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GB/T 39672-2020 English PDF

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GB/T 39672-2020: Mancozeb
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GB/T 39672-2020469 Add to Cart 5 days Mancozeb Valid

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Basic data

Standard ID: GB/T 39672-2020 (GB/T39672-2020)
Description (Translated English): Mancozeb
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.30
Word Count Estimation: 25,250
Date of Issue: 2020-12-14
Date of Implementation: 2021-07-01
Older Standard (superseded by this standard): GB/T 20699-2006; GB/T 20700-2006
Regulation (derived from): National Standard Announcement No. 28 of 2020
Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration

GB/T 39672-2020: Mancozeb

---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.
Mancozeb ICS 65.100.30 G25 National Standards of People's Republic of China Replace GB/T 20699-2006, GB/T 20700-2006 Mancozeb 2020-12-14 release 2021-07-01 implementation State Administration for Market Regulation Issued by the National Standardization Management Committee

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces GB/T 20699-2006 "Mancozeb Technical" and GB/T 20700-2006 "Mancozeb Wettable Powder", and Compared with GB/T 20699-2006 and GB/T 20700-2006, in addition to editorial changes, the main technical changes are as follows. ---Modified the quality score index of mancozeb original drug from no less than 88.0% to no less than 85.0% (see 3.2, 3.2 of the.2006 edition); ---Modified the index of suspension rate in mancozeb wettable powder from not less than 60% to not less than 70% (see 3.2,.2006 Version 3.2); ---Modified the wetting time index in mancozeb wettable powder from no more than 60s to no more than 90s (see 3.2,.2006 edition 3.2); ---Added arsenic control project indicators and test methods (see 3.2 and 4.7); ---Increase the long-lasting foam control project indicators and test methods (see 3.2 and 4.14); ---The liquid chromatography method for the determination of mancozeb mass fraction has been added (see 4.3.1); ---Added the atomic absorption method for the determination of manganese and zinc mass fractions (see 4.6); ---The method of moisture determination by halogen moisture analyzer has been added (see 4.9.2). This standard was proposed by the China Petroleum and Chemical Industry Federation. This standard is under the jurisdiction of the National Pesticide Standardization Technical Committee (SAC/TC133). The main drafting units of this standard. Limin Chemical Co., Ltd., Shaanxi Thompson Biotechnology Co., Ltd., Anhui Tianchengji Agricultural Branch Research Institute Co., Ltd., Jiangxi Zhengbang Crop Protection Co., Ltd., Shenyang Chemical Research Institute Co., Ltd. The main drafters of this standard. Ma Yaguang, Xu Mei, Wang Xinran, Fan Xiaolong, Chu Dayong, Lu Yuanwen, Gu Bing, Lei Shuying, Chen Biyun. The previous versions of the standard replaced by this standard are as follows. ---GB/T 20699-2006; ---GB/T 20700-2006. Mancozeb

1 Scope

This standard specifies the technical requirements, test methods, acceptance and quality assurance period, as well as marks and standards for mancozeb technical and wettable powders. Sign, packaging, storage and transportation. This standard applies to the quality control of mancozeb technical and mancozeb wettable powder products. Note. See Appendix A for other names, structural formulas and basic physical and chemical parameters of mancozeb and ethylene thiourea.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated references, the latest version (including all amendments) applies to this document. GB/T 601 Preparation of Standard Titration Solution for Chemical Reagents Preparation of preparations and products used in GB/T 603 chemical reagent test method GB/T 1600-2001 Pesticide moisture determination method GB/T 1601 Method for determination of pesticide pH GB/T 1604 Acceptance Rules for Commodity Pesticides GB/T 1605-2001 Commercial pesticide sampling method GB 3796 General Rules for Pesticide Packaging GB/T 5451 Test method for wettability of pesticide wettable powder GB/T 6682-2008 Analysis laboratory water specifications and test methods GB/T 8170-2008 Numerical rounding rules and the expression and determination of limit values GB/T 14825-2006 Determination method of pesticide suspension rate GB/T 16150-1995 Determination of the fineness of pesticide powders and wettable powders GB/T 19136-2003 Method for determination of thermal storage stability of pesticides GB/T 28137 Determination method for persistent foaming of pesticides

3 Technical requirements

3.1 Appearance Mancozeb original drug should be light yellow or grayish yellow powder. Mancozeb wettable powder should be uniform and loose powder without lumps. 3.2 Technical indicators The control project indicators of mancozeb technical materials should meet the requirements of Table 1, and the control project indicators of mancozeb wettable powder should meet the requirements of Table 2.

