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GB 28154-2011: [GB/T 28154-2011] 75% Nicosulfuron water dispersible granules
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[GB/T 28154-2011] 75% Nicosulfuron water dispersible granules
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Basic data
| Standard ID | GB 28154-2011 (GB28154-2011) |
| Description (Translated English) | [GB/T 28154-2011] 75% Nicosulfuron water dispersible granules |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | G25 |
| Classification of International Standard | 65.100.20 |
| Word Count Estimation | 11,174 |
| Date of Issue | 2011-12-30 |
| Date of Implementation | 2012-04-15 |
| Quoted Standard | GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 5451; GB/T 6682-2008; GB/T 8170-2008; GB/T 14825-2006; GB/T 16150; GB/T 19136 |
| Adopted Standard | FAO specifications 709/WG-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 Nicosulfuron WDG requirements, test methods and marking, labeling, packaging, storage, guarantee period. This standard applies to Nicosulfuron original drug, carriers and processing aids made ??Nicosulfuron water dispersible granule. |
GB 28154-2011: [GB/T 28154-2011] 75% Nicosulfuron water dispersible granules
---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.
75% Nicosulfuron water dispersible granules
ICS 65.100.20
G25
National Standards of People's Republic of China
75% Nicosulfuron WG
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 FAO Specifications 709/WG (May2006) "nicosulfuron water dispersible granules."
This standard FAO Specification 709/WG (May2006) and the main technical difference Cause "nicosulfuron water dispersible granules" are as follows.
--- This standard suspension rate ≥80%, FAO Specifications predetermined suspension ratio ≥70%;
This standard specifies --- dispersibility (after 1min) ≥90%, FAO Specifications predetermined dispersibility (after 1min) ≥70%;
--- This standard specifies Persistent foaming (foam volume after 1min) is ≤40mL, FAO specifications as prescribed Persistent foaming (1min
After) ≤60mL;
--- This standard size (250μm ~ 1180μm) ≥95%, FAO Specifications predetermined control dust and flowability two indicators, Kam
At present there is no test to these two methods, the present standard two alternative dust and mobility index with product size;
--- The standard controlling the moisture content and pH range of two indicators, FAO specifications uncontrolled these two indicators.
Please note that some of the content of this document may involve patents, the issuing authority of this document does not assume responsibility for identifying these patents.
The standard proposed by China Petroleum and Chemical Industry Federation.
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. Anhui Fengle Agrochemical Co., Ltd., Zibo new agro-based pesticides Chemical Co., Ltd., Hefei Long-agriculture
Development Co., Ltd., Jiangsu Rui Wo Chemical Co., Ltd., Jiangsu Agrochemical Co., Ltd. Qantas.
The main drafters. the bright, Ma Yaguang, Jin Jinsong, Tian Junsheng, Shen canal, Yu Guoxin, Chen Jie.
75% Nicosulfuron WG
1 Scope
This standard specifies nicosulfuron water dispersible granules of requirements, test methods and marking, labeling, packaging, storage, guarantee period.
This standard applies to the processing by the original drug nicosulfuron, carriers and adjuvants nicosulfuron made water dispersible granules.
Note. Other names, structural formulas and physicochemical parameters of the basic nicosulfuron 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.
GB/T 1600 Pesticide Method Moisture
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
GB/T 5451 method for measuring the wettability of agrochemical wettable
GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD)
GB/T 8170-2008 rounding off means about rules and determining limiting values
GB/T 14825-2006 Method for determination of pesticide suspension
GB/T 16150 pesticide powders, wettable powder fineness measurement method
GB T 19136 Determination of heat storage stability of pesticide /
3.1 Composition and appearance
This product should be compliant nicosulfuron the drug and appropriate processing auxiliaries and fillers are made as a dry, free-flowing solid particles
Grain, almost no powder, no lumps visible and extraneous matter.
3.2 Technical Specifications
Nicosulfuron WG should meet the requirements in Table 1.
