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GB 2548-2008: Dichlorvos emulsifiable concentrates
Status: Valid GB 2548: Evolution and historical versions
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Dichlorvos emulsifiable concentrates
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GB 2548-2008
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| GB 2548-1993 | English | 239 |
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Dichlorvos emulsifiable concentrates
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PDF similar to GB 2548-2008
Standard similar to GB 2548-2008 GB 2763.1 GB/T 18419 GB/T 18418 Basic data | Standard ID | GB 2548-2008 (GB2548-2008) | | Description (Translated English) | Dichlorvos emulsifiable concentrates | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.10 | | Word Count Estimation | 11,163 | | Date of Issue | 2008-12-17 | | Date of Implementation | 2009-06-01 | | Older Standard (superseded by this standard) | GB 2548-1993 | | Adopted Standard | FAO 11/EC/S-1989, MOD | | Regulation (derived from) | Announcement of Newly Approved National Standards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 requirements of dichlorvos, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the original drug with dichlorvos emulsifier dissolved in a suitable solvent in the preparation of dichlorvos. | GB 2548-2008: Dichlorvos emulsifiable concentrates---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.
Dichlorvos emulsifiable concentrates
ICS 65.100.10
G25
National Standards of People's Republic of China
Replacing GB 2548-1993
Dichlorvos EC
Published 2008-12-17
2009-06-01 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 modification uses standard FAO specifications 11/EC/S (1989) "DDVP" (in English).
This standard modification method using foreign advanced standards for the redrafted law.
This standard and FAO specification "DDVP" The main technical differences.
1) an increase of chloral control project milestones.
2) The standard pH indicators ≤0.3%, while the FAO specifications for ≤5g/kg (0.5%).
Instead of the standard GB 2548-1993.
The main difference between this standard and "DDVP" of GB 2548-1993 are.
1) Specification DDVP 50% and from 80% to 77.5% and 48.0%, respectively.
2) increase chloral control project.
Appendix A of this standard is an informative annex.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Pesticide Standardization Technical Committee (CSBTS/T C133).
This standard is drafted. Shenyang Chemical Research Institute.
Participated in the drafting of this standard. Nantong Jiangshan Agrochemical & Chemical Co., Ltd., Hubei Sanonda Co., Ltd., Hebei Xinfeng Pesticide
Chemical Corporation.
The main drafters. ZHANG Pi Long, Wang Zhimin, Lee Yuan, Zhou Guozhu.
This standard was first published in 1981.
This standard is the first revision in 1993.
This revision is the second revision.
Dichlorvos EC
Other names, structural formulas and physicochemical parameters of the product substantially dichlorvos active ingredient is as follows.
ISO common name. dichlorvos
CIPAC digital code. 11
Chemical name. O, O- dimethyl -O- (2,2- dichlorovinyl) phosphate
Structure.
Empirical formula. C4H7Cl2O4P
Molecular weight. 221.0 (according to 2007 international relative atomic mass)
Biological activity. insecticide
Boiling point. 234.1 ℃/1 × 105Pa
Vapor pressure (25 ℃, mPa). 2.1 × 103
Relative density (D20n). 1.425
Refractive index .( shape 20D). 1.4523
Solubility. Water 18g/L (25 ℃), dissolved in kerosene, 0.2% to 0.3%, soluble in most organic reagent
Stability. The thermal stability, slow hydrolysis, in a basic medium faster in water or in an acidic medium, the generation of hydrogen and dichloro dimethyl phosphate
Acetaldehyde, DT50 (22 ℃) (pH4 about 31.9d, pH72.9d, pH92.0d, have a corrosive effect on the iron and mild steel, stainless steel, aluminum, nickel not
Corrosive
Range 1
This standard specifies requirements for DDVP, Test Method for marking, labeling, packaging, storage and transportation.
This standard applies to the drug and dichlorvos dissolved emulsifiers formulated in a suitable solvent DDVP.
2 Normative references
Terms of the following documents become provisions of this standard by reference in this standard. For dated reference documents, all later
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to agreements based on this standard
Whether the latest versions of these documents. For undated references, the latest version applies to this standard.