4 Test method

Warning---Personnel using this standard should have practical experience in laboratory work. This standard does not point out all safety issues. use It is the responsibility of the individual to take appropriate safety and health measures and to ensure compliance with relevant national laws and regulations. 4.1 General rules The reagents and water used in this standard refer to analytical reagents and the third level specified in GB/T 6682-2008 unless other requirements are indicated. water. The judgment of the inspection result shall be carried out according to 4.3.3 of GB/T 8170-2008. 4.2 Sampling The original medicine is carried out according to 5.3.1 of GB/T 1605-2001, and the wettable powder is carried out according to 5.3.3 of GB/T 1605-2001.Use random The number table method determines the number of packages sampled. Final sampling volume. Mancozeb technical drug should be no less than 100g, mancozeb wettable powder should be no less 于200g. 4.3 Identification test 4.3.1 Liquid chromatography This identification test can be carried out simultaneously with the determination of mancozeb mass fraction. Under the same chromatographic operating conditions, the main color in the sample solution The relative difference between the retention time of the peak and the retention time of the mancozeb derivative in the standard solution should be no more than 1.5%. 4.3.2 Dithizone colorimetry 4.3.2.1 Reagents and instruments 4.3.2.1.1 Trichloromethane. 4.3.2.1.2 Glacial acetic acid. 4.3.2.1.3 Dithizone. known mass fraction w dithizone ≥99.0%. 4.3.2.1.4 Dithizone trichloromethane solution. mass fraction w dithizone = 1g/kg. 4.3.2.1.5 Dithizone glacial acetic acid solution. Take 2 mL of dithizone chloroform solution, add 0.25 mL of glacial acetic acid, and dilute with chloroform to 10mL, shake well. 4.3.2.1.6 Qualitative filter paper. 4.3.2.1.7 Capillary. 4.3.2.2 Measurement procedure Test 1.Weigh about 0.5g of the sample, add 2mL~3mL of distilled water, stir to make the sample evenly dispersed. Prepared with capillary The sample is dripped onto the filter paper, dripped into powder dots, placed to dry naturally. Use a capillary to suck the dithizone glacial acetic acid solution and drop it onto the powder spot. The center of the powder spot appears yellow and the surroundings appear pink. Test 2.Weigh about 0.5g of the sample, add 2mL~3mL chloroform, stir to make the sample evenly dispersed. Prepare the The good sample is dripped on the filter paper, dripped into powder dots, and placed to dry naturally. Use a capillary to suck the dithizone trichloromethane solution and drop it onto the powder spot. The center of the powder spot appears yellow, and then quickly turns to bright purple. If the test results satisfy both test one and test two, it can be confirmed that the sample is mancozeb. 4.4 Determination of appearance Determined by visual inspection. 4.5 Determination of the mass fraction of mancozeb 4.5.1 Method summary The manganese ion and zinc ion in mancozeb and the chelating agent disodium ethylenediaminetetraethanol (EDTA) form complexes and water under alkaline conditions Soluble ethylene dithiocarbamate anion (referred to as mancozeb derivative). The substance uses reversed-phase high-performance liquid at a wavelength of 282nm Chromatographic separation and determination. The determination of mancozeb mass fraction can also be done by chemical methods. For specific analysis methods, see Appendix B in B.1. 4.5.2 Reagents and solutions 4.5.2.1 Methanol. chromatographically pure. 4.5.2.2 Tetrabutylammonium hydrogen sulfate. 4.5.2.3 Disodium ethylenediaminetetraacetic acid. 4.5.2.4 Disodium hydrogen phosphate. 4.5.2.5 Sodium sulfite. 4.5.2.6 Sodium hydroxide. 