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GB 28152-2011: [GB/T 28152-2011] Pyrimethanil aqueous suspension concentrates
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[GB/T 28152-2011] Pyrimethanil aqueous suspension concentrates
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Basic data
Standard ID: GB 28152-2011 (GB28152-2011)
Description (Translated English): [GB/T 28152-2011] Pyrimethanil aqueous suspension concentrates
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.30
Word Count Estimation: 13,196
Date of Issue: 2011-12-30
Date of Implementation: 2012-04-15
Quoted Standard: GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 6682-2008; GB/T 8170-2008; GB/T 14825; GB/T 16150; GB/T 19136; GB/T 19137
Regulation (derived from): Announcement of Newly Approved National Standards No. 23 of 2011
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 requirements pyrimethanil SC, test methods and marking, labeling, packaging, storage and warranty. This standard applies to pyrimethanil original drug with a suitable additives and fillers processed into pyrimethanil SC.
GB 28152-2011: [GB/T 28152-2011] Pyrimethanil aqueous suspension 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.
Pyrimethanil aqueous suspension concentrates
ICS 65.100.30
G25
National Standards of People's Republic of China
Pyrimethanil SC
Issued on. 2011-12-30
2012-04-15 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 is mandatory, the rest are recommended.
This standard was drafted in accordance with GB/T 1.1-2009 given rules.
Please note that some content of this document may involve patents, the issuing authority of this document does not assume responsibility for the identification of these patents.
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. Shenyang Chemical Research Institute Co., Ltd.
Participated in the drafting of this standard. Pesticide Co., Ltd. Jiangsu Feng Deng, Qantas Jiangsu Agrochemical Co., Ltd. Limin Chemical Company Limited
Secretary, Jiangsu hard Chemical Co., Ltd.
The main drafters of this standard. High Scenic, Zan Yan Kun, Shen Jian, Gengrong Wei, Zhang Ruifang, Liu Mulan, Chen Jie.
Pyrimethanil SC
1 Scope
This standard specifies the pyrimethanil SC requirements, test methods and marking, labeling, packaging, storage and transportation, the guarantee period.
This standard applies to the suspension of pyrimethanil pyrimethanil original drug with suitable additives and fillers processed into.
Note. Other name, structural formula and basic physicochemical parameters pyrimethanil see Appendix A.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
Determination of GB/T 1601 Pesticides pH value
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB 3796 pesticide packaging General
GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD)
GB/T 8170-2008 revised value represents about rules and limit values and judgment
GB/T 14825 method for determination of pesticide suspension
GB/T 16150 pesticide powder, wettable powder fineness measurement method
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 pyrimethanil original drug, additives and fillers processed and should be mobile, easy to measure the volume of liquid suspension, deposit
Discharge may occur during precipitation, but after shaking, restitution should, there should be no lumps.
3.2 Technical Specifications
Pyrimethanil SC shall meet the requirements of Table 1.
Table 1 pyrimethanil SC Control Project Index
project
index
20% 30% 40%
Pyrimethanil mass fraction /% 20.0 40.0 2.0-2.0 1.5-1.5 1.2-1.2 30.0
pH range 6.0 to 10.0
Suspension rate /% ≥ 90
Table 1 (continued)
project
index
20% 30% 40%
Pourability /%
After pouring the residue ≤ 5.0
After washing the residue ≤ 0.5
Wet sieve test (through 75μm test sieve) /% ≥ 98
Persistent foaming (foam volume after 1min)/mL ≤ 30
Low temperature stability of a /% qualified
Thermal storage stability of a /% qualified
When a normal production, low temperature stability, thermal storage stability test was measured at least once every three months.
Test Method 4
Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make
With those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations.
4.1 General provisions
This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in
water. Test results determined in accordance with GB/T 8170-2008 4.3.3 Rounding the value comparison method.
4.2 Sampling
According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determining sample package using a random number table method; the final sample size
Not less than 600mL.
4.3 Identification Test
HPLC --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyrimethanil. In the same chromatographic operating conditions
, The retention time of the standard solution and the sample solution to a peak of pyrimethanil retention time, the relative difference should be less than 1.5%.
Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyrimethanil. Under the same chromatographic operating conditions, the test
The retention time of the sample solution and the standard solution to a peak of pyrimethanil retention time, the relative difference should be less than 1.5%.
When using the above method for identification of effective ingredients have questions, other effective methods can be used for identification.
4.4 Determination of the mass fraction of pyrimethanil
4.4.1 Method summary
Sample dissolved in mobile phase, methanol aqueous phosphoric acid as the mobile phase, use as filler to C18 stainless steel column and UV detector
(300nm), the sample of Pyrimethanil high performance liquid chromatography, external standard. It can also be measured using gas chromatography, chromatography operation
See Appendix B. for conditions
4.4.2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Phosphoric acid;
Pyrimethanil standard. Known pyrimethanil mass fraction w≥98.0%.
4.4.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor;
Column. 250mm × 4.6mm (id) stainless steel column contents C18,5μm filler;
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Quantitative sample line. 5μL;
Ultrasonic cleaner.
4.4.4 HPLC operating conditions
Mobile phase. [Psi] [methanol. water (adjusted with phosphoric acid to pH = 3)] = 75.25, filtered through a filter membrane and degassed;
Flow rate. 1.0mL/min;
Column temperature. room temperature;
Detection wavelength. 300nm;
Injection volume. 5μL;
Retention time. pyrimethanil about 5.5min.
It said operating parameters are typical, according to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results.
Typical pyrimethanil SC HPLC is shown in Figure 1.
1 --- pyrimethanil.
Figure 1 pyrimethanil SC high performance liquid chromatogram
4.4.5 measuring step
4.4.5.1 Preparation of standard solution
Weigh pyrimethanil standard 0.1g (accurate to 0.0001g), a 50mL volumetric flask, add the mobile phase was shaken mobile phase and dilute to
Mark and shake. With pipette 5mL said test solution to another 50mL volumetric flask mobile phase and dilute to the mark.
4.4.5.2 Preparation of sample solution
Weigh containing pyrimethanil 0.1g sample (accurate to 0.0001g), a 50mL volumetric flask, add the mobile phase was shaken with dilute phase flow
Release to the mark. With pipette 5mL said test solution to another 50mL volumetric flask mobile phase and dilute to the mark. through
Membrane filter.
4.4.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Pyrimethaml peak area relative change
After less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.4.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution Pyrimethanil peak areas are averaged. Sample Pyrimethanil
The mass fraction according to equation (1).
w1 = A2
· M1 · w
A1 · m2
(1)
Where.
w1 --- sample pyrimethanil mass fraction, expressed as a percentage;
A2 --- sample solution, pyrimethanil amine mean peak area;
m1 --- standard mass in grams (g);
w --- Sample pyrimethanil mass fraction, expressed as a percentage;
A1 --- standard solution, pyrimethanil amine mean peak area;
m2 --- sample mass, in grams (g).
4.4.7 allowable difference
Pyrimethanil parallel determination of the mass fraction of the difference between the two results, the 20% pyrimethanil content should be less than 0.5%, and 30% of the mass fraction of Pyrimethanil
The number should be less than 0.6%, 40% pyrimethanil content should not exceed 0.8%, respectively, the arithmetic mean value as a measurement result.
Determination of 4.5 pH value
According to GB/T 1601 carried out.
4.6 Determination of the suspension rate
According to GB/T 14825 performed. Weigh 1g sample (accurate to 0.0001g). The cylinder with 50mL methanol remaining 25mL suspended
Floating liquid and precipitate all transferred to 100mL volumetric flask with methanol to the mark, under ultrasonic oscillations 5min, shake, filtration.
4.4 Determination of pyrimethanil according to quality, calculate the suspension rate (gas chromatography. the inner cylinder remaining 25mL suspension and sediment transfer all
To 100mL beaker, vacuum drying oven at 60 ℃ to nearly dry, measurement method, see Appendix B pyrimethanil quality, calculate the hanging
Floating rate).