Table 1 nicosulfuron WDG control program Index
Item Index
Nicosulfuron mass fraction /% 2.5-2.5 75.0
Moisture content /% ≤ 3.0
The pH range of 4.0 to 7.0
TABLE 1 (cont.)
Item Index
Wetting time/s ≤ 20
Fineness (75μm test sieve) /% ≥ 98
Suspension rate /% ≥ 80
Particle size (250μm ~ 1180μm) /% ≥ 95
Dispersibility /% ≥ 90
Persistent foaming (amount of foam after 1min)/mL ≤ 40
Passing a heat storage stability
When a normal production, the thermal storage stability test was measured at least once every three months.
Test Method 4
Safety Tips. to use this standard shall have practical experience of laboratory work. This standard does not indicate any safety issues. Make
With those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the provisions of relevant state laws and regulations.
4.1 General provisions
This standard reagent in the absence of water and other requirements stated, refer to three predetermined analytical reagents and GB/T 6682-2008 of
water. The test results performed by determining 4.3.3 rounding value in comparison 8170-2008 GB/T .
4.2 Sampling
Carried out in GB/T 1605-2001 of "commodity solid preparation sampling" approach. Determining Sample packages with a random number table method; final draw
Sample size should be no less than 1000g.
4.3 Identification Test
The present liquid chromatography --- identification test can be carried out simultaneously with the measurement nicosulfuron mass fraction. Chromatography under the same operating conditions,
Sample solution of a chromatographic peak with a retention time of the standard solution nicosulfuron retention time of the peaks, the relative difference should
1.2% or less.
4.4 Determination of nicosulfuron mass fraction
4.4.1 Method summary
Sample was dissolved in acetonitrile aqueous ammonia solution, acetic acid aqueous acetonitrile as the mobile phase, used as a filler stainless SymmetryC18
Column and a UV detector (240nm), the sample nicosulfuron and high performance liquid chromatography assay.
4.4.2 Reagents and solutions
Acetonitrile (HPLC grade);
Water. The new secondary steam distilled water;
Glacial acetic acid;
Aqueous ammonia (NH3 · H2O). w (NH3) = 26% ~ 30%;
Ammonia solution. Ψ (H2O.NH3 · H2O) = 300.1;
Ammonia solution in acetonitrile. [Psi] (acetonitrile. ammonia solution) = 50.50;
Nicosulfuron Sample. nicosulfuron known mass fraction w≥97.0% (at 105 ℃, 1h drying after use).
4.4.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor or workstation;
Column. 250mm × 4.6mm (id) stainless steel column, SymmetryC18,5μm filler contents (or equivalent effect column);
Filter. membrane pore size of about 0.45 m;
Microsyringe. 50μL;
Quantitative sampling tube. 5μL;
Ultrasonic cleaning.
4.4.4 HPLC operating conditions
Mobile phase. Ψ (CH3CN.H2O) = 40.60, glacial acetic acid adjusted to pH 3.0;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should be less than 2 deg.] C);
Detection wavelength. 240nm;
Injection Volume. 5μL;
Retention time. nicosulfuron about 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 nicosulfuron WDG HPLC is shown in Figure 1.
1 --- nicosulfuron.
FIG 1 nicosulfuron water-dispersible granules by HPLC FIG.
4.4.5 Determination Step
4.4.5.1 Preparation of standard solution
Weigh 0.05g nicosulfuron standard (accurate to 0.0002g), was placed in a 50mL volumetric flask, 40mL of acetonitrile was added aqueous ammonia solution,
To dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaken, ammonia water diluted to the mark with acetonitrile. Pipette with a pipette to the solution
10mL to 50mL volumetric flask, dilute to volume with acetonitrile and aqueous ammonia solution, shake.
