GB 28140-2011 English PDF

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GB 28140-2011: [GB/T 28140-2011] 75% Acephate water soluble powders
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 28140-2011	339	Add to Cart	3 days	[GB/T 28140-2011] 75% Acephate water soluble powders	Valid

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Basic data

Standard ID: GB 28140-2011 (GB28140-2011)
Description (Translated English): [GB/T 28140-2011] 75% Acephate water soluble powders
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.10
Word Count Estimation: 13,116
Date of Issue: 2011-12-30
Date of Implementation: 2012-04-15
Quoted Standard: GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 6682-2008; GB/T 8170-2008; GB/T 19136
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 75% soluble powder acephate requirements, test methods and marking, labeling, packaging, storage and warranty. This standard applies to acephate original drug with a suitable additives and fillers processed into acephate 75% soluble powder.

GB 28140-2011: [GB/T 28140-2011] 75% Acephate water soluble powders

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75% Acephate water soluble powders ICS 65.100.10 G25 National Standards of People's Republic of China 75% acephate soluble powders 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. Please note that some content of this document may involve patents, the issuing authority of this 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 is drafted by. Shenyang Chemical Research Institute Co., Ltd. Participated in the drafting of this standard. Hubei Sanonda Co., Ltd., Zhejiang Jia Group Co., Ltd., Jiangsu Blue abundance of chemical Co., Ltd., Hangzhou Agrochemical Co., Ltd. Qingfeng. The main drafters of this standard. High Scenic, Dong, Lee Yuan Liao Yan, Zhang Shurong, India Xie Gang, He Hongdong. 75% acephate soluble powders

1 Scope

This standard specifies 75% acephate soluble powders requirements, test methods and marking, labeling, packaging, storage and transportation, the guarantee period. This standard applies to 75% of acephate acephate soluble powders by the original drug with suitable additives and fillers processed into. NOTE. acephate and impurities acetamide Other names methamidophos, O, O, S- trimethyl phosphorothioate, structural formula and basic physicochemical parameters, see 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 1600 Determination of Water Pesticides Determination of GB/T 1601 Pesticides pH value GB/T 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB 3796 pesticide packaging General GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD) GB/T 8170-2008 revised value represents about rules and limit values and judgment GB/T 19136 Determination of Pesticide Thermal storage stability

