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GB 28153-2011: [GB/T 28153-2011] Thiosultap-monosodium water soluble powders
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[GB/T 28153-2011] Thiosultap-monosodium water soluble powders
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Basic data
Standard ID: GB 28153-2011 (GB28153-2011)
Description (Translated English): [GB/T 28153-2011] Thiosultap-monosodium water soluble powders
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.10
Word Count Estimation: 11,131
Date of Issue: 2011-12-30
Date of Implementation: 2012-04-15
Quoted Standard: GB/T 601; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 6682-2008; GB/T 8170-2008; GB/T 19136
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 Monosultap soluble powders, test methods and marking, labeling, packaging, storage and warranty. This standard applies to monosultap original drug, suitable additives and fillers Monosultap processed into soluble powder.
GB 28153-2011: [GB/T 28153-2011] Thiosultap-monosodium water soluble 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.
Thiosultap-monosodium water soluble powders
ICS 65.100.10
G25
National Standards of People's Republic of China
Monosultap soluble powders
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. Zhejiang Bo Shida Technology Co. crop Jiang Su Tianrong Group Co., Ltd., Jiangsu Ampang electrochemical
Co., Ltd. Jiangsu Feng Deng pesticides.
The main drafters of this standard. Meibao Gui, Zhang Xuebing, Xuli Ting, Wang Qiang, Jiang Yutian, Gengrong Wei, Li Maoqing.
Monosultap soluble powders
1 Scope
This standard specifies the requirements Monosultap soluble powders, test methods and marking, labeling, packaging, storage and warranty.
This standard applies to Monosultap soluble powders by the Shachongdan original drug, suitable additives and fillers processed into.
Note. Other name, structural formula and basic physicochemical parameters Monosultap 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.
Preparation of GB/T 601 chemical reagent standard titration solution
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 19136 Determination of Pesticide Thermal storage stability
3 Requirements
3.1 Composition and appearance
This product should be compliant Monosultap original drug is made, the appearance of a homogeneous powder, without clumps.
3.2 Technical Specifications
Monosultap soluble powders should meet the requirements of Table 1.
Table 1 Monosultap soluble powders Control Project Index
Thermal storage stability test a qualified
When a normal production, the degree of dissolution and solution 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. The test standard titration solution, did not indicate when the other requirements, according to GB/T 601 requirements preparation and calibration. test result
Determination of GB/T 8170-2008 4.3.3 Rounding the value comparison method.
4.2 Sampling
According to GB/T 1605-2001 "on solid preparation sampling" approach. Determined by sampling a random number table method packages, the final sample size
Not less than 300g.
4.3 Identification Test
HPLC --- The identification test can be carried out simultaneously with the determination of the mass fraction of Shachongdan. In the same chromatographic operating conditions
, The sample solution to a chromatographic retention time and Monosultap standard solution Shachongdan chromatographic retention time should be relative difference
1.5% or less.
4.4 Determination of the mass fraction of Shachongdan
4.4.1 Method summary
Sample dissolved in mobile phase, methanol aqueous potassium dihydrogen phosphate (pH7.0) as the mobile phase, to use as filler AgilentTCC18
Stainless steel column and UV detector (220nm), the sample of Shachongdan reverse phase high performance liquid chromatography, external standard.
4.4.2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Potassium hydroxide solution. c (KOH) = 2mol/L;
Potassium dihydrogen phosphate. c (KH2PO4) = 0.035mol/L, potassium hydroxide solution with a pH value adjusted to 7.0;
Monosultap standard. a known mass fraction w≥99.0%.
4.4.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column. 250mm × 4.6mm (id) stainless steel column, built AgilentTCC18,5μm filler (or with equivalent effect
Column);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Quantitative sample line. 10μL;
Ultrasonic cleaner.
4.4.4 HPLC operating conditions
Mobile phase. Ψ (methanol. potassium dihydrogen phosphate) 5.95, with 0.45μm filter membrane, ultrasound 10min spare;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 220nm;
Injection volume. 10μL;
Retention time. 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 Monosultap soluble powders HPLC is shown in Figure 1.
1 --- Monosultap.
Figure 1 Monosultap Soluble Powder by HPLC diagram
4.4.5 measuring step
4.4.5.1 Preparation of standard solution
Weigh 0.1g (accurate to 0.0002g) Shachongdan standard, a 50mL volumetric flask, dissolved in mobile phase and dilute to the mark,
Shake well.
