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GB 22171-2008: [GB/T 22171-2008] 15% paclobutrazol wettable powders
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[GB/T 22171-2008] 15% paclobutrazol wettable powders
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GB 22171-2008
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Basic data | Standard ID | GB 22171-2008 (GB22171-2008) | | Description (Translated English) | [GB/T 22171-2008] 15% paclobutrazol wettable powders | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 10,139 | | Date of Issue | 2008-07-11 | | Date of Implementation | 2009-01-01 | | Quoted Standard | GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 5451; GB/T 14825; GB/T 16150; GB/T 19136 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 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 15% wettable powder MET requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to MET original drug, fillers and additives suitable for the processing of 15% of the MET WP. | GB 22171-2008: [GB/T 22171-2008] 15% paclobutrazol wettable powders---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.
15% paclobutrazol wettable powders
ICS 65.100.20
G25
National Standards of People's Republic of China
Paclobutrazol 15% WP
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.
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.
Participated in the drafting of this standard. Sichuan Chemical Industry Research and Design Institute, Jiang Su Jiannong pesticides Chemical Co., Ltd., Jiang Su Qizhou green
Engineering Co., Ltd., Jiangsu sword licensing pesticides Chemical Co., Ltd.
The main drafters of this standard. to Xu Wei, Zhang Xuebing, Xing Hong, Duan Xiu Hong, Xu Xiangsheng, Chenru Juan, Zhou Jianhua, Hu Chunhong.
The standard commission Secretariat of National Pesticide Standardisation Technical Committee responsible for the interpretation.
Paclobutrazol 15% WP
Other name, structural formula and basic physicochemical parameters of the active ingredient paclobutrazol product as follows.
ISO common name. Paclobutrazol
CAS Registry Number. [76738-62-0]
Chemical name. (2RS, 3RS) -1- (4- chlorophenyl) -4,4-dimethyl -2- (1H-1,2,4- triazol-1-yl) pentan-3-ol
Structure.
Empirical formula. C15H20ClN3O
Molecular Weight. 293.8 (according to 2005 international relative atomic mass)
Biological activity. Plant Growth Regulator
Melting point. 165 ℃ ~ 166 ℃
Vapor Pressure. 1μPa (20 ℃)
The relative density (25 ℃). 1.22
Solubility (20 ℃, g/L). water, 2.6 × 10-2, 110 acetone, cyclohexanone, 180, 100 methylene chloride, hexane 10, xylene 60,
150 methanol, propylene glycol 50
Stability. 20 ℃ storage stable for more than 2 years; 50 ℃ stored for 6 months or more stable; stable at pH4 ~ pH9 water; at pH7 conditions
10d does not degrade under UV light
1 Scope
This standard specifies 15% Paclobutrazol wettable powder requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the processing by the MET original drug, fillers and additives suitable from 15% Paclobutrazol wettable powder.
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 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB 3796 pesticide packaging General
GB/T 5451 WP Pesticide wettability measurement method
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
3 Requirements
3.1 Composition and appearance. This product should be compliant MET original drug with suitable additives and fillers processed into for loose uniform composition
Powder, there should be no lumps.
3.2 15% Paclobutrazol wettable powder shall comply with the requirements in Table 1.
Table 1 15% Paclobutrazol wettable powder control project indicators
Item Index
MET mass fraction /% 15.0 ± 1.0
Suspension rate /% ≥ 75
Moisture /% ≤ 2.0
pH range 6.0 to 10.0
Wetting time/s ≤ 90
Fineness (through 44μm standard sieve) /% ≥ 98
Thermal storage stability test a qualified
When a normal production, heat storage stability test every three months at least once.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 "on solid preparation sampling" approach. Determining sample package using a random number table method; the final sample size
Not less than 300g.
4.2 Identification Test
Liquid chromatography --- The identification test can be carried out simultaneously with the determination of MET Quality Score. Under the same chromatographic operating conditions, the test
The retention time of the sample solution and the standard solution to a peak in the MET peak 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 MET Quality Score. Under the same chromatographic operating conditions, the test
The retention time of the sample solution and the standard solution to a peak in the MET peak retention time, the relative difference should be less than 1.5%.
Determination of the mass fraction of 4.3 MET
4.3.1 Liquid Chromatography (Arbitration Act)
4.3.1.1 Method summary
Sample was dissolved in methanol, methanol - acetonitrile - water as mobile phase, the choice of Nova-pakC18,5μm stuffing column and UV variable
Wavelength detector to sample the MET liquid chromatography separation and determination.
