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Chemical Industry Standard of the People's Republic of China
HG2676-95
4% Gibberellin Emulsifiable Concentrate
Published on April 5, 1995
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1996www.bzxz.net
Chemical Industry Standard of the People's Republic of China
4% Gibberellin Emulsifiable Concentrate
Subject Content and Scope of Application
HG2676-95
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of 4% Gibberellin Emulsifiable Concentrate. This standard applies to the emulsifiable concentrate prepared by adding emulsifiers to the mother liquor left after the Gibberellin extract is concentrated and crystallized to precipitate the Gibberellin original drug.
Cited standards
GB/T1600
GB/T1601
GB/T1603
GB/T1604
GB/T1605
GB3796
GB4838
Determination of moisture content in pesticides
Determination of pH value in pesticides
Determination of stability of pesticide emulsions Method
Pesticide acceptance rules
Commercial pesticide sampling methods
General rules for pesticide packaging
EC pesticide packaging
GB/T6682
GB8170
Technical requirements
3.1 Appearance
Analytical laboratory water specifications and test methods numerical rounding rules
Brown stable liquid, no visible suspended matter and precipitation. 3.24% gibberellin emulsifiable concentrate should meet the requirements of the following table. Item
Gibberellin content, μg/mL
Water, %
Emulsion stability (diluted 500 times)
Low temperature stability\)
Hot storage stability2
Note: 1) and 2) should be sampled at least once every six months. 4 Test method
Unless otherwise specified, the reagents used in this test are all analytically pure reagents, and the water should meet the third-grade water specifications in GB/T6682. 4.1 Appearance inspection
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996
Visual observation method.
4.2 Determination of gibberellins
4.2.1 Identification test
HG2676-95
This identification test can be carried out simultaneously with the determination of gibberellins content. Pipette 1mL of the sample solution into a test tube, add an appropriate amount of concentrated sulfuric acid, shake gently, and observe against the light. Blue-green fluorescence can be seen. 4.2.2 Determination of Gibberellin Content
4.2.2.1 Method Summary
Gibberellin reacts with concentrated sulfuric acid, and its degradation product produces blue fluorescence under ultraviolet light. Within a certain concentration range (i.e., between 1 and 18 μg per mL), the intensity of the fluorescence is proportional to the concentration of gibberellin. 4.2.2.2 Reagents and Solutions
Absolute ethanol (GB/T678);
Sulfuric acid (GB/T625);
Gibberellin Standard Sample: Known Gibberellic Acid GA: Content above 98%: Fluorescent Yellow Sodium Salt;
Preparation of 0.2mg/L Fluorescent Yellow Sodium Standard Solution: Weigh 50mg of fluorescent yellow sodium salt (accurate to 0.2mg), place in a 500mL volumetric flask, dilute to the mark with distilled water, shake to make a 100mg/stock solution; store away from light (shelf life 2 months). When using, accurately pipette 2mL of the stock solution into a 1000mL brown volumetric flask, dilute to the mark with distilled water, and shake to hook. This is the 0.2mg/L standard solution (shelf life 1 week). Use this solution to calibrate the zero point of the fluorometer. 4.2.2.3 Instruments
Stoppered glass test tube: 25×200mm;
Fluorescence spectrophotometer.
4.2.2.4 Determination steps
a Preparation of standard solution
Weigh 50mg of gibberellin standard (accurate to 0.2mg), place in a 50mL volumetric flask, dissolve and dilute to the mark with anhydrous ethanol, and shake well; accurately pipette 1mL of this solution into a 100mL volumetric flask, dilute to the mark with anhydrous ethanol, and shake to hook. The concentration c (ug/mL) of the standard solution is calculated according to formula (1):
o= m1X1000XW= 0. 2m:w
50X100
Wherein: m1——mass of gibberellin standard, mg, -content of gibberellin standard, %.
