Some standard content:
UDC 661.718.1:543.06
National Standard of the People's Republic of China
GB 4651—84
Adjusted to: HG z-8y
Analytical method for technical phosphamidon1984-08-4Published
Implementation on 1985-06-01
National Standard Approved
National Standard of the People's Republic of China
Analytical method for technical phosphamidonUDC 661.718.1
GB4651—84
This name is applicable to the above-mentioned phosphamidon prepared by the condensation of methyl phosphatate and α,α-dichloro-N,N-ethylacetoacetamide. Compound CHuO, NC!
Structural formula:
P_0-C =C_C
Molecular weight: 2997 (according to the international standard in 1979)Test method
1.1 Determination of phosphoamine content
1.1.1 Instruments and reagents
1.1.1.1 Constant temperature water solution: Temperature control accuracy ±1℃: 1.1.1.2 Sodium hydroxide (GB629-77), analytically pure#1.1.1.3
Hydrochloric acid (G622-77), analytically pure
Sodium carbonate (GB639-77), analytically pure: 1.1.1.4
1. 1.1.1. 6
Sodium thiosulfate (637-77), analytically pure: Iodine (GB 675-77), pure;
washing powder;
water: fresh deionized water or distilled water that has passed through the exchange resin; 2N sodium hydroxide solution: prepared according to Article 2, Chapter 2 of GB601-77 "Standard Method for Preparation of Chemical Reagents"; 1.1.1. 10
1.1. 1. 13
1.1.1. 14
.
2V sodium carbonate solution: Prepare according to Article 5, Chapter 2 of GB601-77 5N hydrochloric acid solution: Prepare according to Article 3, Chapter 2 of GB601-77 0.1N iodine standard solution: Prepare according to Article 10, Chapter 2 of GB601-77 0.1N sodium thiosulfate standard solution: Prepare and standardize according to Article 7, Chapter 2 of GB601-77 0.5% starch solution: Prepare according to Article 221.1.2 of GB603-77 "Chemical Reagents and Reagents Preparation Methods" 2nd New Article 34 Determination steps
Weigh 1.2 g of phosphamidon oil (accurate to 0.001 g), place in 20 ml of water in advance 0 ml volume version, dilute with water to the scale, shake, pipette 10.0 ml of this solution into a 250 ml iodine bottle, add 20.0 liters of 0.1N iodine standard solution, wipe the iodine bottle carefully, mix it thoroughly, then add 20 ml of 2N sodium hydroxide solution, shake it, seal it with water, place it in a constant temperature (25±1℃) water bath in a dark place for 4-, keep it for 30 minutes, take it out, add 20 ml of 5N hydrochloric acid to acidify it, titrate it with 0.1N sodium thiosulfate standard solution until the solution is light brown, add 3 liters of 0.5% sodium sulfate solution, and continue titrating until the blue color of the solution just disappears as the end point, and record the milliliters of sodium thiosulfate standard solution consumed.
Take another 10.0 ml sample solution and place it in another 250 open iodine bottle, add 20.0 ml 0.1N iodine standard solution, and shake carefully. 1984-0814 issued by the National Bureau of Standards
1985-06-01 implementation
GB 4651-84
bottle, mix thoroughly, add 5 ml of 2N sodium carbonate solution, shake, seal with water, place in a constant temperature (25±1℃) water bath in the dark, keep for 30 minutes, take out, add 5 ml of 5N hydrochloric acid to acidify, titrate with 0.1N sodium thiosulfate standard solution until the solution turns light yellow, add 3 ml of 0.5% starch solution, continue titrating until the blue color of the solution disappears as the end point, and record the number of milliliters of sodium thiosulfate standard solution consumed.
1.1.3 Expression and calculation of results
The weight percentage content of phosphoamine (X) is calculated according to formula (1): 299.7
(V2-V))Nx
武: N
(V2-15) N ×149.8
---the equivalent concentration of sodium thiosulfate standard solution, N× 100 - 0.115 × X,
The volume of sodium thiosulfate standard solution consumed when titrating the sample with sodium hydroxide solution, liter; V,
The volume of sodium thiosulfate standard solution consumed when titrating the sample with sodium carbonate solution, dry liter: sample one, grams
Molecular weight of phosphamide;
The relatively high value of phosphamide content caused by dechlorophosphamide; X.—The weight percentage of dechlorophosphamide.
1.2 Determination of acidity of phosphamide
Reagents and solutions
Sodium hydroxide (GB629-77), analytical grade 1.2.1.1bzxZ.net
1.2.1,2 Bromophenol blue (HG 3 1224-79) 1.2.1.3 Sodium hydroxide standard solution, 0.02. Prepare and calibrate according to GB601-77 Chapter 2, Article 2. 1.2.1.4 0.4% phenol monitoring indicator: Prepare according to GB603-77 Chapter 2, Article 34, Item 31. 1.2.1.5 Water: Fresh deionized water or distilled water treated with ion exchange resin. (1)
1.2.2 Determination steps||tt| |Weigh 1-2 g of sample (accurate to 0.001 g), cover in a 250 ml triangular jar, add 100 ml of water, add 4-6 drops of bromophenol blue, and immediately titrate with 0.02N sodium oxychloride standard solution until the solution turns purple as the end point, record the number of milliliters, and perform a blank test at the same time. 1.2.3 Expression and calculation of results
Phosphoamine acidity percentage (2) According to (2), calculate (in terms of H2O2): (V/-V2) N×0.049
Where: N-
equivalent concentration of sodium oxychloride standard solution, N; V--volume of sodium oxychloride standard solution consumed when titrating the sample, ml; V
-volume of sodium hydroxide standard solution consumed when titrating the sample, ml: one sample, g;
grams of sulfuric acid per gram.