Preparation GB/T 601 standard titration solution Chemicals
GB/T 1600 Pesticide Method Moisture
GB/T 1603 Determination of emulsion stability of pesticide
GB/T 1604 pesticide regulations for acceptance of goods
GB/T 1605-2001 sampling commercial pesticides
GB 4838 EC pesticide packaging
GB T 19136 Determination of heat storage stability of pesticide /
GB/T 19137 Pesticide low temperature stability determination
3.1 appearance and composition
This product is compliant with the original drug dichlorvos dissolved emulsifiers formulated in a suitable solvent, yellow-brown to pale yellow or colorless
Stable homogeneous liquid, free from visible foreign matter.
3.2 dichlorvos EC shall comply with the requirements of Table 1.
Table 1 dichlorvos EC Control Project Index
project
index
77.5% 48.0%
Dichlorvos mass fraction /% 3.5-2.5 77.5 + 48.0
+3.0
-2.0
Chloral mass fraction /% a ≤ 0.4
Acidity (H2SO4 basis) /% ≤ 0.3
Moisture content /% ≤ 0.1
Emulsion stability (200-fold dilution) Eligible
Low temperature stability of a qualified
Passing a heat storage stability
In a normal production conditions, the mass fraction of chloral, heat storage stability, low-temperature stability test at least once every three months.
Test Method 4
4.1 Sampling
Carried out in GB/T 1605-2001 of "liquid formulation sampling" approach. Determining Sample packages with a random number table method; final sample size
Not less than 100g.
4.2 Identification Test
GC --- present identification test can be performed simultaneously with dichlorvos content. Chromatography under the same operating conditions, the sample solution
Liquid retention time of the main peaks of the standard solution of dichlorvos peak retention time of which relative difference should be less than 1.5%.
4.3 Determination of mass fraction dichlorvos
4.3.1 Method summary
Sample was dissolved in chloroform to n-pentadecane as an internal standard was chromatographed in 10% DC-550 column, with a hydrogen flame ionization
Measuring detector, internal standard. Dichlorvos mass fraction measured thermal conductivity detector may also be employed measurement method, see the attached chromatographic operating conditions
Record A.
4.3.2 Reagents and solutions
Chloroform;
Stationary phase. silicone DC-550;
Vector. a test 101 (180μm ~ 250μm) (or other vector with the same performance), freshly prepared with aqua regia digestion at 80 ℃
After 16 ~ 24h, washed with water, dried, sift;
Sample dichlorvos. DDVP known mass fraction ≥99.0%;
Internal standard. n-pentadecane (no interference of impurities chromatography analysis);
Internal standard solution. Accurately weigh 5g n-pentadecane, was placed 500mL volumetric flask, dissolve and dilute to volume with chloroform, shake.
4.3.3 Instruments
GC. a hydrogen flame ionization detector;
Chromatography or chromatography ChemStation data processor;
Column. 2m × 3.2mm (i.d.) Borosilicate glass column (column or stainless steel);
Microsyringe. 10μL.
Column packing. DC-550 coated on the test carrier 101 (180μm ~ 250μm), stationary phase. (+ vector fixative) =
10.100.
4.3.4 GC operating conditions
Temperature (℃). oven 174, the gasification chamber 200, detector 250;
Gas flow rate (mL/min). carrier gas (N2 of) 30, hydrogen gas 30, air 300;
Retention time (min). about 2.2 dichlorvos, n-pentadecane 3.8.
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 gas chromatograph DDVP shown in Figure 1.
1 --- solvents;
2 --- dichlorvos;
3 --- n-pentadecane.
Gas chromatogram of FIG. 1 DDVP
4.3.5 Determination Step
4.3.5.1 Sample Weigh 0.15 g of DDVP (accurate to 0.0002g) was placed in a glass bottle with a stopper, with a pipette accurately added to 5mL
Standard solution, shake.
4.3.5.2 weighed sample containing 0.15g of dichlorvos (accurate to 0.0002g), placed in a stoppered glass bottle by using the 4.3.5.1
With an accurate pipette 5mL was added to the standard solution, shake.
4.3.5.3 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 pins and the internal standard peak area dichlorvos adjacent peaks
After the area ratio of relative change is less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.3.6 computing
Dichlorvos mass fraction of the sample 1 (%), according to equation (1).