4.7 Test dumping
4.7.1 Method summary
Will be placed in the container suspending sample placed after a certain time, in accordance with the procedure laid dumping determined trapped in the sample container
Volume; the vessel was washed with water, the amount of the sample container and then measured.
4.7.2 Instruments
With ground joint stopper cylinder. 500mL ± 2mL, cylinder height 39cm, the upper and lower scale spacing 25cm (or equivalent for the determination of dumping
Other containers of).
4.7.3 measuring step
Mix well enough samples, some of which will be placed in time already weighed cylinder (including plug), and attached to the cylinder volume of 8
Office, plug
Tight grinding gag, weighed, placed 24h. The tap is opened, the upright position of the rotating cylinder by a 135 °, pouring 60s, then invert 60s, re-weighed amount
Tube and stopper.
Would be equivalent to 80% of the cylinder volume of water (20 ℃) was poured into a measuring cylinder, stoppered plug grinding mouth, the cylinder upside down 10 times, according to the above tilting operation
Pour the contents of the third weighing cylinder and a stopper.
4.7.4 Calculation
The residue mass fraction and mass fraction of the residue washed after dumping respectively formula (2) and (3) Calculated.
w2 = m2-m0m1-m0
(2)
w3 = m3-m0m1-m0
(3)
Where.
The residue mass fraction w2 --- after dumping, expressed as a percentage;
After m2 --- dumping, quality cylinder, grinding gag and residue, in grams (g);
m0 --- cylinder, quality is more important after grinding gag constant in units of grams (g);
m1 --- cylinder, grinding gag and quality of the sample, in grams (g);
The residue mass fraction w3 --- washed in%;
--- Washing m3, the quality of the cylinder, grinding gag and residue, in grams (g).
4.8 wet sieve test
According to GB/T 16150 in the "wet sieve method".
4.9 Persistent foaming
4.9.1 Method summary
The samples and standards prescribed amount of mixing hard water, foam volume after standing record.
4.9.2 Reagents
Standard hard water. ρ (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0.
4.9.3 Instruments
Stoppered cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom plug
4cm ~ 6cm);
Balance. a sense of the amount of 0.1g, range 500g.
4.9.4 measuring step
The cylinder is added to 180mL standard hard water scale line at set cylinder on balance, weighed into the sample 1.0g (accurate to 0.1g), added to hard water
Plug from the cylinder to the mark at the bottom of 9cm, back cover plug for the bottom of the cylinder as the center, upside down 30 times (2s). On test bench
On standing 1min, record lather volume.
4.10 Low temperature stability test
According to GB/T 19137 method "suspension formulation" provision was. 4.8 Determination by wet sieve test, and the results meet the standard requirements
qualified.
4.11 Thermal storage stability test
According to GB/T 19136 in "liquid formulation" to. After the thermal storage, pyrimethanil content should not be lower than the measured thermal storage mass fraction ago
97% rate is still suspended shall meet the standards.
4.12 Product inspection and acceptance
Shall comply with GB/T 1604's.
5 marking, labeling, packaging, storage, security, guarantee
5.1 marking, labeling, packaging
Pyrimethanil suspending signs, labels, packaging shall comply with the provisions of GB 3796.
Pyrimethanil SC packaging applications, clean, dry cover with plastic bottles, net weight 80g, 100g, 200g. also may
According to user requirements or other forms of ordering agreement package, subject to the provisions of GB 3796.
5.2 Storage
Pyrimethanil SC package should be stored in well-ventilated, dry coffers. Storage and transportation to prevent moisture and sun, not with food, seeds,
Feed-mixing, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.3 Security
Pyrimethanil as low toxicity fungicides, are swallowed and inhaled toxic, irritating to the eyes, the FDA should wear protective equipment, after application
Wash with soap, if ingested, immediately sent to hospital symptomatic treatment.
5.4 Warranty Period
Under the specified conditions of storage, pyrimethanil guarantee amine suspension of two years from date of manufacture.
Appendix A
(Informative)
Other names pyrimethanil, structural formula and basic physicochemical parameters
This product is an active ingredient pyrimethanil other name, structural formula and basic physicochemical parameters are as follows.