4.5.2.7 Sodium hydroxide solution. mass concentration ρNaOH=50g/L. 4.5.2.8 Water. Freshly steamed twice distilled water. 4.5.2.9 Mancozeb standard sample. known mass fraction w≥86.0%. 4.5.2.10 Buffer solution A. Weigh 3.40g of tetrabutylammonium hydrogen sulfate, 3.72g of disodium edetate, and 1.42g of disodium hydrogen phosphate, respectively. Dissolve in 1000mL water, adjust pH=10 with sodium hydroxide solution, mix well with ultrasound, filter with filter membrane, and set aside. 4.5.2.11 Buffer solution B. Weigh 7.44g disodium ethylenediaminetetraacetic acid and 1.42g disodium hydrogen phosphate, dissolve them in 1000mL water, and use Adjust pH to 11 with sodium hydroxide solution, then add 3g of sodium sulfite, dissolve and mix well and place in the refrigerator (at least 50min) for use. 4.5.3 Apparatus 4.5.3.1 High performance liquid chromatograph. with variable wavelength ultraviolet detector. 4.5.3.2 Chromatographic data processor or chromatographic workstation. 4.5.3.3 Chromatographic column. 150mm×4.6mm (inner diameter) stainless steel column with C18 and 5μm packing (or a chromatographic column with equivalent effect). 4.5.3.4 Filter. The pore size of the filter membrane is about 0.45μm. 4.5.3.5 Micro-injector. 50μL. 4.5.3.6 Quantitative sample injection tube. 5μL. 4.5.3.7 Ultrasonic cleaner. 4.5.4 HPLC operating conditions 4.5.4.1 Mobile phase. volume ratio ψ methanol. buffer solution A = 30.70, filtered through a membrane, and degassed. 4.5.4.2 Flow rate. 1.0mL/min. 4.5.4.3 Column temperature. room temperature (temperature change should not exceed 2°C). 4.5.4.4 Detection wavelength. 282nm. 4.5.4.5 Injection volume. 5μL. 4.5.4.6 Retention time. Mancozeb derivative is about 7.5min. 4.5.4.7 The above operating parameters are typical, and the given operating parameters can be adjusted appropriately according to the characteristics of different instruments in order to obtain the best effect. Typical derivatized mancozeb technical and wettable powder high performance liquid chromatograms are shown in Figure 1 and Figure 2, respectively. 4.5.5 Measurement procedure 4.5.5.1 Preparation of standard solution Weigh 0.04g (accurate to 0.0001g) mancozeb standard sample in a 100mL volumetric flask, add 80mL buffer solution B under shaking. In the ultrasonic (add ice cubes in the ultrasonic oscillator, so that the ultrasonic temperature is not higher than 20 ℃), oscillate for 5 minutes, and dilute to the mark with buffer solution B Shake well. Use a pipette to transfer 5 mL of the above solution into a 50 mL volumetric flask, dilute to the mark with buffer solution B, shake well, and filter with a filter membrane spare. (The solution is stored at low temperature, the temperature should not be higher than 20 ℃). 4.5.5.2 Preparation of sample solution Weigh a sample containing 0.035g (accurate to 0.0001g) of mancozeb into a 100mL volumetric flask, add 80mL buffer solution under shaking Liquid B. In the ultrasonic (add ice cubes in the ultrasonic oscillator, so that the ultrasonic temperature is not higher than 20 ℃), oscillate for 5 minutes, and dilute to the volume with buffer solution B Scale and shake well. Use a pipette to transfer 5 mL of the above solution into a 50 mL volumetric flask, dilute to the mark with buffer solution B, shake well, and use a filter membrane Filter for use. (The solution is stored at low temperature, the temperature should not be higher than 20℃) 4.5.5.3 Determination Under the above operating conditions, after the instrument is stable, continuously inject several needles of the standard solution until the peak area of the adjacent two needles of mancozeb derivative After the relative change is less than 1.5%, the determination is carried out in the order of standard solution, sample solution, sample solution, and standard solution. 