(1)
Where.
--- [gamma] l standard solution, dichlorvos average peak area ratio of the peak area of the internal standard;
--- [gamma] 2 in the sample solution, dichlorvos average peak area ratio of the peak area of the internal standard;
--- standard of dichlorvos mass fraction, expressed as%.
4.3.7 allows poor
The measurement results of the two parallel error should not exceed 1.0%, and the arithmetic mean value as a measurement result.
4.4 Determination of the mass fraction of chloral
4.4.1 Method summary
Sample was dissolved in chloroform, dried over 5% HP-5 capillary column separation, determined by a flame ionization detector, external standard.
4.4.2 Reagents and solutions
Chloroform;
Chloral hydrate Sample. A known mass fraction ≥99.0%.
4.4.3 Instruments
GC. a hydrogen flame ionization detector;
Chromatography or chromatography ChemStation data processor;
Column. 30m × 0.32mm (. I.d) fused silica capillary column, wall coated with 5% HP-5 fixative, a film thickness of 0.2 m;
Microsyringe. 10μL.
4.4.4 GC operating conditions
Temperature (℃). oven maintained 41 ℃ 5min, 30 ℃/min was heated to 200 deg.] C maintained 5min, the gasification chamber 200, detector 250;
Gas flow rate (mL/min). carrier gas (N2 of) 30, hydrogen gas 30, air 300;
Injection volume (μL). 1.0;
Retention time (min). chloral about 3.3.
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 gas chromatograph chloral shown in Figure 2.
1 --- chloral;
2 --- dichlorvos.
FIG 2 is a gas chromatogram of chloral
4.4.5 Determination Step
4.4.5.1 Preparation of standard solution
Bonding said water chloral 0.13 g of standard sample (accurate to 0.0002g) was placed in a 25mL volumetric flask, dissolved with chloroform, diluted
To the mark and shake. With a pipette to another 10mL of 2mL volumetric flask, dissolved with chloroform, shake diluted to the mark.
4.4.5.2 Preparation of sample solution
3g weighed sample chloral (accurate to 0.0002g), placed in a 10mL volumetric flask, dissolved with chloroform, dilute to the mark with
Degree, shake.
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, the needle until two adjacent peak area becomes relatively chloral
After less than 1.2% of, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.4.6 computing
Chloral content of the sample 2 (%), according to equation (2).
147.4
165.4
(2)
Where.
A1 --- the standard solution, chloral peak area;
A2 --- sample solution, chloral peak area;
Molecular Weight 147.4 --- chloral;
165.4 --- molecular weight of chloral hydrate;
--- Sample mass fraction of hydrated chloral, expressed in%.
4.5 Determination of acidity
4.5.1 Reagents and solutions
Ba standard titration solution of sodium hydroxide (NaOH) = 0.02mol/L; according to GB/T 601 is formulated;
Methyl red indicator solution. 2g/L ethanol solution.
4.5.2 Determination Step
1g sample was weighed (accurate to 0.0002g), placed in 250mL Erlenmeyer flask, was added 100mL of water, was added 3 drops of methyl red indicator
Solution immediately with 0.02mol/L sodium hydroxide standard titration solution was titrated to orange is the end. At the same time a blank determination.
The acidity of the sample 3 (%), according to equation (3) is calculated.
× 3 = Ba
(Qiao Qiao 1- 0) × M
(3)
Where.
--- Ba actual concentration of sodium hydroxide standard titration solution in units of moles per liter (mol/L);
Qiao 1 --- titration sample solution, the consumption of sodium hydroxide standard titration solution volume in milliliters (mL);
V0 --- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution in milliliters (mL);
--- molar mass M sulfuric acid values, in units of grams per mole (g/mol), M 12H2SO () 4 [] = 49.
4.6 Determination of Moisture
Carried out in GB/T 1600 in the "Karl Fischer" method. Allows the use of equivalent accuracy trace moisture analyzer.
Determination of emulsion stability 4.7
The standard hard water sample was diluted 200-fold, proceed as GB/T 1603. The test results, without the oil slick, with no sink or precipitated as an oil
qualified.
