This standard specifies the test method for chlorotoluron residues in grains. This standard is applicable to the determination of chlorotoluron residues in wheat, corn and soybeans that have been treated with this herbicide. The detection limit of this method is 0.01mg/kg; the linear range is 0.04mg～2.00mg. GB/T 5009.133-2003 Determination of chlorotoluron residues in grains GB/T5009.133-2003 Standard download decompression password: www.bzxz.net

ICS67.040
National Standard of the People's Republic of China
GB/T5009.133--2003
Replaces GB/T16338--199S
Detertninalion nf chlnrotnlurnn residues in grains
Detertninalion nf chlnrotnlurnn residues in grains2003-08-11Promulgated
Ministry of Health of the People's Republic of China
Standardization Administration of China
2004-01-01Implementation
This standard replaces 6H/16338-19 Determination of the content of chlorotoluron residues in grains3. GR/T 5068.133--2003
This standard follows GB/T 2009-1.4-2001$ standard writing rules Part 1, chemical analysis methods 3. The original standard was revised.
This standard was issued and returned by the Ministry of Health of the People's Republic of China. The sponsoring units of this standard are: Public Health College of West China University of Medical Sciences, Sichuan Provincial Health Prevention and Control Station, Sichuan Institute of Labor Health and Occupational Disease Prevention and Control.
The main drafters of this standard are: Yuan Qing, Hu Wenzao, Sun Chengye, Xiang Renxue, Zhang Lishi. According to the standard, it was published in 2003, and this is the first revision. 15
GB/T 5009.133-2003
Chloroquine (c:hlnininlurnm), chemical name is N-(3-4-methylphenyl)-N,N-methylpyridine, is a selective endosmotic herbicide. It is used to control various weeds in rice, corn and soybean. It has been widely used in China since the 1990s. The original drug and 25% wettable powder are produced by some domestic agricultural factories and have obtained the agricultural product tax registration. 60
1 Scope
Determination of residual chlorine in green wheat
This standard specifies the test method for residual chlorine in grain. The standard is used to determine the residual chlorine in wheat, corn and soybean that have been treated with this herbicide. The detection limit of this method is 0.01\/k and the linear curve is 0.04mg-2.00. 2. Reagents
GB/E5009.133—2003
The green in the sample is removed by shaking with medium alcohol water, filtered: the filtrate is extracted with hydrogen methane-phenol mixture, washed with phenol, adsorbed on silica, the eluent is concentrated and then precipitated under oxygen, the derivatives are determined by gas spectroscopy and electron capture detector, the retention time is used for qualitative analysis, and the curve is used for quantitative analysis. 3. Reagents
3.1 Methanol, or distilled.
3.2 Dimethoate or distilled
3.3 Methane monoxide: calorimetric
3.4 ​​Petroleum nitrate, boiling range 6℃~90℃, 3.5 Acetone: distilled.
3.6 Hexane distilled.
3.7 Anhydrous sodium sulphate,
3.652g/mol carbonate:
3.9 Ground and oxidized liquid,
3.10 Heptachlorohydrin: pure
3.11 Iron adsorbent, 100~200g, calcine at 50℃ for 5 minutes, place in a container, collect 100g silica-magnesium adsorption sieve and add 5mL fire water to activate before use, balance overnight, set aside, and place for more than 3 hours If the amount is too large, it should be dried at 130℃ for 5 minutes before use, and then activated by adding ice according to the ratio stated in the process:
3.12 Green branch sequence new performance: Prepare deep space standard (heart hour, use two ions to make a 1m/mL standard solution and store it in ice box (4℃). When using disease oil, it is necessary to select a 10/mL standard solution. 4.1 Gas chromatograph: equipped with electron capture detector (E: 4, 2 small food chromatograph. || tt||4.3 Electric vibrator.