4.5.6 Calculation The measured peak areas of mancozeb derivatives in the two needles of the sample solution and the two needles of the standard solution before and after the sample were averaged respectively. Sample The mass fraction of mancozeb is calculated according to formula (1). 4.5.7 Tolerance The difference between the results of two parallel determinations. Mancozeb technical drug should not exceed 1.5%, 80% mancozeb wettable powder should not exceed 1.2%, 70% mancozeb wettable powder should not exceed 1.0%, 50% mancozeb wettable powder should not exceed 0.7%, take their arithmetic average respectively The value is used as the measurement result. 4.6 Determination of manganese and zinc mass fraction 4.6.1 Method summary The sample is dissolved in the disodium ethylenediaminetetraacetic acid solution and introduced into the atomic absorption spectrometer. After the flame is atomized, the characteristic absorption of manganese (zinc) is measured The absorbance under the spectrum was quantified by the working curve measured by manganese and zinc standard solutions. The determination of manganese and zinc mass fractions can also use chemical methods. For the analysis method, see B.2 and B.3. 4.6.2 Reagents and solutions 4.6.2.1 Disodium ethylenediaminetetraacetic acid. 4.6.2.2 Disodium ethylenediaminetetraacetic acid solution. Weigh 7.44g disodium ethylenediaminetetraacetic acid and dissolve it in 1000mL water. 4.6.2.3 Manganese standard solution. mass concentration ρMn=1000μg/mL. Keep refrigerated. 4.6.2.4 Zinc standard solution. mass concentration ρZn=1000μg/mL. Keep refrigerated. 4.6.3 Apparatus 4.6.3.1 Atomic absorption spectrometer. 4.6.3.2 Manganese hollow cathode lamp. 4.6.3.3 Zinc hollow cathode lamp. 4.6.4 Preparation of sample solution Weigh a sample containing 0.045g (accurate to 0.0001g) mancozeb into a 100mL volumetric flask, add 80mL ethylenediaminetetraacetic acid The disodium solution was ultrasonically oscillated for 5 minutes, and the volume was adjusted to the mark with disodium ethylenediaminetetraacetic acid solution, and then shaken. Use a pipette to pipette the above solution 0.5mL in a 50mL volumetric flask, dilute to the mark with disodium ethylenediaminetetraacetic acid solution, shake. At the same time, prepare a blank solution without mancozeb sample as the reference solution according to the above method. 4.6.5 Determination of standard curve 4.6.5.1 Preparation of standard stock solutions Manganese standard stock solution. mass concentration ρMn=20μg/mL. Pipette 0.5mL manganese standard solution into a 25mL volumetric flask, dilute with water Release to the mark and shake well. Zinc standard stock solution. mass concentration ρZn=10μg/mL. Pipette 0.5mL zinc standard solution into a 50mL volumetric flask, dilute with water Release to the mark and shake well. 4.6.5.2 Preparation of standard solution 4.6.5.2.1 Preparation of manganese standard solution Pipette 0mL, 0.2mL, 0.5mL, 1.0mL, 2.0mL, 3.0mL of manganese standard stock solution into a 50mL volumetric flask. Dilute to the mark with water and shake well. 4.6.5.2.2 Preparation of zinc standard solution Pipette 0mL, 0.5mL, 0.8mL, 1.5mL, 3.0mL, 5.0mL of the zinc standard stock solution into a 50mL volumetric flask. Dilute to the mark with water and shake well. 4.6.5.3 Determination of the standard curve After the instrument is stabilized and the zero point is adjusted, the standard solution without manganese (zinc) is used as the reference solution, and the measurement is performed at a wavelength of 279.5nm (213.9nm). Determine the absorbance of each standard solution of manganese (zinc). Take the concentration of the standard solution as the abscissa and the corresponding absorbance as the ordinate to draw the standard curve. 