3 Requirements

3.1 Appearance This product should be compliant acephate original drug with suitable additives and fillers processing is made uniform loose powder, no visible external To matter and mass. 3.2 Technical Specifications Acephate soluble powder shall meet the requirements of Table 1. Table 1 75% acephate soluble powders Control Project Index Item Index Acephate mass fraction /% 75.0 3.0-3.0 Acetamide mass fraction /% ≤ 0.3 Methamidophos mass fraction /% ≤ 0.5 O, O, S- trimethyl phosphorothioate mass fraction a /% ≤ 0.1 Moisture content /% ≤ 2.0 pH range 3.0 to 7.5 Table 1 (continued) Item Index The degree of dissolution and solution stability (through 75μm test sieve) a /% (5min after residue) ≤ (18h after residue) ≤ 2.0 0.5 Thermal storage stability of a qualified When a normal production, O, O, S- trimethyl phosphorothioate content, the degree of dissolution and solution stability, thermal storage stability test was measured at least every three months once. Test Method 4 Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make With those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations. 4.1 General provisions This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in water. Test results determined in accordance with GB/T 8170-2008 4.3.3 Rounding the value comparison method. 4.2 Sampling According to GB/T 1605-2001 "on solid preparation sampling" approach. Determining sample package using a random number table method; the final sample size Not less than 300g. 4.3 Identification Test Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of acephate. In the same chromatographic operating conditions , The sample solution to a chromatographic retention time and acephate standard solution peak retention time, the relative difference should 1.5% or less. 4.4 Determination of acephate, methamidophos acetamide and mass fraction 4.4.1 Method summary Sample dissolved in mobile phase, acetonitrile and water (pH = 3) as the mobile phase, use as filler to C18 stainless steel column and UV detector (210nm), the sample of acephate, methamidophos acetamide and reverse phase high performance liquid chromatography, external standard. 4.4.2 Reagents and solutions Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; Phosphoric acid; Acephate standard. a known mass fraction w≥99.0%; Acetamide standard. a known mass fraction w≥98.0%; Methamidophos standard. a known mass fraction w≥98.0%; Sample preparation and methamidophos acetamide standard solution. Weigh acetamide standard 0.06g, methamidophos standard 0.1g (accurate to 0.0002g) placed in 50mL volumetric flask, add the mobile phase dissolved and diluted to the mark. 4.4.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or workstation; Column. 250mm × 4.6mm (id) stainless steel column, built C18,5μm filler (or with equivalent effect column); Filter. filter pore size of about 0.45μm; Micro injector. 250μL; Ultrasonic cleaner. 4.4.4 HPLC operating conditions Mobile phase. Ψ. after (acetonitrile, water) = 10.90 adjusted to pH with phosphoric acid to water is 3, mixed, filtered through a filter membrane, and Degassing; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 210nm; Injection volume. 20μL; Retention time. acetamide 3.6min, methamidophos 5.0min, acephate 5.7min. 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 75% acephate soluble powders HPLC is shown in Figure 1. 1 --- acetamide; 2 --- methamidophos; 3 --- acephate. 1 75% acephate soluble powders by high performance liquid chromatogram 4.4.5 measuring step 4.4.5.1 Preparation of standard solution Weigh acephate standard 0.06g (accurate to 0.0002g) placed in 50mL volumetric flask, with a pipette Pipette 2.0mL acetyl Amine standards and methamidophos standard solution in the same volumetric flask, dissolved in mobile phase and dilute to the mark. 4.4.5.2 Preparation of sample solution Weigh containing acephate 0.06g (accurate to 0.0002g) sample, placed in 50mL volumetric flask, dissolved in mobile phase and diluted To the mark. 4.4.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles acephate relative peak area 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. 4.4.5.4 Calculation The two front and rear needle sample solution measured sample and two doses of the standard solution of acephate (acetamide, methamidophos) peak area, respectively Averaged. Sample acephate (acetamide, methamidophos) mass fraction, according to equation (1). w1 = A2 · M1 · w A1 · m2 × f (1) Where. w1 --- sample acephate (acetamide, methamidophos) mass fraction, expressed as a percentage; A2 --- sample solution, the average acephate (acetamide, methamidophos) peak area; m1 --- standard mass in grams (g); w --- Sample acephate (acetamide, methamidophos) mass fraction, expressed as a percentage; f --- dilution factor of acephate f = 1, acetamide and methamidophos f = 0.04; A1 --- the standard solution, the average acephate (acetamide, methamidophos) peak area; m2 --- sample mass, in grams (g). 4.4.5.5 allowable difference Acephate poor quality score of two parallel determination results shall not be greater than 1.2% acetamide and methamidophos should be less than the relative difference 20%, respectively, the arithmetic mean value as a measurement result. Determination 4.5 O, O, S- trimethyl phosphorothioate mass fraction 4.5.1 Method summary Sample dissolved in mobile phase, acetonitrile and water (pH = 3) as the mobile phase, use as filler to C18 stainless steel column and UV detector (210nm), the sample of O, O, S- trimethyl phosphorothioate reverse phase high performance liquid chromatography, external standard. 4.5.2 Reagents and solutions With 4.4.2; O, O, S- trimethyl phosphorothioate Sample. A known mass fraction w≥95.0%. 4.5.3 Instruments With 4.4.3. 4.5.4 HPLC operating conditions With 4.4.4; Retention time. O, O, S- trimethyl phosphorothioate 15min. 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 acephate soluble powders HPLC is shown in Figure 2. 