1.3 Determination of water solubility of phosphamide
1.3.1 Instruments and reagents
1.8.1.1 100 ml glass volume with ground mouth; 1.3. 1.2
Anhydrous calcium fluoride, analytical grade,
GB 4651-
1.3.1.3 Magnesium chloride (GB672-78), analytical grade 1.3.1.4 Calcium carbonate (HG3-1066-77), analytical grade, 1.3.1.5 Hydrochloric acid (GB622-77), analytical grade; R
1.3.1.6 Standard hard water: with a hardness of 342 ppm calculated as calcium carbonate. Prepared according to Article 6 of GB1603-79 "Determination of stability of pesticide emulsions".
1.3.2 Determination steps
Take 100 ml of standard hard water, add 100 ml of measuring cylinder with ground stopper, use a pipette to draw 0.25 liters of phosphamide sample, add it to the hard water in the measuring cylinder, cover the stopper, within 5 seconds, up and down three times, and observe the sample for 30 seconds. If the sample is completely dissolved in hard water, it is qualified for water solubility.
1.4 Determination of dechlorophosphamide content
1.4.1 Instruments
Gas chromatograph: 102G (produced by Shanghai Analytical Instruments) or other types of instruments with thermal conductivity cell detector. b.
Chromatographic column: 2 meters long, 3 mm inner diameter stainless steel column. c.
Micro syringe: 10 microliters.
1.4.2 Reagents
Acetone (GB686-78), analytical grade:
Trichloromethane (GB682-78), analytical grade 1.4.2.3 Dechlorophosphamide standard
1.4.2.4 Tris 1 phosphate (internal standard), chromatographic grade; 1.4.2.5 101 silylated support (Shanghai Reagent-produced), 60-80 days 1.4.2.6 SE-30 (stationary phase), imported. 1.4.3 Preparation of chromatographic column
Use trichloromethane as solvent, prepare 10% SE-30 stationary phase, use 1u1 silylated support (60-80 taels) as support, and load the column after the solvent evaporates. Install the column into the chromatograph, do not connect the detector to the column outlet, pass a low flow rate (such as 15L/min) of carrier gas, slowly raise the temperature to 250℃ in sections, and age continuously for 24 hours. Adjust the instrument to normal working state according to the operation, and start the measurement after the stop line is stable.
1.4.4 Operating conditions
Take 102G instrument as an example:
Column temperature: 200℃ (actual temperature);
Vaporization temperature: 220℃ (surface temperature);
Carrier gas: Hydrogen (H2O);
Pressure before column: 1 kg/cm2
Carrier gas flow rate: 17 ml/min;
Bridge flow: 200 mA;
Attenuation: 1/1;
Paper speed: 5 mm/min,
Injection volume: 4 μm;
Pressure holding time: Dechlorophosphamide 5.1 points, phosphate ester 3.2 points 1.4.5 Determination steps
Take 0.1 part of phosphate diester, put it in a 25-liter volumetric flask, dilute to the scale, this is the internal standard solution, and then weigh 0.15 grams of dechlorophosphamide standard sample and 0.28-0.32 grams of phosphate amine sample (accurate 0.0002 grams), two vials of comminuted, weigh the solution in 2.5 milliliters of standard sample and test sample, and mix them thoroughly. After the instrument is normal, measure in the order of one needle standard, "needle sample crystal needle standard". Calculate the average value of the peak height ratio of dechlorophosphamide to the internal standard of the standard sample and the test sample. The chromatogram of the dechlorophosphamide standard is as follows:
GB 4651
Chromatogram of dechlorophosphamide standard
1 -acetyl ether-ethylamine, 2-chloroacetoacetamide, -nitrogen-substituted diethylamine: 4-phosphoric acid: ester: 5-dephosphamide: 6-α-phosphamide, 7-phosphocolloid 1.4.6 Expression and calculation of results
The weight percentage of dechlorophosphamide (Xs) is calculated according to formula (3): Wherein, H,
GB4651-84
the average value of the peak height ratio of dechlorophosphamide to the internal standard of the tested sample, 11-the half-mean value of the peak height ratio of dechlorophosphamide to the internal standard of the standard sample; W,-the weight of the tested sample, g,
the weight of the standard sample, g;
-the content of dechlorophosphamide in the standard sample, %. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is issued by the Qingdao Pesticide Department of Shandong Province! The main drafters of this standard are:
People's Republic of China
National Standard Beach
Phosphamide crude oil analysis method
GB 4651-84
Published by China Standard Press
(Beijing Fuwai Erlihe)
Printed by China Standard Press Printing Workshop
Distributed by Xinhua Peidian North Distribution Office in various Xinhua Bookstores Jingzhe Format 880×12301/16 Printing Sheet 1/2
Number of copies 9,000
First and last edition in March 1985
1985: March 1st Edition
Printing Quantity 1—7,000
Book Number: 151691-2901
Price 0.20 yuan
Standard 15-51
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