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[GB/T 28126-2011] Imidacloprid technical material
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GB 28126-2011
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Basic data | Standard ID | GB 28126-2011 (GB28126-2011) | | Description (Translated English) | [GB/T 28126-2011] Imidacloprid technical material | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.10 | | Word Count Estimation | 10,150 | | 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 | | Adopted Standard | FAO specification 582/TC-2006, MOD | | 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 imidacloprid, test methods and marking, labeling, packaging, storage and acceptance period. This standard applies to imidacloprid and its impurities generated in the production of imidacloprid. |
GB 28126-2011: [GB/T 28126-2011] Imidacloprid technical material---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.
Imidacloprid technical material
ICS 65.100.10
G25
National Standards of People's Republic of China
Imidacloprid
Published 2011-12-30
2012-04-15 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China issued
Foreword
This standard in Chapter 3, Section 5 is mandatory, the rest are recommended.
This standard was drafted in accordance with rules GB/T 1.1-2009 given.
This draft standard method using the reformed modified using FAOspecification582/TC (May2006) "imidacloprid"
The main technical differences and the reasons are as follows.
--- This increases the control over the standard loss on drying, pH value range, dimethylformamide insolubles, more comprehensive index item, the FAO
Specifications not control these three indicators.
Please note that some of the content of this document may involve patents. The issuing authority of this document does not assume responsibility to identify these patents.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Pesticide Standardization Technical Committee (SAC/TC133).
This standard is drafted. Shenyang Chemical Research Institute Co., Ltd.
Participated in the drafting of this standard. Jiangsu Changqing Agrochemical Co., Ltd., Nanjing Red Sun Co., Ltd., Zhejiang Hisun Chemical Co.
Co., Ltd., Jiangsu Suke Sheng Group Co., Ltd., Qingdao Hailier Pharmaceutical Co., Ltd.
The main drafters. Hou Chunqing, Zan Yan Kun, Lvliang Zhong, Liu Kuitao, Wang Tiansheng, WANG Chun-ling, Jerry incense, Li Xuechen.
Imidacloprid
1 Scope
This standard specifies the requirements, test methods and marking, labeling, packaging, storage and acceptance of imidacloprid the original drug.
This standard applies to imidacloprid and imidacloprid impurities generated in the production thereof.
Note. The other name, structural formula and basic physicochemical parameters of imidacloprid see Appendix A.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
Determination 1601 pH value pesticides GB/T
GB/T 1604 pesticide regulations for acceptance of goods
GB/T 1605-2001 sampling commercial pesticides
GB 3796 pesticide packaging General
3.1 Appearance
White to beige powder, without visible foreign matter.
3.2 Technical Specifications
Imidacloprid should also meet the requirements of Table 1.
Table 1 imidacloprid Control Project Index
Item Index
Imidacloprid content /% ≥ 97.0
Loss on drying /% ≤ 0.5
The pH range of 5.0 to 8.0
Dimethylformamide insolubles mass fraction a /% ≤ 0.2
When a normal production, dimethylformamide insolubles content was measured at least once every three months.
Test Method 4
4.1 Sampling
Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determining Sample packages with a random number table method; final sample size
Not less than 100g.
4.2 Identification Test
The present liquid chromatography --- identification test can be conducted simultaneously with the determination of the mass fraction of imidacloprid. Chromatography under the same operating conditions, the test
Main peaks in the retention time of the sample solution and the standard solution imidacloprid retention time of the peaks, the relative difference should be less than 1.5%.
Infrared spectroscopy --- imidacloprid standard sample and the infrared 4000cm -1 ~ 400cm-1 absorption spectrum range should not significantly
the difference. Imidacloprid standard infrared spectra of Figure 1.
FIG 1 imidacloprid standard IR spectrum
4.3 Determination of the content of Imidacloprid
4.3.1 Method summary
Sample dissolved in mobile phase, methanol and water as mobile phase, used as a filler C18 stainless steel column and UV detector wavelength
At 260nm, of the sample imidacloprid RP-HPLC separation and determination, external standard.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Imidacloprid Sample. A known mass fraction w≥99.0%.
4.3.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column. 250mm × 4.6mm (id) stainless steel column, the contents C18,5μm filler;
Filter. membrane pore size of about 0.45 m;
Microsyringe. 50μL;
Quantitative sampling tube. 5μL;
Ultrasonic cleaning.
4.3.4 HPLC operating conditions
Mobile phase. [Psi] (methanol. water) = 40.60, by membrane filtration, and degassing;
Flow rate. 0.8mL/min;
Column temperature. room temperature (temperature change should be less than 2 deg.] C);
Detection wavelength. 260nm;
Injection Volume. 5μL;
Retention time. imidacloprid 6.0min.
Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.
Typical HPLC imidacloprid shown in Figure 2.
1 --- imidacloprid.
FIG 2 FIG imidacloprid original drug HPLC
4.3.5 Determination Step
4.3.5.1 Preparation of standard solution
0.1 g of weighed (accurate to 0.0002g) imidacloprid in Sample 100mL volumetric flask, dissolved in methanol and diluted to the mark, ultrasonic
5min shaken to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with the mobile
Phase was diluted to the mark.
4.3.5.2 Preparation of sample solution
Containing 0.1 g of imidacloprid was weighed (accurate to 0.0002g) sample in 100mL volumetric flask, dissolved in methanol and diluted to the mark, ultra
5min sonication to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with
Mobile phase and dilute to the mark.