Thermal storage stability test 4.8
According to GB/T 19136 and is complete measurement dichlorvos content, acidity, and emulsion stability within 24h after the heat storage, the measurement result
Dichlorvos mass fraction should be greater than the measured average mass fraction of 85% prior to storage, the acidity should not exceed 1.0%, the emulsion stability should be qualified.
4.9 Low temperature stability test
/ T 19137 performed in GB , the volume of the precipitated solid or oil is not more than 0.3mL qualified.
4.10 product inspection and acceptance
Product inspection and acceptance shall comply with GB/T 1604's. Process limit values, the comparison value using rounding.
5 marking, labeling, packaging, storage and transportation
5.1 dichlorvos EC mark, labeling and packaging should comply with the provisions of GB 4838.
5.2 dichlorvos EC application of clean, dry glass bottles, bottle net weight 100g, 200g, 500g, etc.; with the packaging plastic box,
Carton net content not exceeding 15kg.
5.3 protocol based on user requirements or orders, may take other forms of packaging, subject to the provisions of GB 4838.
5.4 DDVP package airiness, dry place.
5.5 storage and transportation to prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, nose and mouth to prevent inhalation.
If swallowed, immediately induce vomiting.
5.7 Warranty. Under the provisions of storage and transportation conditions, DDVP guarantee period, counting from the date of manufacture 2 years. Within six months dichlorvos quality
Fraction should meet the requirements of 3.2, the acidity should not exceed 0.6%; 2 years, 77.5% DDVP mass fraction of not lower than 73.0%,
48.0% of the mass fraction of dichlorvos should not be below 45.5%, the acidity should not exceed 1.0%.
Appendix A
(Informative)
Dichlorvos gas chromatographic mass fraction of the thermal conductivity
A. 1 Method summary
Sample was dissolved in chloroform to n-pentadecane as an internal standard, using the DC-550 is a thermal conductivity detector and a column filler, for test
Samples dichlorvos and measured by gas chromatography.
A. Reagents and Solutions 2
With 4.3.2.
A. 3 Instrument
Gas chromatograph. a thermal conductivity detector;
The other with 4.3.3.
A. 4 GC operating conditions
Temperature (℃). 174 column temperature, the gasification chamber 200, the detector chamber 180;
Gas flow rate (mL/min). carrier gas (H2) 100;
Retention time (min). about 2.2 dichlorvos, n-pentadecane 3.8.
Analysis may according to the difference of instrument performance and columns, chromatographic operating conditions appropriately adjusted to obtain the best result.
A. Determination Step 5
A. 5.1 preparation of standard solution
Sample Weigh 0.15 g of DDVP (accurate to 0.0002g) was placed in a glass bottle with a stopper, with a pipette 5mL accurate internal standard solution was added
Liquid, shake.
A. 5.2 of the sample solution prepared
Weigh a sample contains about 0.15 g of DDVP (accurate to 0.0002g), and placed in a stoppered glass bottle, added with a pipette 5mL internal standard
Solution, shake.
A. 5.3 Determination
Under the above operating conditions, the instrument until a stable baseline, the number of consecutive doses of the standard solution is injected, the needle was calculated for each dichlorvos internal standard peak area
The ratio of repeatability, when change in the relative ratio of the two needles dichlorvos internal standard peak area of less than 1.2% to be adjacent, in accordance with standard sample solution, the sample
Solution, the sample solution and standard solution were sequentially measured.
A. 6 computing
The two pins of the sample solution and measured peak area ratio in the two doses of the standard solution and internal standard substance dichlorvos longitudinal samples were averaged.
Dichlorvos mass fraction of the sample 1 (%), according to equation (A.1) is calculated.
1 = γ2
(A.1)
Where.
--- [gamma] l standard solution, the average peak area dichlorvos internal standard peak area ratio;
--- [gamma] 2 in the sample solution, the average peak area dichlorvos internal standard peak area ratio;
Book GB 2548-2008
--- standard of dichlorvos mass fraction, expressed as%.
A. 7 allows poor
The measurement results of the two parallel should be less than 1.0%, and the arithmetic mean value as a measurement result.
8002-
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