4.6.6 Determination Under the same conditions as the standard curve determination, measure the absorbance of the sample solution and find out the corresponding concentration on the working curve. 4.6.7 Calculation Find the concentration of manganese (zinc) on the standard curve, and calculate the mass fraction of manganese (zinc) in the sample according to formula (2). 4.6.8 Tolerance The relative deviation of the results of two parallel determinations. manganese should not be greater than 5%, zinc should not be greater than 10%, and the arithmetic average of them should be taken as the determination. result. 4.7 Determination of arsenic mass fraction 4.7.1 Method summary After the sample is digested with acid, it is prepared into an aqueous solution, and the content of arsenic in the solution is measured with an atomic fluorescence spectrometer. The limit of quantification is 0.01μg/g. The determination of arsenic mass fraction can also use chemical methods, see B.4 for specific operations. 4.7.2 Reagents and solutions 4.7.2.1 Nitric acid solution. solution concentration cHNO3=0.2mol/L. 4.7.2.2 Perchloric acid. 4.7.2.3 Hydrochloric acid. mass fraction wHCl=36.0%~38.0%. 4.7.2.4 Mixed acid. volume ratio ψHClO4.HNO3=1.3. 4.7.2.5 Hydrochloric acid solution. volume ratio ψHCl.H2O=1.9. 4.7.2.6 Hydrogen peroxide. 4.7.2.7 Ascorbic acid. 4.7.2.8 Thiourea. 4.7.2.9 Ascorbic acid-thiourea mixed solution. 10g ascorbic acid and 10g thiourea are dissolved in 100mL water. 4.7.2.10 Arsenic standard solution. mass concentration ρAs=1.0mg/mL. Sealed and refrigerated. 4.7.2.11 Potassium borohydride. 4.7.2.12 Sodium hydroxide. 4.7.2.13 High purity argon gas. 4.7.3 Apparatus 4.7.3.1 Atomic fluorescence spectrometer. 4.7.3.2 Electric heating plate. 4.7.4 Operating conditions of atomic fluorescence spectroscopy 4.7.4.1 Negative high voltage of photomultiplier tube. 260V. 4.7.4.2 Lamp current. 80mA. 4.7.4.3 Carrier gas flow. 600mL/min. 4.7.4.4 Auxiliary gas flow. 800mL/min. 4.7.4.5 Pump speed. 100r/min. 4.7.4.6 Integration time. 5s. 4.7.5 Measurement procedure 4.7.5.1 Preparation of standard solution 4.7.5.1.1 Preparation of arsenic standard stock solution Use a pipette to draw 1mL of arsenic standard solution in a 1000mL volumetric flask, and dilute with nitric acid solution. Prepared into 1mg/L standard storage Prepare solution. It can be stored in the refrigerator for 1 month. 4.7.5.1.2 Preparation of arsenic standard solution Prepare 6 levels of standard solutions with different concentrations in the range of 0μg/L~10μg/L. Draw 0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL of 1mg/L arsenic standard stock solution to 50mL volume respectively In the bottle, add 25mL of hydrochloric acid solution, then add 5mL of ascorbic acid-thiourea mixture, and dilute to 50mL with water. Place at room temperature for 2h the above. 4.7.5.2 Preparation of sample solution 4.7.5.2.1 Wet digestion Weigh 0.5g of the sample (accurate to 0.0001g), place it in a 150mL conical flask, add 10mL nitric acid, and place the conical flask on the electric heating plate Slowly heat on the upper surface until the yellow smoke basically disappears; after a little cold, add 10 mL of mixed acid, and heat it on the heater until the sample is completely digested. To a transparent solution (sometimes it is necessary to add mixed acid as appropriate); add 10mL of water after a little cold, heat to boiling and emit white smoke, and keep it for a few minutes to drive off The remaining mixed acid, then cooled to room temperature, to prepare the sample solution. 4.7.5.2.2 Preparation of sample solution Transfer all the prepared digestion solution to......
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