1 --- O, O, S- trimethyl phosphorothioate. 2 75% acephate soluble powders by high performance liquid chromatogram 4.5.5 measuring step 4.5.5.1 Preparation of standard solution Weigh O, O, S- trimethyl phosphorothioate standard 0.05g (accurate to 0.0002g) placed in 50mL volumetric flask with mobile compatibility Solution and diluted to the mark. 4.5.5.2 Preparation of sample solution Weigh containing O, O, S- trimethyl phosphorothioate 0.05g (accurate to 0.0002g) sample, placed in a 50mL volumetric flask, with the mobile Phase dissolved and diluted to the mark. 4.5.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles acephate relative peak area 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. 4.5.5.4 Calculation The measured before and after the two-needle sample solution and sample two doses of the standard solution of O, O, S- trimethyl phosphorothioate peak area, respectively, into the Line averaging. Sample O, O, S- trimethyl phosphorothioate mass fraction, according to equation (2). w2 = A2 · M1 · w A1 · m2 (2) Where. --- w2 of the sample O, O, S- trimethyl phosphorothioate mass fraction in%; --- The A2 in the sample solution, the average of O, O, S- trimethyl phosphorothioate peak area; m1 --- standard mass in grams (g); w --- standard samples O, O, S- trimethyl phosphorothioate mass fraction, expressed as a percentage; The A1 --- standard solution, O, O, S- trimethyl phosphorothioate average peak area; m2 --- sample mass, in grams (g). 4.5.5.5 allowable difference O, O, S- trimethyl phosphorothioate mass fraction determination of the relative difference between the two results in parallel should not exceed 20% of the arithmetic mean for To determine the results. 4.6 Determination of moisture content According to GB/T 1600 in the "azeotropic distillation method". Determination of 4.7 pH value According to GB/T 1601 carried out. 4.8 degree of dissolution and solution stability 4.8.1 Method summary The 75% acephate soluble powder is dissolved in 25 ℃ water standard, inverted 15 times and allowed to stand for 5min, with over 75μm test sieve Filtered and quantitative determination of sieve residue. Determination of the stability of solution after the solution is allowed to stand for 18h, with 75μm test sieve again. 4.8.2 Instruments Standard sieve. aperture 75μm, diameter 76mm; Graduated cylinder. glass, stoppered, between 0mL ~ 250mL scale distance 25cm ~ 21.5cm, 250mL scale line and the bottom plug Distance of 4cm ~ 6cm. 4.8.3 Preparation of test solution Added 250mL graduated cylinder 2/3 standard hard water, which is heated to a temperature of 25 ℃, 5g of the sample, plus a standard hard water to the mark. Stoppered. Standing 30s, the cylinder 15 reverses the hand (180 °), reset, inverted, the reset time should not exceed the time spent 2s. 4.8.4 5min after test The cylinder in the test solution was allowed to stand 5min ± 30s after a 75μm test sieve Pour into a constant, and the filtrate was collected 500mL Beaker, reserved for the next test. Measuring cylinder with 100mL of distilled water 5 times, all insolubles were quantitatively transferred to a sieve, washed discarded Liquid residue on the screen to check. If there is residue on the sieve, sieve test at 100 ℃ drying to constant weighed. 4.8.5 18h after the test After standing 18h, carefully observe whether the precipitation filtrate in the beaker. If there are insoluble materials, and then the solution was 75μm sieved test Filtered, washed with distilled water 100mL test sieves. If the presence of solid or crystalline, will screen at 60 ℃ dried to a constant weighed. 4.8.6 Calculation 5min 18h residue remaining after the mass fraction and mass fraction respectively of formula (3) and (4) Calculated. w3 = m2-m1m × 100 (3) w4 = m'2-m'1m × 100 (4) Where. Mass fraction w3 --- 5min after residues, expressed in%; Mass fraction w4 --- 18h after the residue, expressed in%; m1, quality m'1 --- sieve after constant in units of grams (g); Quality m2, m'2 --- sieve and residue, in grams (g); m --- test mass in grams (g). 4.9 Thermal storage stability test According to GB/T 19136 in "solid preparation" to. Within 24h acephate, acetamide, methamidophos after thermal storage mass fraction dissolved Level solutions and solution stability test, after 75% of acephate soluble powders thermal storage, acephate content should not be lower than the previous receptacles 95% acetamide content should not be higher than 0.5%, mass fraction of methamidophos should be no higher than 0.8%, the degree of dissolution and solution stability in line with standard Registration requirement is qualified. 4.10 Product inspection and acceptance Shall comply with GB/T 1604's. 5 marking, labeling, packaging, storage, security, guarantee 5.1 marking, labeling, packaging 75% acephate soluble powder marking, labeling and packaging should comply with the provisions of GB 3796. Within 75% of acephate soluble powder packaging aluminum foil bags or plastic bags double thick quality. Net weight 50kg, for use cardboard Overpack. According to user requirements or the order agreement, other forms of packaging may be used, subject to the provisions of GB 3796. 5.2 Storage 75% acephate soluble powder packaging should be stored in well-ventilated, dry, low temperature warehouse. Storage and transportation, to prevent moisture and sunlight, not Get food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.3 Security Acephate low toxicity organophosphate pesticides. The FDA should wear protective gloves, masks, wearing clean protective clothing. Spray when the wind Direction, nose and mouth to prevent inhalation, skin or exposed parts of the body after contact with the product, should be washed with soap and water. In case of poisoning, Should go to hospital for treatment. 5.4 Warranty Period Under the specified storage conditions, warranties of 75% acephate soluble powder, two years from date of manufacture.