4.4 Water tank for packaging
4.3 Small to full-scale medical screen device or age converter. 5 Analysis steps
5.7 Sample pretreatment
5.1.1 Take the soybean, wheat and powder samples and pass them through 20-month sieves, weighing about 35% of the sample, and sell them to .001. It takes 25 plugs, 120m of water for 3+2000min with electric lifting. Rapid qualitative analysis, 161
CB/I5009.133-2003
Filter into a 25°C container, add 80 ml of formaldehyde (3+2) to the residue, sieve for 30 min, thin, combine the solution, dilute with formaldehyde 5+ to mt:
For the corn sample, collect 59 ml of the solution (equivalent to 5 g of dry sample) and place it in a 250 ml separatory bucket, add 20 ml of sodium chloride and 30 ml of distilled water, and use monoxide-free formaldehyde (3. 5+5,5> mixture was shaken and extracted 3 times, each time with 20mL of solvent, and shaken for 1min. Combined dichloromethane-petroleum ether extract and dried wheat sample, 50mL of filtrate (equivalent to 5g sample) was placed in a 250ml separatory funnel, cut into 0ml of energy and sodium chloride solution, and extracted 3 times with triclosan-nitropropane [3.5+6.5), each time with 2UmL, and shaken for 1min: Combined dichloromethane-petroleum ether extract and acetylene ether extract, 20ml. saturated sodium chloride solution was added, and after standing for stratification, the lower layer of sodium chloride was obtained. Extraction was carried out by reverse extraction through a funnel with 1g of anhydrous active ingredient, and the mixture was poured into a 0ml bottle. A small amount of the residue was removed by washing the funnel and its contents, and the washing liquid was formed into a filtrate. 6) Most of the solvent was condensed under reduced pressure in a warm water bath at -1°C: the solution was dried with nitrogen or purified air, and 5mL of the right oil solution was used for treatment.
5.1.2 Purification In a chromatography column with an inner diameter of 1m to 2m, load 2 anhydrous sodium sulfate, weigh 1g to 15g of the sample. Use 30mL of petroleum aldehyde to wet-pack the column, and spread 1cm of anhydrous sodium sulfate on the top of the column. When the liquid level in the column drops to the surface of the column, turn the test column over and carefully transfer it to the chromatography column. Elute with 5mL of acetone-no-oil fermentation (1 + 1). Wash the column several times with the eluent. After the sample solution is filled in a steel-bottomed flask, transfer it to the chromatography column. The elution rate is 0.5mL/min. mir~2,0mL/min, collect the eluent in a 150ml bottle with two stoppers at the bottom. Add 62℃+1* constant temperature water to reduce the concentration of the solution, use nitrogen or purified air to dry the solution once, add 0.00ml of n-butyl ether to stabilize the solution,
5.1.3 Add 20L of 1% anhydride to the flask, cover it and put it in a 60℃ constant temperature water pan, heat the reaction for 1 hour. After taking it out, cool it to room temperature with water, add 4% carbon monoxide and sodium nitrogen solution, and mix. Transfer the new biomass into a 100 mL stopper tube, and take the upper layer of n-hexane to melt for gas chromatography analysis: 5.2 Instrumental analysis
Gas chromatography equipment: 2mm×3mm stainless steel column, with a stationary phase of V-17, ChromugorbAWDMcS (30 days~1 day). The column temperature is 75, the sample detection room temperature is 230℃, and the chlorine gas flow rate is 30L/min: 5.3 Preparation of standard solution Www.bzxZ.net
Take 0, 0, 0.0.0.0.20, 0.40).9.600.81.1. (10m green kettle standard is used in 10m test tube. Add n-hexane to 4.00mL. Derivatize according to 5.1,3 derivatization steps, collect the upper layer of n-hexane drops for gas chromatography analysis ：Take 2.0L of standard solution and inject it into gas phase chromatography. Repeat the measurement \ times each time. Take the concentration of standard solution as the yellow axis and the average value of the peak height as the ordinate to construct a standard curve.
5.4 Determination
Take 2.0L of the sample solution after derivatization and inject it into the gas phase chromatography. Repeat the measurement 3 times and measure the average value of the peak height of the sample. Take the holding time for qualitative analysis and the standard curve and sample for quantitative analysis. 5.5 Calculation of results
During the determination, when the injection volume of the sample solution and the standard solution is the same, the amount of isocyanate in the sample is calculated according to the following formula. XV
The total amount of isocyanate in the test solution, the unit is grams per gram
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