GB 22600-2008 English PDF

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GB 22600-2008: [GB/T 22600-2008] 2, 4-D butyl technical
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 22600-2008	259	Add to Cart	3 days	[GB/T 22600-2008] 2, 4-D butyl technical	Valid

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Basic data

Standard ID: GB 22600-2008 (GB22600-2008)
Description (Translated English): [GB/T 22600-2008] 2, 4-D butyl technical
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.20
Word Count Estimation: 10,128
Date of Issue: 2008-12-17
Date of Implementation: 2009-06-01
Quoted Standard: GB/T 601; GB/T 1604; GB/T 1605-2001; GB 3796
Adopted Standard: FAO 1.3/TC/S/F-1992, NEQ
Regulation (derived from): Announcement of Newly Approved National Standards No. 21 of 2008 (No. 134 overall)
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 2, 4 butylate original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the 2, 4 butylate and impurities generated in the production of 2, 4 Butyl original drug.

GB 22600-2008: [GB/T 22600-2008] 2, 4-D butyl technical

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2, 4-D butyl technical ICS 65.100.20 G25 National Standards of People's Republic of China 2,4-D butyl ester original drug Posted 2008-12-17 2009-06-01 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. The FAO standards and specifications 1.3/T C/S/F (1992) "2,4-Desterstechnical" of non-equivalent. Appendix A of this standard is an informative annex. Since the implementation of this standard, the original chemical industry standard HG2319-1992 "2,4- butylate original drug" void. 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. Participated in the drafting of this standard. Dalian Songliao Chemical Co., Ltd., Shandong Weifang Rainbow Chemical Co., Ltd., Jiamusi Heilong Pesticide Chemical Co., Ltd., Wing Tai Fung Changzhou Chemical Co., Ltd. The main drafters of this standard. Meibao Gui, Xing Jun, Miao innovation, in bright, Hou Yongsheng Dong Xia, Fang Yun, Chen. Yanggui Qin, Du Jianping. 2,4-D butyl ester original drug Other name, structural formula and basic physicochemical parameters of the active ingredient 2,4-D butyl ester product as follows. ISO common name. 2,4-Dbutyl Chemical Name. 2,4-dichlorophenoxyacetic acid, n-butyl Structure. Empirical formula. C12H14C12O3 Molecular weight. 277.15 (according to 2007 international relative atomic mass) Biological activity. weeding