Appendix A

(Informative) Other name, structural formula and basic physicochemical parameters and impurities acetamide acephate, methamidophos, O, O, S- of trimethyl phosphorothioate Other name, structural formula and basic physicochemical parameters of the active ingredient acephate product as follows. ISO common name. Acephate CAS Registry Number. 30560-19-1 CIPAC Numeric Code. 338 Chemical Name. O, S- dimethyl acetyl-phosphoramidothioate -N- Structure. OCH3 H3CS N H - CH3 Empirical formula. C4H10NO3PS Molecular Weight. 183.2 Biological activity. Insecticidal Melting point. 88 ℃ ~ 90 ℃ Vapor pressure (24 ℃). 0.226mPa The relative density (20 ℃). 1.35 Solubility (20 ℃, g/L). water, 790; 151 acetone; Ethanol > 100; 35 ethyl acetate; benzene 16; n-hexane 0.1 Stability. stable under acidic conditions, the half-life DT50 (40 ℃) 60h (pH = 9), 710h (pH = 3). Other names for this product, structural formula and basic physicochemical parameters impurity acetamide as follows. ISO common name. Acetamide CAS Registry Number. 60-35-5 Chemical name. acetamide Structure. H3C NH2 Empirical formula. C2H5NO Molecular Weight. 59.07 Melting point. 81 ℃ Boiling point. 222 ℃ Vapor pressure (65 ℃). 0.13kPa The relative density (20 ℃). 1.16 Solubility. soluble in water, ethanol, chloroform, pyridine and glycerine, slightly soluble in ether, insoluble in n-octanol. Other names for this product, structural formula and basic physicochemical parameters impurity methamidophos as follows. ISO common name. Methamidophos CAS Registry Number. 10265-92-6 CIPAC Numeric Code. 355 Chemical Name. O, S- dimethylamino phosphorothioate Structure. OCH3 H3CS NH2 Empirical formula. C2H8NO2PS Molecular Weight. 141.1 Biological activity. insecticide, acaricide Melting point. 44.9 ℃ Vapor Pressure. 2.3mPa (20 ℃), 4.7mPa (25 ℃) The relative density (20 ℃). 1.27 Solubility (20 ℃, g/L). water > 200, isopropyl alcohol > 200, dichloromethane > 200, 0.1 to 1 hexane, toluene, 2 to 5 Stability. stable at room temperature, thermal decomposition, so no boiling point. In the range of pH3 ~ 8 stability, half-life DT501.8a (pH4), 120h (pH7), 70h (pH9). This product impurities O, O, other names S- trimethyl phosphorothioate, structural formula and basic physicochemical parameters are as follows. Generic name. O, O, S- trimethyl phosphorothioate CAS Registry Number. 152-20-5 Chemical Name. O, O, S- trimethyl phosphorothioate Structure. OCH3 H3CS OCH3 Empirical formula. C3H9O3PS Molecular Weight. 156.15. ......

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