b. Preparation of sample solution
Accurately pipette 5.0mL of sample into a stoppered glass test tube, add 15.0mL of anhydrous ethanol with a burette, and shake well; pipette 1.0mL into another stoppered glass test tube, add 9.0mL of anhydrous ethanol with a burette, and shake well. Pipet 1.0mL from this test tube into a 100mL volumetric flask, dilute to the mark with anhydrous ethanol, and shake well for later use. c. Determination of the sample
Accurately pipette 1.0mL of the sample solution into a stoppered glass test tube, and then accurately pipette 1.0mL of the standard solution into a stoppered glass test tube of the same size, and add 1.0mL of anhydrous ethanol to each and shake well. Place the stoppered glass test tube in an ice water bath to cool for 10 minutes, and then slowly add 18mL of concentrated sulfuric acid pre-cooled to 0℃ along the tube wall with a burette (the addition speed is controlled at about 6 minutes). After about 10 minutes, take out the glass test tube, gently rotate and shake well, place it in a 2528℃ constant temperature box for 1 hour, then take it out, place it at room temperature for 10 minutes, and pour the solution into a 10mm colorimetric cell. Measure the fluorescence value of the solution on a fluorescence photometer, and calibrate the fluorescence meter positioning value with a standard solution of fluorescent yellow sodium. 4.2.2.5 Calculation:
The gibberellin content X in the sample (ug/mL) is calculated according to formula (2): Xi
(2)
Where: E. Fluorescence value of the sample solution;
E.——Fluorescence value of the standard solution;
c——Concentration of the standard solution, ug/mL; N—Dilution volume of the sample, mL,
V——Amount of the sample absorbed, mL.
4.2.2.6 Allowable difference
HG2676-95
The difference between the two determination results should not be greater than 0.2×10μg/mL. 4.3 Determination of moisture
According to the Karl-Fries method in GB/T1600. The sample weighing is 0.3～0.6g (accurate to 0.0002g). 4.4 Determination of pH value
According to the pH meter method in GB/T1601.
4.5 Determination of emulsion stability
According to GB/T1603, the dilution multiple of the emulsifiable concentrate is 500 times. 4.6 Determination of low temperature stability
Weigh about 50g of the sample into a 100mL beaker, put it into an ice water bath, and place it at a temperature of (0±1)℃ for 1h. During the placement period, stir it once every 15min for 30s each time. Check whether there is solid or oily matter precipitated in the cup. If there is no solid or oily matter precipitated, it is qualified. 4.7 Determination of thermal storage stability
4.7.1. Instrument
Oven: temperature control accuracy is ±2℃;
Ampoule: capacity is 30mL, long neck.
4.7.2 Determination
Use a medical syringe to draw 10mL of sample and inject it into a clean and dry ampoule (note: do not let the sample touch the neck of the ampoule). Place the ampoule in an ice bath and seal it with a gas lamp (or alcohol lamp). (Note: Avoid solvent evaporation when sealing) Seal at least 4 bottles, weigh the sealed ampoules and put them into a metal container, and then place them in a (54 ± 2) ℃ oven. After 14 days of storage, take out the ampoules from the oven, cool and weigh them. If there is no leakage, it can be measured, and the content separation rate is not more than 5% to be qualified. 5 Inspection rules
5.1 Sampling method
Carry out in accordance with the GB/T1605 "sampling of emulsions and liquid states" method. Determine the sampling package by random method; the final sampling volume is not less than 100mL.
5.2 Acceptance rules
Acceptance is carried out in accordance with GB/T1604 standards.
6 Marking, packaging, transportation and storage
6.1 The packaging and marking of 4% gibberellin emulsion should comply with the relevant provisions of GB3796 and GB4838. 6.24% gibberellin emulsifiable concentrate should be packaged in brown glass bottles or plastic bottles with stoppers and caps, 100mL per bottle. Use shockproof net sleeves, foam plastics or corrugated paper as cushions, and arrange them tightly in calcium plastic boxes, cartons or wooden boxes, 100 bottles per box. 6.3 Other forms of packaging can also be used according to user requirements or agreements reached between supply and demand parties, but they must comply with the relevant provisions of GB4838.
6.4 Avoid impact and rain during transportation, and keep away from fire. Be careful when handling, loading and unloading. 6.5 The package should be stored in a cool, dry place; fireproof and moisture-proof, and must not be stacked in the open air with toxic substances, flammable and explosive materials and alkaline substances.
6.6 Warranty period: Under the specified storage and transportation conditions, the warranty period for 4% gibberellin emulsifiable concentrate in good packaging is at least 23
HG2676-95
years from the date of production. During the warranty period, the gibberellin content meets the requirements of this standard. Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shanghai Pesticide Research Institute, and the Huaxin Biochemical Products Factory of the Ministry of Nuclear Industry, the 18th Shanghai Pharmaceutical Factory, the Zhejiang Haining Pesticide Factory, and the Chengdu Pharmaceutical Machinery Factory of the Ministry of Agriculture participated in the drafting. The main drafters of this standard are Ye Wenbing, Wang Yonglan, Guo Jiwen, Gu Ximei, Hao Xiang, and Xu Jiayan.
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