4.4.5.2 Preparation of sample solution
Tobacco samples weighed 0.05g of ethyl (accurate to 0.0002g), was placed in a 50mL volumetric flask, 40mL of acetonitrile was added aqueous ammonia solution
Solution, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaken, ammonia water diluted to the mark with acetonitrile. Pipette with a pipette to the solution
10mL to 50mL volumetric flask, dilute to volume with acetonitrile and aqueous ammonia solution, shake.
4.4.5.3 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 needles nicosulfuron peak area becomes relatively
After less than 1.2% of, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.4.6 computing
Sample mass fraction nicosulfuron according to formula (1).
w1 = A2
· M1 · w
A1 · m2
(1)
Where.
W1 --- sample nicosulfuron content, expressed in%;
A2 --- sample solution, nicosulfuron average peak area;
M1 --- Sample mass in grams (G);
W --- nicosulfuron standard mass fraction in%;
A1 --- the standard solution, nicosulfuron average peak area;
--- M2 sample mass, in grams (g).
4.4.7 allows poor
Results replicates difference nicosulfuron content twice, should not exceed 1.2%, and the arithmetic mean value as a measurement result.
4.5 Determination of Moisture
According to GB/T 1600 in the "azeotropic distillation method".
4.6 pH value measured
Carried out in GB/T 1601.
4.7 Determination of the suspension rate
Proceed as GB/T 14825-2006 4.1. Tobacco samples weighed 0.1g of ethyl (accurate to 0.0001g), the remaining
1/10 suspensions and the precipitate was transferred to a 100mL volumetric flask, the residue three times with 25mL of a solution of ammonia in acetonitrile 60mL all
Washed into 100mL volumetric flask, under ultrasonic shaking 5min, cooled to room temperature, the volume, shake, after filtration, was measured according to 4.4 of nicosulfuron
Mass, suspension rate calculated.
4.8 Determination of wetting time
Carried out in GB/T 5451.
4.9 Determination of fineness
According to GB/T 16150 in the "wet sieve method".
Determination of particle size 4.10
4.10.1 Instruments
Group standard sieve. aperture (250μm ~ 1480μm);
Sieve Shaker. amplitude of 25mm, 1400 times/min.
4.10.2 measuring step
The standard sieve vertically stacked, placed in a small sieve large particle size above a particle size sieve, sieve bottoms receiving pan while the combination of a good set of fixed sieve vibrating sieve
Machine, accurately weighed 100g sample taken granules (accurate to 0.1 g of), placed on the top sieve, stamped seal, shock promoter sieve shaker 5min, close
Set within a predetermined size range oversize weighed (to the nearest 0.1g).
4.10.3 computing
The particle size of the sample according to the formula (2).
w2 = m1m × 100
(2)
Where.
--- size w2 of the sample, expressed in%;
--- M1 predetermined oversize mass within the particle diameter range in grams (G);
--- m sample mass, in grams (g).
Determination dispersible 4.11
4.11.1 Method summary
The amount of water in water dispersible granules was added under stirring and mixing to prepare a suspension, after standing for some time, removing a top 9/10
Suspension, suspension and 1/10 bottom drying the precipitate was measured gravimetrically.
4.11.2 reagents and equipment
Standard hard water. ρ (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825-2006 formulation;
Beaker. 1000mL, inner diameter (102 ± 2) mm;
Electric mixer. with speed control (0 ~ 1000) r/min;
Stainless stirring rod. four fixed with a propeller stirring blade stirring bar, the angle between the blades is 45 ° (see FIG. 2);
A rotary vacuum evaporator;
Stopwatch.
