer relative change in peak area is less than 1.0% (both enantiomers area ratio should be 50.50, deviation does not exceed 1%. If more than
1%, calculated oxazole diclofop R- enantiomer ratios should be corrected for), then two injection needles sample solution.
4.3.2.6 Calculation
Specimen
Oxazole diclofop R- enantiomer ratio of K, according to equation (3) Calculated.
K = ARAR + AS
(3)
Where.
AR --- two needles in the sample solution, oxazole diclofop mean R- enantiomer peak area;
AS sample solution --- two needles, oxazole diclofop mean S- enantiomer peak area.
When the standard sample solution
When oxazole diclofop R- enantiomer area beyond the area of the two enantiomers and the (50 ± 1)%, the sample azole Wo
Grass Ling R- enantiomer ratio of K ', according to equation (4) Calculated.
K '= ARAR + AS (A'R/A'S)
(4)
Where.
A'R --- two doses of the standard solution, oxazole diclofop mean R- enantiomer peak area;
A'S --- two doses of the standard solution, oxazole diclofop mean S- enantiomer peak area.
4.3.3 fine oxazole diclofop mass fraction calculation
The sperm sample
2 mass fraction (%) oxazole diclofop according to equation (5) to calculate the mass concentration ρ2 (g/L) according to equation (6) Calculated.
2 = 1 × K (5)
ρ2 = ρ1 × K (6)
When the standard sample solution oxazole diclofop R- enantiomer area beyond the area of the two enantiomers and the (50 ± 1)%, sample fine azole
Diclofop mass fraction '2 (%), according to equation (7) to calculate the mass concentration ρ'2 (g/L) according to equation (8) Calculated.
'2 = 1 × K' (7)
ρ'2 = ρ1 × K '(8)
4.4 Determination of Moisture
According to GB/T 1600 the "Karl Fischer" method.
According to GB/T 1601 carried out.
4.6 Emulsion stability test
Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, the non-oil slick, no precipitation under qualified.
4.7 Low temperature stability test
According to GB/T 19137 in "homogeneous emulsion and liquid preparations" to. The bottom of the centrifuge tube educt volume of less than 0.3mL qualified.
4.8 Thermal storage stability test
According to GB/T 19136 in "liquid formulation" to. Fine grass azole azole diclofop reconciliation after the mass fraction of heat storage thermal storage mass allow the former dropped
Volume fraction of 95%, emulsion stability should continue to meet the standards.
4.9 product testing 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 oxazole diclofop fine EC marking, labeling, packaging, should meet the requirements of GB 4838.
5.2 azole fine grasses Ling EC package should be stored in well-ventilated, dry coffers.
5.3 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.4 Safety. This product is a low-toxicity herbicides. Poisoning symptoms are nausea, vomiting, drowsiness occur subsequent, limb numbness, severe muscle fibrillation
Move, convulsions, coma, respiratory failure. The FDA should wear protective gloves, masks and goggles, wear clean protective clothing with soap immediately after application
Washed with water to avoid skin and eye contact with liquid. If swallowed, immediately induce vomiting, gastric lavage, activated charcoal and a laxative can also be used, symptomatic treatment.
5.5 Warranty. under the specified storage conditions to ensure the precision of oxazole diclofop EC, from date of manufacture for 2 years.
Appendix A
(Informative)
Oxazole diclofop content by capillary gas chromatographic method
A. 1 Method summary
Sample was dissolved in acetone, phthalate, dicyclohexyl phthalate as internal standard, and the use of silica capillary column HP-5 (5% phenyl methyl silicone) coated wall
Flame ionization detector, the sample
Oxazole diclofop and measured by gas chromatography, internal standard.
A. 2 Reagents and solutions
acetone;
Oxazole diclofop standard. a known mass fraction, ≥99.0%;
Internal standard. phthalate, dicyclohexyl phthalate, should not interfere with the analysis of impurities;
Internal standard solution. Weigh phthalate, dicyclohexyl phthalate 5g, placed 1000mL volumetric flask, dissolved in acetone and diluted to the mark.
A. 3 Instrument
Gas chromatograph. with a hydrogen flame ionization detector;
Chromatographic data processor or chromatography workstation;
Column. 30m × 0.32mm (i.d.) Fused silica capillary column, wall coated HP-5 (5% phenyl methyl silicone), a film thickness of 0.25μm.
A. 4 GC operating conditions
Temperature (℃). Room 250 column, the gasification chamber 260, detection chamber 270;
Gas flow rate (mL/min). carrier gas (N2) 1.5, hydrogen gas 30, air 300;
Injection volume. 1.0μL;
keep time.
Oxazole diclofop about 7.8min, dicyclohexyl phthalate esters about 5.9min.
The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to
To obtain the best results. Typical fine
Oxazole diclofop EC gas chromatography is shown in Figure A. 1.
1 --- internal standard (dicyclohexyl phthalate esters);
2 --- oxazole diclofop.
Figure A. 1 fine oxazole diclofop EC gas chromatogram
Book GB 22618-2008
A. 5 measuring step
A. 5.1 Preparation of standard solution
Weigh
Oxazole diclofop standard 0.07g (accurate to 0.0002g), placed in 15mL stoppered glass bottle with a pipette accurately added
Internal standard solution 10mL, shake.
A. 5.2 Preparation of sample solution
Weigh containing
Sample of 0.07g oxazole diclofop (accurate to 0.0002g), placed in 15mL stoppered glass vial, with the A. 5.1 the same
Branch pipette accurately added internal standard solution 10mL, 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
Oxazole diclofop and the internal standard peak
After the relative change in area ratio is less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
A. 6 Calculation
The measured before and after the two-needle sample solution and two doses of the standard sample solution
Oxazole diclofop and the internal standard peak area ratios are flat
all. Specimen
Oxazole diclofop mass fraction of 1 (%), according to equation (A.1) Calculated.
(A.1)
Where.
--- Standard samples azole diclofop mass fraction,%.
A. 7 allowable difference
Two parallel determination results relative error should not exceed 5% of the arithmetic mean as a measurement result.
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