4.3.5.3 Determination
Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two adjacent pins relative change in peak area imidacloprid
After less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.3.5.4 computing
The two needle and the sample solution was measured before and after the two doses of the standard sample solution and peak areas were averaged imidacloprid. Imidacloprid sample
Mass fraction by formula (1).
w1 = A2
· M1 · w
A1 · m2
(1)
Where.
W1 --- imidacloprid sample mass fraction in%;
A2 --- sample solution, imidacloprid average peak area;
M1 --- imidacloprid standard mass in grams (G);
W --- the mass fraction of imidacloprid standard sample, expressed in%;
A1 --- the standard solution, the average peak area imidacloprid;
--- M2 sample mass, in grams (g).
4.3.6 allows poor
The difference between the results of two replicates imidacloprid content should not exceed 1.2%, and the arithmetic mean value as a measurement result.
Determination of loss on drying 4.4 mass fraction
4.4.1 Instruments and Appliances
Weighing bottle. diameter 50mm, height 20mm;
Oven. 105 ℃ ± 2 ℃;
Dryer.
4.4.2 Determination Step
The weighing bottle placed in an oven bake IH, then cooled to room temperature in a desiccator, weighed (accurate to 0.0002g). Repeating the above steps
Step, until a constant weight weighing bottle. 10g weighed into a weighing bottle in a sample, paving weighed (accurate to 0.0002g). The weighing bottle back into the oven
Me, IH bake uncovered, capped, removed and placed in a desiccator was cooled to room temperature, weigh (accurate to 0.0002g). Repeating the above operation,
Weighing bottle and the sample until a constant weight.
4.4.3 computing
Drying loss mass fraction in a sample according to the formula (2).
w2 = m1-m2m × 100
(2)
Where.
--- drying loss mass fraction w2 of the sample, expressed in%;
M1 --- sample mass before drying and weighing bottles in grams (G);
--- M2 sample mass after drying and weighing bottles in grams (G);
--- m sample mass, in grams (g).
4.4.4 allows poor
The measurement results of the two parallel relative deviation should not exceed 30%, and the arithmetic mean value as a measurement result.
4.5 pH value measured
Carried out in GB/T 1601.
Determination of insoluble material content of the amide methyl two 4.6
4.6.1 Reagents
dimethylformamide.
4.6.2 Instruments
Erlenmeyer flasks. glass with ground joints, 250mL;
Sand core glass crucible. G3;
Oven. 110 ℃ ± 2 ℃.
4.6.3 Determination Step
Sample Weigh 10g (accurate to 0.01g), placed in 250mL Erlenmeyer flask, 60mL of dimethylformamide was added, shaken to all
Solution was taken, filtered through a crucible constant weight solution, and then dimethylformamide 60mL conical flask was washed three times, and suction filtered. The crucible set
Dried in an oven 30min, then cooled to room temperature and weighed.
Dimethylformamide insolubles fraction of mass (3) is calculated according to the formula.
w3 = m1-m0m × 100
(3)
Where.
W3 --- dimethylformamide insolubles content, expressed in%;
After constant weight mass M1 --- crucible and the insolubles in grams (G);
M0 --- crucible mass in grams (G);
--- m sample mass, in grams (g).
4.6.4 allows poor
The measurement results of the two parallel relative deviation should not exceed 30%, and the arithmetic mean value as a measurement result.
4.7 product testing and acceptance
Product inspection and acceptance shall comply with GB/T 1604's. Process limit values using rounding value comparison method.
5 marking, labeling, packaging, storage, security, acceptance period
5.1 marking, labeling, packaging
Flag imidacloprid, labeling and packaging should comply with the provisions of GB 3796. Imidacloprid original medicinal lined iron drum, barrel, net weight
Generally 50kg, 100kg or 200kg. Other forms may also be packed according to the requirements of the protocol or order, subject to
The provisions of GB 3796.
5.2 Storage
Imidacloprid package airiness, dry place. Storage and transportation, to prevent moisture and sunlight, no food, seed, feed
Feed mix, to avoid contact with the skin, eyes, mouth and nose to prevent inhalation.
5.3 Security
This is a moderately toxic pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product
Necessary to wear protective clothing. After application with soap and rinse with water. Coverage should be immediately sent to hospital for symptomatic treatment.
5.4 Acceptance of
Acceptance of imidacloprid for a month. From the date of delivery, product quality inspection completed within one month, the indicators should be
Meet the standards.
Appendix A
(Informative)
Other names, formulas and basic physicochemical parameters of imidacloprid
Other names, structural formulas and physicochemical parameters of the product basic active ingredient imidacloprid is as follows.
ISO common name. Imidacloprid
CAS Registry Number. 138261-41-3
CIPAC Numeric Code. 582
Chemical name. 1- (6-chloro-3-pyridylmethyl) -N- nitromethylene-imidazol-2-yl-amine
Structure.
Empirical formula. C9H10ClN5O2
Molecular weight. 255.7
Biological activity. insecticide
Melting point. 144 ℃
Vapor pressure (20 ℃). 4 × 10-7mPa
Solubility (20 ℃, g/L). water 0.61, 0.68 toluene, methylene chloride 55, 1.2 isopropanol, n-hexane is less than 0.1
Stability follows. pH of 5 to 11 stable, hard to be hydrolyzed.
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