In millimeters
FIG 2 stainless stirring rod
4.11.3 measuring step
At 20 ℃ ± 1 ℃, standard hard water was added to the 900mL beaker, stir bar is fixed in the center of the beaker, stirring the beaker from the blade bar
Bottom 15mm, and a stirring blade pitch rotation direction advancing the rod to ensure that the liquid swirls up stir bar, a speed of 300r/min stirring opening
Stirrer, the sample 9g water dispersible granules (to the nearest 0.1g) was stirred in water was added, stirring was continued for 1min. Close stirring, so that hydrostatic suspension
Home 1min, 9/10 withdrawn suspension (810mL), the entire operation should be completed within 30s ~ 60s, slender glass tube and held always tip
In the subsurface, and the suspension is possible without stirring, 90mL of water was distilled off remaining suspension using a rotary vacuum evaporator at 90 ℃ ~ 100 ℃
Dried to constant weight, weighed (to the nearest 0.1g).
4.11.4 computing
Dispersion of the sample according to equation (3) is calculated.
w3 = 10
(M-m1)
9m × 100
(3)
Where.
W3 --- dispersibility of the sample, expressed in%;
m --- the mass of the sample taken, in grams (G);
After mass M1 --- dried residue, in grams (g).
4.12 Persistent foaming test
4.12.1 Method summary
A predetermined amount of sample is mixed with standard hard water, the foam volume recorded on standing.
4.12.2 Reagent
Standard hard water. ρ (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825-2006 formulation.
4.12.3 Instruments and Appliances
Stoppered graduated cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom of the stopper
4cm ~ 6cm);
Industrial balance. a sense of the amount of 0.1g.
4.12.4 measuring step
Was added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a measuring cylinder (to the nearest 0.1 g of), was added to the standard hard water from the cylinder
9cm scale line of the bottom plug, the plug cover to the bottom of the cylinder as the center, upside down 30 times (2s). Standing on the bench
1min, foam volume recorded.
4.13 Thermal storage stability test
According to GB/T 19136 in the "solid preparation" performed. After the heat storage nicosulfuron content should be not less than 95% prior to storage, the suspension was still to be
Meet the standards for qualified.
4.14 product inspection and acceptance
Product inspection and acceptance shall comply with GB/T 1604's.
5 marking, labeling, packaging, storage, security, guarantee period
5.1 marking, labeling, packaging
Flag nicosulfuron water dispersible granules, labeling, packaging should meet the requirements of GB 3796; Nicosulfuron WG woven applications
Clean-lined plastic bags or cardboard drum lined with clean plastic bag, barrel net content is generally 20kg. It can also be based on user
Seeking agreement or order other forms of packaging, subject to the provisions of GB 3796.
5.2 Storage
Nicosulfuron package WDG airiness, dry place; storage and transportation, prevent moisture and sunlight, not with food,
Seed, feed-mixing, avoid contact with the skin, eyes, mouth and nose to prevent inhalation.
5.3 Security
This is a moderately toxic herbicide. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using the 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 Warranty Period
Warranty. Storage conditions specified in, nicosulfuron water dispersible granules guarantee, since two years from the production date.
Appendix A
(Informative)
Smoke Other names, formulas and basic physicochemical parameters of ethyl
This product is an active ingredient of smoke other names, structural formulas and physicochemical parameters of ethyl substantially as follows.
Common name. nicosulfuron
ISO common name. Nicosulfuron
CAS Registry Number. 111991-09-4
Chemical Name. 2- (4,6-dimethoxypyrimidin-2-ylcarbamoyl sulfamoyl) -N, N- dimethyl-nicotinamide
Structure.
Empirical formula. C15H18N6O6S
Molecular weight. 410.4
Biological activity. Herbicides
Melting point. 141 ℃ ~ 144 ℃
Vapor pressure. 1.6 × 10-11Pa (20 ℃)
Solubility (25 ℃, g/kg). Water 3.59 (pH = 5 buffer solution), 12.2 (pH = 7 buffer solution), 39.2 (pH = 9 buffer solution
Solution); acetone 18; Ethanol 4.5; chloroform, dimethylformamide, 64; 23 acetonitrile; toluene 0.37; n-hexane < 0.02; dichloromethane 160
Stability. an aqueous solution at 25 deg.] C to about DT50 15d (pH5), at pH7, pH9 stable.
1102-
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