4.3.1.2 Reagents and solutions
Methanol. HPLC grade;
Acetonitrile. chromatographic pure;
Water. The new secondary steam distilled water;
MET standard. a known mass fraction ≥99.0%.
4.3.1.3 Instruments
LC. a variable wavelength UV detector and quantitative injection valve;
Chromatographic data processor or chromatography workstation;
Column. 3.9mm (i.d.) × 150mm stainless steel columns, built-Nova-pakC18,5μm filler (or with the same column efficiency
Other reversed phase columns);
Ultrasonic bath;
Filter. filter pore size of about 0.45μm;
Micro Injector. not less than 50μL.
4.3.1.4 LC operating conditions
Mobile phase. ψ (CH3OH.CH3CN.H2O) = 35.20.45;
The mobile phase flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 230nm;
Injection volume. 10μL;
Retention time (min). 4-H 3.8 MET, MET Ⅱ body 6.3, 7.7 MET, chlorine trazodone 9.6.
HPLC 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 liquid chromatograph Paclobutrazol 15% wettable powder shown in Figure 1.
1 --- 4-H MET;
2 --- MET Ⅱ body;
3 --- MET;
4 --- chlorine trazodone.
Figure 1 LC 15% Paclobutrazol wettable powder
4.3.1.5 Measurement procedure
4.3.1.5.1 preparation of standard solution
Weigh MET standard 0.10g (accurate to 0.0002g), a 50mL volumetric flask, add 40mL of methanol, in an ultrasonic
Bath sonication 5min. Remove cooled to room temperature, add methanol to volume, shake; pipette imbibe 5mL, set another
50mL volumetric flask, add methanol to volume, shake.
4.3.1.5.2 preparation of the sample solution
Weigh the sample 0.07g (accurate to 0.0002g), a 50mL volumetric flask, add 40mL of methanol, in an ultrasonic bath
Sonication 5min. Removed, cooled to room temperature, add methanol to volume, shake; filtered through a membrane filter pore size of about 0.45μm.
4.3.1.5.3 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 MET relative peak area
After the change is less than 1.0%, according to the order of the standard solution, sample solution, sample solution, standard solution injection analysis.
4.3.1.6 Calculation
The two needle sample solution measured before and after the peak area of the sample and two doses of the standard solution MET are averaged. Sample pleiotropic
Azole mass fraction of 1 (%) according to equation (1).
(1)
Where.
A1 --- the average peak area of standard solution MET;
The average peak area A2 --- MET in the sample solution;
--- Paclobutrazol standard mass fraction, expressed as a percentage.
4.3.1.7 allowable difference
The difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.
4.3.2 Gas Chromatography
4.3.2.1 Method summary
Sample was dissolved in chloroform to triphenylmethane as the internal standard, using a HP-5 (5% + 95% diphenyl dimethyl polysiloxane) painted walls
Quartz capillary column and flame ionization detector to sample the MET gas chromatography separation and determination.
4.3.2.2 Reagents and solutions
Chloroform;
Triphenylmethane. Do not interfere with the analysis of impurities;
Internal standard solution. Weigh 5.8g triphenylmethane, in 1000mL volumetric flask with chloroform dissolved and diluted to scale, shake;
MET standard. a known mass fraction ≥99.0%.
4.3.2.3 Instruments
Gas chromatograph. with a hydrogen flame ionization detector;
Column. 30m × 0.32mm (i.d.) Quartz capillary column, wall coated HP-5 (5% diphenyl + 95% dimethyl polysiloxane), membrane
Thick 0.25μm;
Chromatographic data processor or chromatography workstation.
4.3.2.4 GC operating conditions
Column compartment temperature (temperature programming). initial 200 ℃, holding 8min; then to 20 ℃/min temperature is increased up to 250 ℃, 7min maintained;
Gasification chamber temperature. 280 ℃;
Detector temperature. 280 ℃;
Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300, the compensation gas (N2) 25;
Split ratio. 40.1;
Injection volume (μL). 1.0;
Retention time (min). internal standard 5.0, chlorine trazodone 5.6, 6.9 MET, MET MET Ⅱ body 7.3,4-H 15.1.
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. A typical gas chromatogram of 15% Paclobutrazol wettable powder shown in Figure 2.
1 --- internal standard;
2 --- chlorine trazodone;
3 --- MET;
4 --- MET Ⅱ body;
5 --- 4-H MET.
Figure 2 Gas chromatogram MET 15% wettable powder
4.3.2.5 Measurement procedure
4.3.2.5.1 preparation of standard solution
Weigh MET standard 0.10g (accurate to 0.0002g), was placed in a 15mL stoppered glass bottle with a pipette accurately added
10mL internal standard solution, dissolve, shake.