ISO common name. Pyrimethanil
CAS Registry Number. 53112-28-0
CIPAC Numeric Code. 714
Chemical name. N- (4,6- dimethyl-pyrimidin-2-yl) aniline
Structure.
Empirical formula. C12H13N3
Molecular Weight.199.25
Biological activity. bactericidal
Melting point. 96.3 ℃
Vapor pressure (25 ℃). 2.2 × 10-3Pa
Solubility (20 ℃, g/L). water 0.121 (pH = 6.1,25 ℃), 389 acetone, ethyl acetate, 617, 1000 dichloromethane, n-hexane
23.7, 412 toluene, methanol 176
Stability. Stability in water pH dependent, 54 ℃ save 14d stability.
Appendix B
(Informative)
Pyrimethanil mass fraction of gas chromatographic method
B.1 Method summary
Sample was dissolved in dimethylformamide, di-n-butyl phthalate as the internal standard, using a HP-5 capillary column for the filler and hydrogen
Flame ionization detector, the sample of Pyrimethanil and measured by gas chromatography, internal standard.
B.2 Reagents and solutions
dimethylformamide;
Pyrimethanil standard. a known mass fraction w≥98.0%;
Internal standard. di-n-butyl phthalate, should not interfere with the analysis of impurities;
Internal standard solution. Weigh-n-butyl phthalate 3.5g, set 250mL flask, dissolved in dimethyl formamide and diluted to
Mark and shake.
B.3 Instruments
Gas chromatograph. with a hydrogen flame ionization detector;
Chromatography or chromatography workstation processor;
Column. 30m × 0.32mm (id) capillary column bonded HP-5 (5% phenyl methyl silicone), a film thickness of 0.25μm.
B.4 GC operating conditions
Temperature (℃). 180 column temperature, the gasification chamber 250, the detector chamber 260;
Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300;
Injection volume. 1.0μL;
Retention time (min). 3.9 pyrimethanil, internal standard 6.3.
Said gas chromatography system operating conditions typical operating parameters. It is given the operating parameters adjusted as appropriate depending on the characteristics of the instrument to
To obtain the best results. Typical pyrimethanil SC and the internal standard gas chromatography is shown in Figure B.1.
1 --- pyrimethanil;
2 --- internal standard.
Figure B.1 pyrimethanil SC and the internal standard gas chromatograph
B.5 measuring step
B.5.1 preparation of standard solution
Weigh pyrimethanil standard 0.05g (accurate to 0.0001g), placed in a glass bottle with a stopper with a pipette 5mL internal standard solution,
Shake well.
Preparation B.5.2 the sample solution
Weigh sample containing about Pyrimethaml 0.05g (accurate to 0.0001g), and placed in a stoppered glass vial with pipette 5mL internal standard solution
Liquid, shake.
B.5.3 Determination
Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle pyrimethanil and the internal standard peak area
The ratio of repeatability to be two adjacent needles Pyrimethaml relative change compared with the internal standard peak area of less than 1.2%, the standard sample solution in accordance with the specimen
Solution, sample solution, the order of the standard solution was measured.
B.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution pyrimethanil and the internal standard peak area ratio of the average, respectively.
Pyrimethanil sample mass fraction w1 (%) according to equation (B.1) Calculated.
w1 =
r2 · m1 · w
r1 · m2
(B.1)
Where.
w1 --- sample pyrimethanil mass fraction, expressed as a percentage;
r2 --- sample solution, pyrimethanil and mean internal standard peak area ratio;
m1 --- standard mass in grams (g);
w --- Sample pyrimethanil mass fraction, expressed as a percentage;
r1 --- standard solution, pyrimethanil and mean internal standard peak area ratio;
m2 --- sample mass, in grams (g).
B.7 allowable difference
Pyrimethanil parallel determination of the mass fraction of the difference between the two results, the 20% pyrimethanil content should be less than 0.5%, and 30% of the mass fraction of Pyrimethanil
The number should be less than 0.6%, 40% pyrimethanil content should not exceed 0.8%, respectively, the arithmetic mean value as a measurement result.
......
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