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GB 15955-2011 English PDF

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GB 15955-2011: [GB/T 15955-2011] Gibberellic acid technical material
Status: Valid

GB 15955: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
GB 15955-2011English239 Add to Cart 3 days [Need to translate] [GB/T 15955-2011] Gibberellic acid technical material Valid GB 15955-2011
GB 15955-1995English239 Add to Cart 2 days [Need to translate] Gibberellins technical Obsolete GB 15955-1995

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Basic data

Standard ID GB 15955-2011 (GB15955-2011)
Description (Translated English) [GB/T 15955-2011] Gibberellic acid technical material
Sector / Industry National Standard
Classification of Chinese Standard G25
Classification of International Standard 65.10.30
Word Count Estimation 9,960
Date of Issue 2011-12-30
Date of Implementation 2012-04-15
Older Standard (superseded by this standard) GB 15955-1995
Quoted Standard GB/T 613-2007; GB/T 1604; GB/T 1605-2001; GB 3796
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 original drug gibberellic acid requirements, test methods and marking, labeling, packaging, storage and acceptance period. This standard applies to gibberellic acid and its impurities generated in the production of gibberellic acid composition of the original drug.

GB 15955-2011: [GB/T 15955-2011] Gibberellic acid technical material

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Gibberellic acid technical material ICS 65.10.30 G25 National Standards of People's Republic of China Replacing GB 15955-1995 Gibberellic acid original drug 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. Since the implementation of this standard, instead of GB 15955-1995 "GA original drug." The main differences between standard and GB 15955-1995 "GA original drug" as follows. --- "GA" to "gibberellic acid"; --- Canceled and classification; --- Gibberellic acid to the mass fraction ≥90.0%; --- Loss on drying by the "≤1.0%" to "≤0.5%"; --- Specific rotation to specific rotation ability αm (20 ℃, D) ≥ 80 (°) · m2/kg. Please note that some of the content of this document may involve patents. Release mechanism of the present 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 was drafted. the Ministry of Agriculture, Zhejiang Qianjiang Biochemical Co., Ltd., Shanghai with Swiss biotechnology Limited Secretary, Jiangxi Ruifeng Sheng Chemical Co., Ltd. The main drafters of this standard. Wang Xiaoli, Li Youshun, Chentie Chun, Zhao Yonghui, Yu Rong, Zhu Jianxin, Chenming Lei, Lu love sun. Gibberellic acid original drug

1 Scope

This standard specifies requirements for gibberellic acid original drug, test methods and marking, labeling, packaging, storage and acceptance period. This standard applies to the impurities generated by the production of gibberellic acid, and gibberellic acid composition of the original drug. Note. Other name, structural formula and basic physicochemical parameters of gibberellic acid in 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. GB/T 613-2007 General method for determination of chemical reagents specific rotation ability (specific optical rotation) GB/T 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB 3796 pesticide packaging General