4.4.5.2 Preparation of sample solution
Take a sample containing said Monosultap 0.1g (accurate to 0.0002g), and a 50mL volumetric flask, dissolved in mobile phase and dilute to the mark
Degree, shake.
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 Monosultap 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 Monosultap peak areas are averaged. Sample Monosultap
The mass fraction according to equation (1).
w1 --- Monosultap sample mass fraction, expressed as a percentage;
A2 --- sample solution Monosultap mean peak area;
Sample mass m1 --- Shachongdan in grams (g);
w --- Monosultap standard mass fraction, expressed as a percentage;
A1 --- Sample mean peak area in Monosultap solution;
m2 --- sample mass, in grams (g).
4.4.7 allowable difference
Monosultap fraction relatively poor quality of two parallel determination results shall not be greater than 1.5%, the arithmetic mean value as a measurement result.
4.5 Determination of the mass fraction of sodium chloride
4.5.1 Method summary
Samples dissolved in water, with nitric acid and hydrogen peroxide to destroy thiosulfate and Monitoring for interfering substances, with its ferric ammonium sulfate for directions
Agents, sodium chloride content was measured using the method of silver.
4.5.2 Reagents and solutions
Sucrose solution. ρ = 250g/L;
Silver nitrate standard solution. c (AgNO3) = 0.1mol/L;
Ammonium thiocyanate standard titration solution. c (NH4SCN) = 0.1mol/L;
Nitric acid solution. φ (HNO3) = 50%;
Hydrogen peroxide solution. w (H2O2) = 30%;
Ammonium ferric sulfate saturated solution (add a few drops of sulfuric acid).
4.5.3 Determination
Weigh 1.0g sample (accurate to 0.0002g), placed in 250mL conical flask, nitric acid solution 40mL, 10mL peroxide
Hydrogen solution and 80mL water, heating micro-boiling 10min, cooled to room temperature. Burette with the standard solution of silver nitrate was added 15mL, shake. plus
8mL into the sucrose solution, shaken vigorously 2min, add 1mL ferric ammonium sulfate indicator under shaking with ammonium thiocyanate standard titration solution titration
The solution was light brown to red and remain unchanged at the end of 30s.
4.5.4 Calculation
Sample mass fraction of sodium chloride according to formula (2).
Mass fraction w2 --- sodium chloride in the sample, expressed in%;
c1 --- the actual concentration of silver nitrate standard solution, the unit is mol per liter (mol/L);
Vl --- standard solution of silver nitrate by volume in milliliters (mL of);
c2 --- the actual concentration of ammonium thiocyanate standard titration solution, expressed in moles per liter (mol/L);
V2 --- consumption volume of ammonium thiocyanate standard titration solution, in milliliters (mL);
--- The M NaCl molar mass in grams per mole (g/mol), [M (NaCl) = 58.45g/mol];
M --- the quality of the sample, in grams (g).
4.6 Determination of loss on drying
4.6.1 Instruments
Oven. 105 ℃ ± 2 ℃;
Weighing bottle. diameter 70mm, height 40mm;
Dryer.
4.6.2 measuring step
The weighing bottle placed in an oven bake 1h, was brought out in a desiccator to cool to room temperature, weigh (accurate to 0.0002g). Repeat the above steps
Step, until constant weight weighing bottle. Place the sample in the bottle 2g, paving, weighed (accurate to 0.01g), the weighing bottle placed in an oven, without
Cover and bake 1h, remove and put in the dryer to cool to room temperature, weighed (accurate to 0.0002g).
4.6.3 Calculation
Loss on drying the sample according to equation (3) Calculated.
W3 --- Loss on drying of the sample, expressed in%;
Mass m1 --- weighing bottle and sample before drying, in grams (g);
Mass m2 --- weighing bottle and sample after drying, in grams (g);
M --- the quality of the sample, in grams (g).
4.6.4 allowable difference
The relative deviation of two parallel determination results shall not be greater than 30%; the arithmetic mean value as a measurement result.
Determination of 4.7 pH value
According to GB/T 1601 carried out.
4.8 degree of dissolution and solution stability
4.8.1 Method summary
The sample was dissolved in dissolution degree is 25 ℃ standard hard water, invert 15 times, standing 5min, filtered through a 75μm test sieve, quantitative measurement
Given the sieve residue. The solution stability is the solution to stand after 18h, again using the test sieve, sieve residue quantitatively determined.
