Some standard content:
Industry Standard of the People's Republic of China
HG2105-91
Insecticide Aqueous Agent,
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implementation on July 2, 1992
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HKNiKAca-
HC 2205—91
This standard specifies the technical conditions, test methods, inspection rules, labeling, packaging, transportation and storage of insecticide aqueous agents. This standard is applicable to insecticide aqueous agents synthesized with dimethylformamide, o-methylformamide, etc. as raw materials. Active ingredient: N,N-dimethyl-N-(2-dimethyl-4-nitro)methyleneimine hydrochloride Trade name: Fentanyl
Structural formula:
Molecular formula: cuH,z
CI-IICI
Molecular weight: 233,400 987 International Relative Mass) Reference Standard
Chemical Reagent Titration Analysis (Content Analysis) Preparation of Standard Solution G eo
Test methods for chemical reagents--Preparation of preparations and products B
GB1604 Pesticide inspection rules
GB1605 Commercial pesticide sampling method
GB3706 General rules for pesticide packaging
Technical requirements
3.1 Appearance: light yellow to reddish brown aqueous solution. 3.2 Pesticide aqueous solution should meet the following technical requirements:
Contains modified ingredients. (2/m)
Acidity (calculated as HCI), % (m/m)
Hot storage test dust 1
Note: 1) This is a reverse test item, and it is inspected once every six months. 4 Test methods
4.1 Determination of appearance
Use visual observation method
Approved by the Ministry of Chemical Industry of the People's Republic of China on 1S91-11-18 28+
+, t~-9. 0
1992-07-1 implementation
4.2 Determination of effective or tooth
4. 2. 1 Method summary
HG 2205---91
The effective or tooth of this standard is determined by gas chromatography. After the sample is neutralized with nitrogen water, the distilled water is taken and used as the internal standard. The sample is separated by using 5P G-2IM "=" KOH; : 01AW chromatograph and effective initial ionization detector, and the area method is used for quantification. 4.2.2 Instruments
4.2.2.1 Gas chromatograph: only hydrogen fusion ionization detector; 4.2.2.2 Chromatographic phase, 5% PEG 20M + 5% KOH/101AW, t80~-250μm (6t~-0 4.2.2.3 Microdisc syringe, 14L, 4.2.2.4 Simple separatory funnel: 25ml. 4.2.3 Reagents As stated in the specification, the reagents used in this standard are all analytical functions, and the chromatographic gas should meet the requirements of the chromatographic specification. 4.2.3.1 101 Acid selection (AW) Chromatographic medium: 180-250um (60--8℃) Chromatographic elimination group Polyethylene glycol-20000 (PEG20M): Chromatographic standard: 4.2.3.2 4.2.3.3 Carrier gas: bottle gas, 4.2.3.4 Insecticidal standard: high purity [-99.6%; 4.2.3.5 Water (GR 631)
4. 2. 3. 6 Lactone (GR 686)+
4. 2. 3. 7
Potassium oxychloride (GB 2306):
42.3B Stilbene (trans-diphenylethylene): Experimental reagent 4.2.3.9 Benzene (GB 690).
42.4 Preparation of color samples
4.2.4.1 Disinfection of support
Weigh 30 g of PEG-20M% and 0.33% of potassium hydroxide (accurate to 1.2 g), place in a 250 mL measuring flask, add 40 mL of acetone, and dilute with 5 mL of water. Heat slightly in a hot water bath to completely dissolve, then add 10 mL of acid-washed white solid (accurate to 0.1 g), heat to reflux for 2 h, let stand in the cold water for about 1 h, then drain 10 mL of the solution. Place in a ventilated tube under an infrared lamp without stirring to allow the floating agent to completely evaporate, and bake at 110°C for 2 h. 4.2.4.2 Filling and aging of negative spectral rod
Put the above-mentioned cleaned support into the column so that the filling is even and dense in the column (approximately 3.5g of filling material). Then plug a small amount of glass wool at the inlet of the column and press it appropriately. Connect the inlet of the column to the vaporization chamber and the outlet end to the detector. Age for 24 years at a column temperature of 280°C and a flow pressure of 98MPa (1kgf/cm2). 4.2.5 Determination steps 4.2.5.1 Gas chromatography conditions: Column temperature 154°C, vaporization 20°C, detection 183°C gas flow, carrier gas bottle gas + 40ml./min front positive pressure 0.008MPa (0.kg/cm, air 60cmL/mia, hydrogen 25ml./min retention time, insecticide swelling 11mm2 & s + Mao (internal standard) about 18min, gas chromatogram as shown: HG 2205-91 Figure 丨 Gas chromatogram I-N,N-methyl-( methylbenzene)methoxy; 2N,V--methyl-N*-≤2-methyl-6-methoxy-1-methylbenzene>methylbenzene: 8-methylbenzene 14-methylbenzene The analyst may make appropriate adjustments to the following conditions according to the characteristics of the instrument in order to achieve the best separation effect. 4.2.5.2 Preparation of internal standard solution