1 Scope

This standard specifies the 2,4-D butyl ester original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the impurities from the production of 2,4-butyl and the composition of the produced 2,4-butyl ester original drug.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard. Preparation of GB/T 601 chemical reagent standard titration solution 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 Appearance Colorless to brown oily liquid. 3.2 Technical Specifications 2,4-D butyl ester original drug should also meet the requirements of Table 1. Table 1 2,4-D butyl ester original drug control project indicators Item Index Butyl 2,4 mass fraction /% ≥ 92.0 Free phenol content (2,4-DCP meter) /% ≤ 1.0 Acidity (2,4 meter) /% ≤ 1.5 Test Method 4 4.1 Sampling According to GB/T 1605-2001 "on the original drug product sampling" approach. Determined by sampling a random number table method packages, the final sample size Not less than 100g. 4.2 Identification Test Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of 2,4-D butyl ester. In the same chromatographic operating conditions , The retention time of the standard solution and the sample solution to a peak of 2,4-D butyl retention time, the relative difference should be 1.5% Fewer. Infrared spectroscopy --- sample and 2,4-butyl standards in the infrared range 4000cm-1 ~ 400cm-1 absorption spectrum should Ignorance Significant differences. 2,4-D butyl standard infrared spectrum is shown in Figure 1. 1 of butyl 2,4-standard infrared spectrum 4.3 Determination of the mass fraction of 2,4-D butyl ester 4.3.1 Method summary Sample was dissolved in chloroform, di-isobutyl phthalate as internal standard, the use of polyethylene terephthalate and tetrachlorophthalic Apiezon L To fill a stainless steel column and flame ionization detector, the sample of 2,4-butyl ester by gas chromatography separation and determination. also may Determined using capillary gas chromatography, chromatographic operating conditions, see Appendix A. 4.3.2 Reagents and solutions Chloroform; 2,4-D butyl standard. a known mass fraction ≥98.0%; Internal standard. di-iso-butyl phthalate, should not interfere with the analysis of impurities; Internal standard solution. Weigh isobutyl phthalate 3.5g, set 250mL flask, add appropriate amount of chloroform was dissolved and diluted to Mark and shake. 4.3.3 Instruments Gas chromatograph. with a hydrogen flame ionization detector; Chromatography or chromatography workstation processor; Column. 2m × 3mm (i.d.) Stainless steel (glass) columns, built-in 1.7% tetrachlorophthalic polyethylene terephthalate and 0.3% Appius Song L/ChromosorbW-AWDMCS180 ~ 250μm filler; Micro injector. 10μL. 4.3.4 GC operating conditions Temperature (℃). 170 column temperature, the gasification chamber 260, the detector chamber 260; Gas flow rate (mL/min). carrier gas (N2) 20, hydrogen gas 30, air 300; Injection volume. 0.6μL; Retention time (min). 2,4- 11.0 butylate, internal standard 6.7. 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 2,4-D butyl ester original drug and the internal standard gas chromatography is shown in Figure 2. 1 --- internal standard; 2 --- 2,4-D ester. Figure 2 GC-butyl 2,4-drug and internal standard 4.3.5 measuring step 4.3.5.1 Preparation of standard solution Weigh 2,4-butyl standard 0.1g (accurate to 0.0002g), placed in a glass bottle stuffed with a pipette 5mL internal standard solution Liquid, shake. 4.3.5.2 Preparation of sample solution Weigh containing 2,4-D butyl ester 0.1g (accurate to 0.0002g) sample, placed in a glass vial stopper, and 4.3.5.1 with the same Pipette internal standard solution 5mL, shake. 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 needles 2,4-butyl and the internal standard peak adjacent After the area is less than 1.2% relative change, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured. 4.3.5.4 Calculation The measured before and after the two-needle sample solution and two doses of the standard sample solution were 2,4-D butyl ester ratio and the internal standard peak area average. Sample mass fraction of 2,4-D butyl ester 1 (%), according to equation (1). (1) Where. --- Standard samples of 2,4-butyl ester content, expressed as a percentage. 4.3.6 allowable difference Difference butyl 2,4 mass fraction of two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result. 4.4 Determination of free phenols 4.4.1 Method summary The sample was dissolved in ethanol, ammonia, 4-amino-antipyrine and potassium ferricyanide solution color, absorbance was measured at 520nm place. Isolated from the calibration curve of standard sample absorbance at the same volume, calculated free phenol content. 4.4.2 Reagents and solutions 2,4-dichlorophenol standard. a known mass fraction ≥98.0%; Ethanol; Isopropanol; Ethanol, isopropyl alcohol solution. ψ (ethanol. isopropanol. water) = 2.1.3; Ammonia solution. Ba (NH3 · H2O) = 0.1mol/L; 2,4-DCP standard solution. Weigh 2,4-dichlorophenol standard 0.01g (accurate to 0.0002g), placed in 100mL volumetric flask, add A small amount of ethanol to dissolve, diluted with ethanol to the mark; 4-amino-antipyrine solution. ρ = 2g/L; Ferricyanide solution. ρ = 4g/L. 4.4.3 instruments and equipment Spectrophotometer; Microburette. 2mL; Stoppered cylinder. 30mL; Quartz cuvette. 1cm. 4.4.4 measuring step 4.4.4.1 Correction Followed by microburette draw 0.2mL, 0.5mL, 0.8mL, 1.0mL, 1.2mL, 1.5mL, 2.0mL2,4- dichlorophenol standard Sample solution, adding seven stoppered graduated cylinder, fill with ethanol was added to 10mL, then followed by adding 5mL of isopropanol, 5mL ammonia solution, 5mL4- ammonia Karthikeyan antipyrine 5mL aqueous potassium ferricyanide solution. Each addition are required to shake, and the last intense shaking 1min, standing 5min. Quartz cuvette, ethanol isopropyl alcohol solution as the reference absorbance at 520nm measured. Draw 10mL ethanol, according to the procedure described above was added to each solution, determine the reagent blank absorbance. Blank value is subtracted from the phenol solution absorbance measured absorbance, the corresponding volume of phenol solution was plotting a calibration curve. 4.4.4.2 Determination Weigh containing 2,4-D butyl ester 0.2g (accurate to 0.0002g) sample, placed in 100mL flask, add a small amount of ethanol solution Solution, dilute to the mark with ethanol. With a pipette to the solution of 10mL stoppered measuring cylinder and then followed by adding 5mL of isopropanol, 5mL Ammonia solution, 5mL4- amino antipyrine 5mL aqueous potassium ferricyanide solution. Each addition are required to shake, and the last intense shaking 1min, standing 5min. Quartz cuvette, ethanol isopropyl alcohol solution as the reference absorbance at 520nm measured. Minus empty After the absorbance values of white, from the calibration curve of the absorbance corresponding to 2,4-DCP standard solution volume (mL) to detect. 2 free phenol content (%) according to equation (2). (2) Where. Vp --- measured absorbance of the sample corresponding to the volume of phenol solution in milliliters (mL); --- Sample mass fraction of 2,4-dichlorophenol in%. 4.5 Determination of acidity 4.5.1 Method summary Sample was dissolved in ethanol and methyl red as indicator titration with standard sodium hydroxide solution was titrated to yellow. 4.5.2 Reagents and solutions 95% ethanol; Sodium hydroxide standard titration solution Ba (NaOH) = 0.01mol/L, according to GB/T 601 preparation and calibration; Methyl red ethanol solution. ρ (methyl red) = 1g/L. 4.5.3 measuring step Weigh the sample 0.5g (accurate to 0.0002g), placed in a 250mL Erlenmeyer flask, add 95% ethanol 50mL, shake the sample Dissolved. Add 3 drops of methyl red ethanol solution of sodium hydroxide standard titration solution is titrated to a yellow endpoint. Meanwhile blank determination. 4.5.4 Calculation The acidity of the sample 3 (%), according to equation (3) Calculated. 3 = Ba (Vp Vp 1- 0) · M 100 (3) Where. Ba --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L); Vp 1 --- titration of the sample solution volume consumed sodium hydroxide standard titration solution, in milliliters (mL); V0 --- titrate blank solution volume consumed sodium hydroxide standard titration solution, in milliliters (mL); M --- 2,4- drops molar mass in grams per mole (g/mol), [M = 221g/mol]. 4.6 product testing and acceptance Shall comply with GB/T 1604's. Limit the use of numerical treatment rounding value comparison method. 5 marking, labeling, packaging, storage and transportation 5.1 2,4-D butyl sign the original drug, labeling, packaging shall comply with the provisions of GB 3796. 5.2 2,4-D butyl ester original drug packaging applications clean, dry metal pail, barrel net content should be less than 200kg. 5.3 Other forms of packaging may be used according to user requirements or the order agreement, subject to the provisions of GB 3796. 5.4 2,4-D butyl ester original drug package should be stored in well-ventilated, dry coffers. 5.5 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.6 Security. 2,4-D butyl ester as a low toxicity herbicides, inhalation can cause headache, nausea. The FDA should wear protective equipment, after application Wash with soap, if ingested, immediately sent to hospital. 5.7 Acceptance of. 2,4-D butyl ester original drug acceptance period of one month. From the date of delivery, the quality of the finished product acceptance within one month of its Indicators should meet the standards.