4.8.2 Instruments
Standard sieve. aperture 75μm, diameter 76mm;
Stoppered cylinder. between 250mL (0mL ~ 250mL scale distance 20cm ~ 21.5cm, 250mL graduated from the line and the bottom plug
From a 4cm ~ 6cm);
Standard hard water. ρ (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0.
4.8.3 Preparation of sample solution
In the graduated cylinder was added 250mL 2/3 standard hard water, its temperature was adjusted to 25 ℃, 5g of the sample, a standard hard water added to the mark.
Stoppered. Standing 30s, inverted measuring cylinder 15 times by hand, is reset. Reversed, once used by the reset time should not exceed 2s.
4.8.4 5min after test
The sample solution was allowed to stand in the cylinder after 5min ± 30s, on into the constant weight 75μm sieve, and the filtrate was collected 500mL burn
Cup, reserved for the next test. 20mL graduated cylinder with distilled water five times, all insolubles were quantitatively transferred to a sieve, discard the washing liquid,
Check the sieve residue. If there is residue on the sieve, sieve 60 ℃ dried to constant weight, weighed in.
4.8.5 18h after the test
The filtrate was allowed to stand 18h, carefully observe whether the precipitation filtrate in the beaker. If there are insoluble materials, and then the sample was constant weight of 75μm
Test sieve was filtered, washed with 20mL of distilled water 5 times sieves, if there exists a solid or crystalline sieve, sieve and dried at 60 deg.] C to a constant
Heavy, weighing.
4.8.6 Calculation
5min after the mass fraction of residue according to formula (4) Calculated.
Mass fraction w4 --- 5min after residues, expressed in%;
Quality and test sieve residue after m2 --- 5min, in grams (g);
Quality test sieve constant weight after m1 --- 5min, in grams (g);
M --- the quality of the sample, in grams (g).
After 18h mass fraction residue according to formula (5) Calculated.
Mass fraction w5 --- 18h after the residue, expressed in%;
m2 sieve test mass and residues --- 18h, the units of grams (g);
m1 mass of test sieve after constant weight --- 18h, the units of grams (g);
M --- the quality of the sample, in grams (g).
4.9 Thermal storage stability test
According to GB/T 19136 "other agents" to. After Monosultap thermal storage mass fraction should not be less than the mass fraction of the former reservoir Monosultap
97%.
4.10 Product inspection and acceptance
Shall comply with GB/T 1604's.
5 marking, labeling, packaging, storage, security and guarantee period
5.1 marking, labeling, packaging
Monosultap soluble powder marking, labeling and packaging should comply with the provisions of GB 3796; Monosultap soluble powders applied to clean, dry, lined
Woven plastic bags or aluminum foil bag. Bulk bag net weight of 25kg. Small Package net weight 20g, 50g, 100g. and also
According to user requirements or ordering protocols use other forms of packaging, subject to the provisions of GB 3796.
5.2 Storage
Monosultap soluble powder package should be stored in ventilated, dry warehouse; 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
Nereistoxin Monosultap is a moderately toxic pesticides. Toxic if swallowed or inhaled all, it can penetrate through the skin. The FDA
You should wear protective gloves, gas masks, wear clean protective clothing. After application, immediately wash with soap and water. In case of poisoning, immediately
Sent to hospital for treatment, the antidote atropine; do artificial respiration if necessary.
5.4 Warranty Period
Under the specified storage conditions Shachongdan guarantee soluble powder, two years from date of manufacture.
Appendix A
(Informative)
Monosultap Other name, structural formula and basic physicochemical parameters
Other name, structural formula and basic physicochemical parameters of the active ingredients of this product Monosultap follows.
Generic Name. Monosultap
ISO common name. Thiosultap-monosodium
Chemical Name. Dimethyl monohydrate - Hydrogen-2- (1,3-disulfonate monosodium sulfopropyl) ammonium
Structure.
Empirical formula. C5H14NO7S4Na
Molecular Weight. 351.42
Biological activity. Insecticidal
Melting point. 142.5 ℃ (decomposition)
Solubility (g/L, 25 ℃). 500 water, 20 of methanol, acetone and 2.5 × 10-4
Stability. at 50 ℃ sealed storage stability.
......
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