GB 22601-2008 English PDF

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GB 22601-2008: [GB/T 22601-2008] 2, 4-D butyl emulsifiable concentrates
Status: Valid

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GB 22601-2008	319	Add to Cart	3 days	[GB/T 22601-2008] 2, 4-D butyl emulsifiable concentrates	Valid

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Basic data

Standard ID: GB 22601-2008 (GB22601-2008)
Description (Translated English): [GB/T 22601-2008] 2, 4-D butyl emulsifiable concentrates
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.20
Word Count Estimation: 12,152
Date of Issue: 2008-12-17
Date of Implementation: 2009-06-01
Adopted Standard: FAO 1.3/EC/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 EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the 2, 4 Butyl original drug is dissolved in a suitable solvent and emulsifier in the preparation of 2, 4 butylate EC.

GB 22601-2008: [GB/T 22601-2008] 2, 4-D butyl emulsifiable concentrates

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2, 4-D butyl emulsifiable concentrates ICS 65.100.20 G25 National Standards of People's Republic of China 2,4-D butyl EC 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/EC/S/F (1992) "2,4-Destersemulsifiableconcentrates" degree of consistency Non-equivalent. Appendix A of this standard is an informative annex. Since the implementation of this standard, the original chemical industry standard HG2320-1992 "2,4- butylate EC" 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 EC 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 Structural formula Handkerchief handkerchief handkerchief Division division division  division division division Cl Cl O CH 2  O CH 2 CH 2 CH 2 CH 3 Empirical formula. C12H14C12O3 Molecular weight. 277.15 (according to 2007 international relative atomic mass) Biological activity. Herbicides

1 Scope

This standard specifies the 2,4-butyl EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the 2,4-D butyl ester original drug and preparation of the emulsifier is dissolved in a suitable solvent 2,4-D butyl EC.

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. GB/T 1600 Determination of Water Pesticides Determination of GB/T 1601 Pesticides pH value GB/T 1603 Determination of emulsion stability of pesticide GB/T 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB/T 4472 chemical product density, relative density measurement General GB 4838 EC pesticide packaging GB/T 19136 Determination of Pesticide Thermal storage stability GB/T 19137 Pesticide cryogenic stability Determination

3 Requirements

3.1 Composition and appearance This product should meet the standards of the original drug 2,4-butyl ester prepared as a homogeneous oily liquid without visible suspended matter and sediment. 3.2 Technical Specifications 2,4-D butyl EC shall comply with the requirements of Table 1. Table 1 2,4-D butyl EC indicators Control Project project index 57% 72% 900g/L 999g/L Butyl 2,4 mass fraction of a /% Or 2,4-D butyl ester concentration (20 ℃) / (g/L) 57.0 + 2.5-2.5 72.0 + 2.5-2.5 76.0 + 2.5-2.5 + 25-25 900 82.5 + 2.5-2.5 + 25-25 999 Free phenol content (2,4-DCP meter) /% ≤ 0.6 0.8 0.8 0.9 Moisture content /% ≤ 0.8 pH range of 3.0 to 7.0 Emulsion stability (diluted 200 times) Qualified Low temperature stability Qualified b Thermal storage stability b qualified When a dispute occurs when the mass to the mass fraction of arbitration. b low temperature stability test, the thermal storage stability tests at normal production, at least every three months, once detected. Test Method 4 4.1 Sampling According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determined by sampling a random number table method packages, the final sample size Not less than 200mL. 4.2 Identification Test Gas Chromatography --- The identification test can be carried out simultaneously with the determination of 2,4-D butyl ester content. Under the same chromatographic operating conditions, the test The retention time of the sample solution and the standard solution to a peak of 2,4-D butyl ester peak retention time, the relative difference should be 1.5% Fewer. 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 is a stainless steel column filler and a flame ionization detector, the sample of 2,4-butyl gas chromatography and measurement set. Determination can also be used by capillary gas chromatography, chromatographic operating conditions given in 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 (℃). Column temperature. 170, 260 gasification chamber, 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. A typical gas chromatogram of 2,4-D butyl EC and the internal standard is shown in Figure 1. 1 --- internal standard; 2 --- 2,4-D ester. Figure 1 Gas chromatograms butyl 2,4-EC and the 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 adjacent needle relative peak area of 2,4-butyl After the change is less than 1.2%, 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 ratio 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 peak area, respectively average. Sample mass fraction of 2,4-D butyl ester 1 (%) according to equation (1) calculation of the concentration of 2,4-D butyl ρ1 (g/L) according to equation (2) Calculated. (1) ρ1 = (2) Where. Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured); --- Standard samples of 2,4-butyl ester content, expressed as a percentage. 4.3.6 allowable difference 2,4-D butyl ester content (mass concentration) of two parallel determination results relative difference should be less than 1.5%, and the arithmetic mean for To determine the results. 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 (3) Calculated. (3) 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 Moisture According to GB/T 1600 the "Karl Fischer method". According to GB/T 1601 carried out. 4.7 Emulsion stability test Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, the non-oil slick, no precipitation under qualified. 4.8 Low temperature stability test According to GB/T 19137 in "homogeneous emulsion and liquid preparations", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified. 4.9 Thermal storage stability test According to GB/T 19136 in "liquid formulation" to. After the thermal storage, 2,4-D butyl ester content should not be lower than the measured mass fraction before hot storage 95% emulsion stability should continue to meet the standards. 4.10 Product inspection 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 EC marking, labeling and packaging should comply with the provisions of GB 4838. 5.2 2,4-D butyl EC Bulk or polyurethane with iron drum, barrel net content of not more than 200kg. 2,4-D butyl EC parcel Loaded polyester bottle or glass bottles, bottle net weight 100g (mL), 200g (mL), 250g (mL), 500g (mL), 1kg (1L); overpack Plastic boxes or corrugated boxes, each box of net weight shall not exceed 15kg. 5.3 Other forms of packaging may be used according to user requirements or the order agreement, it should comply with the provisions of GB 4838. 5.4 2,4-D butyl EC packages 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 Warranty. under the specified storage conditions, warranties of 2,4-D butyl EC, from date of manufacture for 2 years.

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 (℃). Column temperature.200, 250 gasification chamber, the detector chamber 300; Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 30, air 300; 25 compensation gas; Injection volume. 1.0μL; Retention time (min). 2,4- butylate 9.0, internal standard 11.6. GC operating conditions described above, the Department of typical operating parameters. 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 EC gas chromatography is shown in Figure A. 1. 1 --- 2,4-butyl; 2 --- internal standard. Figure A. 1 2,4-D butyl EC gas chromatogram 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 ratio 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 peak area, respectively average. Sample mass fraction of 2,4-D butyl ester 1 (%), according to equation (A.1) to calculate the mass concentration ρ1 (g/L) according to equation (A.2) Calculated. (A.1) ρ1 = (A.2) Where. Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured); --- Standard samples of 2,4-butyl ester content, expressed as a percentage. A. 7 allowable difference Two parallel determination results of the relative difference should be less than 1.5%, the arithmetic mean value as a measurement result. ......

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