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GB 29384-2012: Acephate technical material
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Basic data
| Standard ID | GB 29384-2012 (GB29384-2012) |
| Description (Translated English) | Acephate technical material |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | G25 |
| Classification of International Standard | 65.100.10 |
| Word Count Estimation | 12,129 |
| Quoted Standard | GB/T 601; GB/T 1600; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 6682-2008; GB/T 8170-2008 |
| Regulation (derived from) | National Standards Bulletin No. 42 of 2012 |
| 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 requirements for the original drug acephate, test methods and marking, labeling, packaging, storage, inspection period. This standard applies to acephate and its impurities generated in the production of acephate origin |
GB 29384-2012: Acephate technical material
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Acephate technical material
ICS 65.100.10
G25
National Standards of People's Republic of China
Acephate original drug
Published 2012-12-31
2013-07-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China issued
Foreword
This standard in Chapter 3, Section 5 is mandatory, the rest are recommended.
This standard was drafted in accordance with rules GB/T 1.1-2009 given.
Please note that some of the content of this document may involve patents, the issuing authority of this document does not assume responsibility for identifying these patents.
The standard proposed by China Petroleum and Chemical Industry Federation.
This standard by the National Pesticide Standardization Technical Committee (SAC/TC133).
This standard is drafted. Shenyang Chemical Research Institute Co., Ltd.
Participated in the drafting of this standard. Sanonda Co., Ltd. Hubei, Zhejiang Jiahua Group Co., Ltd., Jiangsu blue abundance of chemicals
Co., Ltd., Hangzhou Agrochemical Co., Ltd. Qingfeng.
The main drafters of this standard. High Scenic, Li Dong, Liao Yan, Li Da Yuan, Zhang Shurong, India Xie Gang, He Hongdong.
Acephate original drug
1 Scope
This standard specifies the requirements of the original drug acephate, Test Method for marking, labeling, packaging, storage, and acceptance period.
This standard applies to impurities derived from the production of the composition and acephate acephate original drug.
Note. Acephate acetamide and impurities, other names methamidophos, O, O, S- trimethyl phosphorothioate, structural formulas and physicochemical parameters of the basic see Appendix
Record A.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
Preparation GB/T 601 standard titration solution Chemicals
GB/T 1600 Pesticide Method Moisture
GB/T 1604 pesticide regulations for acceptance of goods
GB/T 1605-2001 sampling 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 rounding off means about rules and determining limiting values
3.1 Appearance
White crystalline powder, no visible foreign matter.
3.2 Technical Specifications
Acephate original drug should also meet the requirements of Table 1.
Table 1 acephate original drug control project indicators
Item Index
Acephate mass fraction /% ≥ 97.0
Acetamide mass fraction /% ≤ 0.3
Methamidophos mass fraction /% ≤ 0.3
O, O, S- trimethyl phosphorothioate mass fraction a /% ≤ 0.1
Moisture content /% ≤ 0.5
Acidity content (in terms H2SO4) /% ≤ 0.5
When a normal production, O, O, S- trimethyl phosphorothioate mass fraction was measured at least once every three months.
Test Method 4
Safety Tips. to use this standard shall have practical experience of laboratory work. This standard does not indicate any safety issues. Make
With those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the provisions of relevant state laws and regulations.
4.1 General provisions
This standard reagent in the absence of water and other requirements stated, refer to three predetermined analytical reagents and GB/T 6682-2008 of
water. The test standard titration solution, in the absence of other requirements specified, and prepared according to GB predetermined calibration/T 601 a. test result
4.3.3 determination performed by the rounding value in comparison 8170-2008 GB/T .
4.2 Sampling
Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determined by sampling a random number table method packages, the amount of the final sample
Not less than 100g.
4.3 Identification Test
The present liquid chromatography --- identification test can be carried out simultaneously with the determination of the mass fraction of acephate. In the same chromatographic operating conditions
, The peak of a retention time in the sample solution acephate chromatographic peak retention time of standard solution, which should be in the relative difference
1.5% or less.
Infrared Spectroscopy Infrared --- sample and standard sample in the range of 4000cm-1 ~ 400cm-1 absorption spectrum should be no difference, see
figure 1.
1 acephate standard infrared spectrum of FIG.
4.4 Determination of acephate, acetamide and mass fraction methamidophos
4.4.1 Method summary
Sample dissolved in mobile phase, acetonitrile-water (pH = 3) as the mobile phase, used as a filler C18 stainless steel column and UV detector
(210nm), the sample 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 standards. a known mass fraction, w ≥99.0%;
Acetamide standard. a known mass fraction, w ≥98.0%;
Methamidophos standards. a known mass fraction, w ≥98.0%;
Sample preparation and methamidophos acetamide standard solution. Weigh acetamide standard 0.06g, 0.1 g of Sample methamidophos (accurate to
0.0002g) was placed in a 50mL volumetric flask, add the mobile phase to dissolve and dilute to the mark.