Appendix A

(Informative) 2,4-D butyl ester content by capillary gas chromatographic method A. 1 Method summary Sample was dissolved in chloroform, di-n-butyl phthalate as the internal standard, using a HP-5 capillary column as filler and flame Ionization detector, the sample of 2,4-butyl ester by gas chromatography separation and determination. A. 2 Reagents and solutions Chloroform; 2,4-D butyl standard. a known mass fraction ≥98.0%; Internal standard. di-n-butyl phthalate, should not interfere with the analysis of impurities; Internal standard solution. Weigh-n-butyl phthalate 3.5g, set 250mL flask, add appropriate amount of chloroform was dissolved and diluted to Mark and shake. A. 3 Instrument Gas chromatograph. with a hydrogen flame ionization detector; Chromatography or chromatography workstation processor; Column. 30m × 0.32mm (. I.d) capillary column bonded HP-5 (5% phenyl methyl silicone), a film thickness of 0.25μm. A. 4 GC operating conditions Temperature (℃).200 column temperature, the gasification chamber 250, the detector chamber 300; Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 30, air 300, the compensation gas 25; Injection volume. 1.0μL; Retention time (min). 2,4- butylate 9.0, internal standard 11.6. Said gas chromatography system operating conditions typical operating parameters. It is given the operating parameters adjusted as appropriate depending on the characteristics of the instrument to To obtain the best results. Typical 2,4-D butyl ester original drug and the internal standard gas chromatography is shown in Figure A. 1. 1 --- 2,4-butyl; 2 --- internal standard. Figure A. 1 2,4-D butyl ester original drug and the internal standard gas chromatograph A. 5 measuring step A. 5.1 preparation of standard solution Weigh 2,4-butyl standard 0.1g (accurate to 0.0002g), placed in a glass bottle with a stopper with a pipette 5mL internal standard solution, Shake well. A. 5.2 Sample preparation solution He said sample containing 2,4-D butyl taking about 0.1g (accurate to 0.0002g), and placed in a stoppered glass vial with pipette 5mL within Standard solution, shake. A. 5.3 Determination Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle 2,4-butyl and the internal standard peak The ratio of the area of repetitive until two adjacent needles 2,4-butyl relative change compared with the internal standard peak area of less than 1.2%, the solution in accordance with standards Solution, sample solution, the sample solution and standard solution were sequentially measured. A. 6 Calculation The peak area was measured before and after the two-needle sample solution and two doses of the standard sample solution of 2,4-butyl and the internal standard ratio, respectively average. Sample mass fraction of 2,4-D butyl ester 1 (%) according to equation (A.1) Calculated. (A.1) Where. --- Standard samples of 2,4-butyl ester content, expressed as a percentage. A. 7 allowable difference The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result. ......

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