4.3.2.5.2 preparation of the sample solution
Weigh the sample 0.67g (accurate to 0.0002g), was placed in a 15mL stoppered glass vial with 4.3.2.5.1 and with a pipette
Accurate internal standard solution was added 10mL dissolved, shake.
4.3.2.5.3 Determination
Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculate the MET needle and the internal standard peak area
Repeatability than when the relative changes in the MET standard peak area ratio of less than 1.2%, according to the standard solution, sample solution to be two adjacent needles,
The sample solution, the order of the standard solution was measured.
4.3.2.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution MET and the internal standard peak area ratios were averaged. test
MET sample mass fraction of 1 (%) according to equation (2).
1 = γ2
(2)
Where.
γ1 --- standard solution, MET and the internal standard peak area ratio of the average;
γ2 --- sample solution, MET and the internal standard peak area ratio of the average;
--- Paclobutrazol standard mass fraction, expressed as a percentage.
4.3.2.7 allowable difference
Twice the difference between the results of the mass fraction of MET parallel determination, should be less than 0.5%, the arithmetic mean value as a measurement result.
4.4 Determination of the suspension rate
4.4.1 Liquid Chromatography (Arbitration Act)
4.4.1.1 Measurement procedure
According to GB/T 14825 performed. Weigh 1.0g sample (accurate to 0.0002g). The cylinder with 60mL methanol remaining 25mL
Suspension and precipitate all transferred to 100mL volumetric flask, ultrasonic oscillating 5min, cooled to room temperature, methanol was added to volume,
Shake; filtered through a membrane filter pore size of about 0.45μm. 4.3.1 Determination of which MET quality.
4.4.1.2 Calculation
Suspension rate 2 (%) calculation formula shown below.
111.1 (3)
(5)
Where.
A1 --- the average peak area of standard solution MET;
A2 --- the average peak area of MET by the remaining 25mL sample solution and precipitate suspension formulated in;
1 --- MET sample mass fraction, expressed as a percentage;
--- Paclobutrazol standard mass fraction, expressed as a percentage.
4.4.1.3 allowable difference
The difference between two parallel determination results shall not be greater than 5% of the arithmetic mean as a measurement result.
4.4.2 Gas Chromatography
4.4.2.1 Measurement procedure
According to GB/T 14825 performed. Weigh 1.0g sample (accurate to 0.0002g). With 60mL of water remaining in the cylinder of 25mL
Suspension and precipitate all transferred to 100mL beaker. After drying the beaker on the 100 ℃ ± 2 ℃ oven or boiling water bath, and
4.3.2.5.1 pipette with an accurate internal standard solution was added 10mL dissolved, shake. 4.3.2 Determination by which MET quality.
4.4.2.2 Calculation
Suspension rate 2 (%) is calculated as follows.
111.1 (6)
(8)
Where.
γ1 --- standard solution, MET and the internal standard peak area ratio of the average;
γ2 --- by the remaining 25mL sample solution and precipitate suspension formulated after drying, the MET and the internal standard peak area ratio
average value;
1 --- MET sample mass fraction, expressed as a percentage;
--- Paclobutrazol standard mass fraction, expressed as a percentage.
4.4.2.3 allowable difference
The difference between two parallel determination results shall not be greater than 5% of the arithmetic mean as a measurement result.
4.5 Determination of Moisture
According to GB/T 1600 in the "azeotropic distillation method".
According to GB/T 1601 carried out.
4.7 Determination of wetting time
According to GB/T 5451 carried out.
4.8 fineness
According to GB/T 16150 in the "wet sieve method".
4.9 Thermal storage stability test
According to GB/T 19136 in "powder formulations" to. MET after the heat storage mass fraction, the suspension was still in line with the requirements for qualified 3.2.
4.10 Product inspection and acceptance
Shall comply with GB/T 1604's. Limit numerical processing using rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 15% Paclobutrazol wettable powder marking, labeling, packaging, should meet the requirements of GB 3796.
5.2 15% Paclobutrazol wettable powder applied to clean, dry, lined with plastic woven bag, net weight 25kg or 50kg.
5.3 According to user requirements or ordering agreement, you can use other forms of packaging, subject to the provisions of GB 3796.
5.4 15% Paclobutrazol wettable powder package should be stored in well-ventilated, dry coffers.
5.5 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.6 Safety. This product is a low-toxic pesticides, are swallowed and inhaled toxic. When using this product to wear goggles and rubber gloves and other necessary
Protective clothing. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. Coverage were immediately sent to hospital for treatment.
5.7 Warranty. under specified conditions of storage, 15% wettable powder MET guarantee, from date of manufacture for 2 years.
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