4.4.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor or workstation;
Column. 250mm × 4.6mm (id) stainless steel column, C18,5μm filler contents (or column with equivalent effect);
Filter. membrane pore size of about 0.45 m;
Microsyringe. 250μL;
Ultrasonic cleaning.
4.4.4 HPLC operating conditions
Mobile phase. Ψ. after (acetonitrile water) = 10.90, with phosphoric acid water adjusted to pH 3, mixed well, filtered through a filter membrane, and
Degassing;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should be less than 2 deg.] C);
Detection wavelength. 210nm;
Injection volume. 20μL;
Retention time. acetamide 3.6min, methamidophos 5.0min, acephate 5.7min.
Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.
Typical HPLC acephate TC shown in Figure 2.
1 --- acetamide;
2 --- methamidophos;
3 --- acephate.
Figure 2 HPLC original drug acephate
4.4.5 Determination Step
4.4.5.1 Preparation of standard solution
Sample Weigh 0.06 g of acephate (accurate to 0.0002g) was placed in a 50mL volumetric flask, with a pipette pipetted 2.0mL acetyl
Methamidophos and amine standards in the standard solution in the same flask, dissolved in mobile phase and dilute to the mark.
4.4.5.2 Preparation of sample solution
Weigh 0.06 g of acephate-containing (accurate to 0.0002g) sample, placed in a 50mL volumetric flask, and dilute with mobile phase to dissolve
To the mark.
4.4.5.3 Determination
Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two adjacent needles acephate relative peak area
After the change is less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.4.5.4 computing
The two doses of the standard sample solution before and after the two-pin and a sample solution is measured acephate (acetamide, methamidophos) peak area, respectively,
Averaged. Acephate sample (acetamide, methamidophos) mass fraction, according to equation (1).
w1 =
A2 · m1 · w
A1 · m2 × f
(1)
Where.
W1 --- sample acephate (acetamide, methamidophos) the mass fraction in%;
A2 --- sample solution, an average value acephate (acetamide, methamidophos) peak area;
M1 --- Sample mass in grams (G);
W --- Sample acephate (acetamide, methamidophos) the mass fraction in%;
f --- dilution factor, acephate f = 1, and methamidophos acetamide f = 0.04;
A1 --- the standard solution, the average value of acephate (acetamide, methamidophos) peak area;
--- M2 sample mass, in grams (g).
4.4.5.5 allow poor
Acephate differential mass fraction of the two parallel measurement result should be less than 1.2%, and methamidophos acetamide relative difference should be less than
20%, respectively, as the measurement result of the arithmetic mean.
Measured 4.5 O, O, S- trimethyl phosphorothioate mass fraction
4.5.1 Method summary
Sample dissolved in mobile phase, acetonitrile-water (pH = 3) as the mobile phase, used as a filler C18 stainless steel column and UV detector
(210nm), of the sample O, O, S- trimethyl phosphorothioate 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.
Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.
Typical HPLC original drug acephate shown in Figure 3.
1 --- O, O, S- trimethyl phosphorothioate.
FIG HPLC original drug acephate 3
4.5.5 Determination Step
4.5.5.1 Preparation of standard solution
Weigh O, O, S- trimethyl phosphorothioate 0.05 g of standard sample (accurate to 0.0002g) was placed in a 50mL volumetric flask, compatible with the mobile
Solution and diluted to the mark.
4.5.5.2 Preparation of sample solution
Weigh 1.0 g of the original drug acephate (accurate to 0.0002g) sample, placed in a 50mL volumetric flask, and dilute with mobile phase to dissolve
To the mark.
4.5.5.3 Determination
Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two adjacent needles acephate relative peak area
After the change is less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.5.5.4 computing
The two doses of the standard peak area was measured before and after the two needles in the sample solution and a sample O, O, S- trimethyl phosphorothioate respectively into
Line averaging. Sample on O, the mass fraction of O, S- trimethyl phosphorothioate, according to equation (2).
w2 = A2
· M1 · w
A1 · m2
(2)
Where.
--- w2 of the sample mass fraction of O, O, S- trimethyl phosphorothioate, expressed in%;
A2 --- sample solution, the average value of O, O, S- trimethyl phosphorothioate peak area;
M1 --- Sample mass in grams (G);
W --- Sample mass fraction of O, O, S- trimethyl phosphorothioate, expressed in%;
A1 --- the standard solution, O, O, S- trimethyl phosphorothioate average peak area;
--- M2 sample mass, in grams (g).
4.5.5.5 allow poor
O, O, S- two parallel score measurement result trimethyl phosphorothioate relative mass difference should be less than 20%, and the arithmetic mean for
To determine the results.
4.6 Determination of moisture content
According to GB/T 1600 in the "Karl Fischer method".
Determination of the mass fraction of 4.7 acidity
4.7.1 Reagents and solutions
Ethanol solution. Φ (C2H5OH) = 95%;
Sodium hydroxide standard titration solution c (NaOH) = 0.02mol/L;
Indicator solution. ethanol solution of methyl red, ρ (methyl red) = 2g/L.