3 Requirements

3.1 Composition and appearance This product should gibberellic acid and impurities generated in the production of the composition, it should be white to light yellow crystalline powder, free from visible foreign matter and filling Modifier. 3.2 Project and indicators Gibberellic acid original drug should be consistent with the requirements in Table 1. Table 1 gibberellic acid original drug control project indicators Item Index Gibberellic acid mass fraction /% ≥ 90.0 Loss on drying /% ≤ 0.5 The specific rotation ability αm (20 ℃, D)/[(°) · m2/kg] ≥ 80 Test Method 4 4.1 Sampling According to GB/T 1605-2001 "on the original drug product sampling" approach. Random sampling method is determined by the package, the final amount of sample lot At 100g. 4.2 Identification Test The identification test can be carried out simultaneously with the determination of the mass fraction of gibberellic acid. Under the same chromatographic operating conditions, the main sample solution chromatogram Retention time and peak standard solution of gibberellic acid chromatographic peak retention time, the relative difference should be less than 1.5%. 4.3 Determination of the mass fraction of gibberellic acid 4.3.1 Method summary Sample dissolved in mobile phase, methanol - phosphoric acid as the mobile phase, use as filler to C18 stainless steel column and UV detector, for Gibberellic acid in the sample by reverse phase HPLC separation and determination of external standard. 4.3.2 Reagents and solutions Phosphoric acid. AR; Methanol. HPLC grade; Water. The new secondary steam distilled water; Phosphoric acid. [Psi] (water. phosphoric acid) = 2000.1; Gibberellic acid standard sample. a known mass fraction w≥98.0%. 4.3.3 Instruments High performance liquid chromatography. a variable wavelength UV detector and quantitative injection valve; Chromatographic data processor or chromatography workstation; Column. 250mm × 4.6mm (id) stainless steel column, built ZORBAX80ÅEXTENDC18 filler (or equivalent Other column effect); Micro injector. 100μL; Filter. filter pore size of about 0.45μm; Ultrasonic cleaner. 4.3.4 HPLC operating conditions Mobile phase. [Psi] (methanol. aqueous phosphoric acid solution) = 35.65; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 210nm; Injection volume. 10μL. Retention time. gibberellic acid about 8.2min. HPLC operating conditions described above, the Department of typical operating parameters, according to the characteristics of different instruments, given operating parameters to make appropriate adjustments to To obtain the best results. Typical gibberellic acid original drug HPLC is shown in Figure 1. 1 --- gibberellic acid. Figure 1 HPLC gibberellic acid original drug 4.3.5 measuring step 4.3.5.1 preparation of standard solution Weigh gibberellic acid standard about 0.05g (accurate to 0.0002g), placed in 100mL flask, add 35mL of methanol to dissolve, then Phosphoric acid aqueous solution was diluted to the mark. 4.3.5.2 preparation of the sample solution Weigh a sample containing about 0.05g of gibberellic acid (accurate to 0.0002g), placed in 100mL flask, add 35mL of methanol to dissolve, Phosphoric acid aqueous solution and then diluted to the mark. Filtered through a 0.45μm pore size filters. 4.3.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles gibberellic acid peak area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured. 4.3.6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution of gibberellic acid peak area were averaged. Sample gibberellic acid The mass fraction according to equation (1). w1 = A2 · M1 · w A1 · m2 (1) Where. w1 --- sample gibberellic acid content, expressed as a percentage; A2 --- sample solution, gibberellic acid, the average peak area; m1 --- gibberellic acid standard mass values in grams (g); Mass fraction w --- standard samples gibberellic acid, expressed in%; A1 --- standard solution, gibberellic acid, the average peak area; Numerical m2 --- sample mass, in grams (g). 4.3.7 allowable difference The difference between two parallel determination results shall not be greater than 1.5%, the arithmetic mean value as a measurement result. 4.4 Determination of loss on drying 4.4.1 Instruments and Appliances Oven. 105 ℃ ± 2 ℃; Weighing bottle. diameter 50mm, height 20mm; Dryer. 4.4.2 measuring step The weighing bottle placed in 105 ℃ ± 2 ℃ oven baking 1h, and then into the dryer to cool to room temperature, weighed (accurate to 0.0002g). Repeat the above steps until constant weight weighing bottle. In weighing bottle was weighed into a 1g sample (paved weighed accurate to 0.0002g). Will be referred Flask placed in an oven, bake uncovered 1h, the lid is removed and placed in the dryer to cool to room temperature, weighed (accurate to 0.0002g). 4.4.3 Calculation Loss on drying of the sample according to equation (2). w2 = m1-m2m (2) Where. w2 --- Loss on drying, 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). 4.5 Determination of specific rotation ability Performed according to GB/T 613-2007 requirements. Wherein the solution to be tested is gibberellic acid ethanol solution of the original drug at a concentration of 0.1g/mL. As solution After the sample is turbid solution was found, after application of rapid quantitative determination of filter paper. Sample specific rotation ability αm (20 ℃, D) [(°) · m2/kg], According to equation (3) Calculated. αm (20 ℃, D) = 100 · Α · V m 1-0.01w () 2 l (3) Where. α --- measured rotation angle in degrees (°); The V --- volume of the sample dilution in milliliters (mL of); M --- the quality of the sample, in grams (g); W2 --- Loss on drying of the sample, expressed in%; --- optical tube length L, the unit decimeter (dm). 4.6 product testing and acceptance Shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method. 5 marking, labeling, packaging, storage, security, acceptance of 5.1 mark, label Gibberellic acid original drug marking, labeling and packaging should comply with the provisions of GB 3796. 5.2 Packaging Gibberellic acid original drug is appropriate, clean, dry metal pail lined with plastic, cardboard, aluminum foil or plastic bucket bag, net weight of each piece is generally 25kg. According to user requirements or the order agreement, the use of other forms of packaging, it should comply with the provisions of GB 3796. 5.3 Storage Gibberellic acid original drug package should be stored in ventilated, cool, dry coffers, fire, moisture, and can not be in the open air with toxic substances, flammable Explosive materials and basic materials stacked together. Not with food, seeds, feed mixed release. Storage and transportation to prevent moisture and sun, and rain to avoid collision, away from fire. 5.4 Security This product is a low toxicity plant growth regulator. The FDA should wear protective gloves, masks, wearing clean protective clothing. Not with the use of basic Mixed goods, can not be mixed with ammonia, calcium polysulfide, soda ash and the like. Used with the distribution, once dubbed the aqueous solution can not go far. Immediately after use with Wash water. In case of poisoning, should go to hospital for treatment. 5.5 Acceptance of Acceptance of gibberellic acid original drug is a month. From the date of delivery, product quality inspection completed within a month, the indicators should meet Combined standards.

Appendix A

(Informative) Other names gibberellic acid, structural formula and basic physicochemical parameters This product is an active ingredient gibberellic acid is another name, structural formula and basic physicochemical parameters are as follows. ISO common name. Gibberelicacid CIPAC Numeric Code. 307 CAS Registry Number. 77-06-5 Chemical name. (1α, 2β, 4aα, 4bβ, 10β) -2,4a, 7- trihydroxy-1-methyl-8-methyl-3-ene-1,10-gibberellic acid -1 , 4a- Lactone Structure. Empirical formula. C19H22O6 Molecular Weight. 346.4 Biological activity. Plant Growth Regulator Melting point. 223 ℃ ~ 225 ℃ (decomposition) Solubility. water 5g/L (room temperature). Soluble in methanol, ethanol, acetone, alkaline aqueous solution, slightly soluble in diethyl ether and ethyl acetate, insoluble Chloroform. Its potassium, sodium, ammonium salts soluble in water (potassium salt 50g/L) Stability. At room temperature in a dry state is stable, slow degradation in aqueous or aqueous alcohol solution in, DT50 (20 ℃) about 14d (pH3 ~ 4), 14d (pH7), alkali metal will be converted into less biologically active compounds, the case of thermal decomposition.

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