4.7.2 Determination Step
2g sample was weighed (accurate to 0.0002g), placed in a 250mL Erlenmeyer flask, was added an ethanol solution of 50mL, shaking the sample solution
solution. Add 5 drops of indicator solution, titrated with standard sodium hydroxide titration solution, the solution changed from red to orange is the end. At the same time a blank
Determination.
4.7.3 computing
Acidity content of the sample, according to equation (3) is calculated.
w3 = c
(V1-V0) M
m × 1000 × 100
(3)
Where.
W3 --- acidity content of the sample, expressed in%;
C --- The actual concentration of sodium hydroxide standard titration solution in units of moles per liter (mol/L);
Vl --- titration of the sample solution, the consumption of sodium hydroxide standard titration solution volume in milliliters (mL);
--- titrate blank solution V0, the volume of consumption of sodium hydroxide standard titration solution in milliliters (mL);
--- numerical molar mass M sulfuric acid (H2SO4), in units of grams per mole (g/mol) M 12H2SO
÷ 4
êê
úú = 49;
--- m sample mass, in grams (g).
4.8 product testing and acceptance
Shall comply with the provisions of GB/T 1604's.
5 marking, labeling, packaging, storage, security, acceptance period
5.1 marking, labeling, packaging
Flag acephate original drug, labeling and packaging should comply with the provisions of GB 3796.
Acephate original drug should be lined with clean plastic bag and the exhaust air, seal it tightly. Topical plastic drum or cardboard packaging, each
Barrel net content should not exceed 50kg. The user requests or orders protocols, other forms of packaging can be employed, subject to the requirements of GB 3796
Provisions.
5.2 Storage
Acephate original drug package airiness, drying, low temperature warehouses.
Storage and transportation, to prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, nose and mouth to prevent inhalation.
5.3 Security
Acephate low toxicity organophosphate pesticides. The FDA should wear protective gloves, masks, wear clean protective clothing. Immediately after use
Wash with water and soap. Such as poisoning occurs, it is timely to hospital for treatment.
5.4 Acceptance of
Acephate original drug acceptance period of one month. The quality of the finished product acceptance within one month from the date of delivery, the indicators should break
Together standards.
Appendix A
(Informative)
Acephate and impurities acetamide, methamidophos,
Other names, structural formulas and physicochemical parameters substantially O, O, S- trimethyl phosphorothioate
Other names, structural formulas and physical and chemical parameters of the basic active ingredient of the product of acephate are as follows.
ISO common name. acephate
CAS Registry Number. 30560-19-1
CIPAC Numeric Code. 338
Chemical name. O, S- dimethyl-acetyl phosphoroamidothioate -N-
Structure.
Empirical formula. C4H10NO3PS
Molecular weight. 183.2
Biological activity. insecticide
Melting point. 88 ℃ ~ 90 ℃
Vapor pressure (24 ℃). 0.226mPa
Relative density (20 ℃). 1.35
Solubility (20 ℃, g/L). water, 790; 151 acetone; ethanol > 100; ethyl acetate, 35; 16 benzene; n-hexane 0.1
Stability. stable under acidic conditions, the half-life DT50 (40 ℃) 60h (pH = 9), 710h (pH = 3).
This other product names, structural formulas and physicochemical parameters of the basic impurity acetamide as follows.
ISO common name. acetamide
CAS Registry Number. 60-35-5
Chemical Name. acetamide
Structure.
Empirical formula. C2H5NO
Relative molecular weight. 59.07
Melting point. 81 ℃
Boiling point. 222 ℃
Vapor pressure (65 ℃). 0.13kPa
Relative density (20 ℃). 1.16
Solubility. soluble in water, ethanol, chloroform, pyridine and glycerin, slightly soluble in diethyl ether, insoluble in n-octanol.
This other product names, structural formulas and physicochemical parameters of the basic impurity methamidophos follows.
ISO common name. methamidophos
CAS Registry Number. 10265-92-6
CIPAC Numeric Code. 355
Chemical name. O, S- dimethyl phosphorothioate group
Structure.
Empirical formula. C2H8NO2PS
Molecular weight. 141.1
Biological activity. insecticide, acaricide
Melting point. 44.9 ℃
Vapor pressure. 2.3mPa (20 ℃), 4.7mPa (25 ℃)
Relative density (20 ℃). 1.27
Solubility (20 ℃, g/L). water > 200, isopropyl alcohol > 200, dichloromethane > 200, 0.1 to 1 hexane, toluene 2-5
Stability. stable at room temperature, thermal decomposition, so no boiling. In the range of pH3 ~ 8 stability, half-life DT501.8年 (pH 4),
120h (pH7), 70h (pH9).
This product impurities O, O, S- other names trimethyl phosphorothioate, structural formulas and physicochemical basic parameters are as follows.
Common name. O, O, S- trimethyl phosphorothioate
CAS Registry Number. 152-20-5
Chemical name. O, O, S- trimethyl phosphorothioate
Structure.
Empirical formula. C3H9O3PS
Molecular weight. 156.15.
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