Weigh 4.0g of stilbene (accurate to ±0.0002g) in a 200ml bottle. Dissolve in benzene and dilute to the mark. 4.2.5.3 Preparation of standard solution
HKNKAca
Weigh about 0.08g (accurate to 0.0002g) of the insecticide standard into a 25mL simple separatory funnel, add 2~3ml of distilled water to dissolve it. Neutralize it with 1+1 nitrogen water to a pH of about 8 (calibrated with a pH test line of [~14]), then take 6mL of it twice, combine the benzene layer, and discard the water layer. Then accurately aspirate 5mL of the internal standard solution, probe and set aside. 4.2.5.4 Preparation of the sample solution
Weigh 0.3~0.5g (accurate to 0.0 002g) in a 25ml. simple separatory funnel, add 2~8mL of ethanol to dilute it, neutralize it with 11% nitrogen water to about 8 (check with 14-15% pH test paper), then extract it once with 6mL of ethanol, combine the benzene layers. Discard the water layer. Then accurately pipette 5ml of internal standard solution, shake the spoon and standby. 4.2.5.5 Determination
Under the chromatographic conditions of 4.2.5.1, first inject several injections of standard solution, and the ratio of the product of the insecticide and internal standard peaks of the two injections of standard solution before and after is equal. When the deviation is not greater than 2%, it is considered that the instrument response base is unstable. Then the sample is analyzed in the following order: standard solution, sample solution: sample solution, d. standard solution. 4.2.5.6 Calculate the chromatograms obtained by injecting the standard solutions a and d, and measure the peaks and products of the internal standard of the insecticide family respectively. The formula is as follows: 1) Calculate the quantitative positive factor of insecticide family
Where: m
The mass index of the standard product!
The mass of the internal standard added;
HG 2205-97
The average value of the peak area of the insecticide on the chromatogram of the two standard solutions, nA: The average peak area of the internal standard on the chromatogram of the two standard solutions: [mI According to the chromatograms obtained from the two test solutions b and c, the peak areas of the insecticide and the internal standard are measured respectively, and the percentage of insecticide contained in the sample (X,) is calculated according to formula (2):
Where:
The mass of the sample·g?
1The mass of the internal standard, 8:
A, The average value of the peak area of the insecticide on the chromatogram of the non-test solution, mm\: A—The average value of the peak area of the internal standard on the chromatogram of the two test solutions, mm,"-The percentage of insecticide contained in the standard, %, 4. 2. 5-7 Method Recommendations
The maximum allowable deviation of the results of two parallel determinations of this method is 1.5%. 4.3 Determination of Acidity
4.3.1 Reagents and Solutions
4.3.1.1 Formaldehyde Red (HG3958) Indicator: 1g/1. Ethanol Solution (prepared according to GB603): 4.3.1.2 Sodium Hydroxide (GB29) Standard Solution: c(VaOH)-U.Imo./L standard solution (connect GH60 preparation standard) 4.3.2 Determination of the media
Weigh about 1g of the sample (accuracy 0.cc02g) and put it into a 250ml. Erlenmeyer flask. Add 5UmL of distilled water, add 2 drops of methyl red index, and titrate with 0.1mul/mL sodium hydroxide standard solution until the color is 4.3.3 Calculate the concentration (x) according to formula (3):
Xx=Vx0.3365x100
Wherein, -
actual liquid density of sodium hydride standard solution, ul/L volume of sodium hydride standard solution, mL; V
m2—mass of the sample, g:
.0865-
and 1.000ml. Standard solution of hydrogen peroxide e(2a0H) = 1.030mol/l equivalent, expressed in grams of hydrochloric acid.
4.4 Thermal stability
4.4.1 Apparatus wwW.bzxz.Net
4.4-1-1 Oven: Temperature control accuracy is ±2°C: 4.4.1.2 Ampoule: Capacity is about >unL, long neck. 4.4.2 Determination
Use a medical sprayer to take about 30ml of sample, put it into a clean ampoule (note! Do not let the sample touch the neck of the ampoule), and use a gas lamp to spray fire to seal it (note: avoid evaporation of the sample when sealing). At least two bottles. Weigh accurately to 0.1g). Place the sealed container in a gold container and then place it in a 151+2" oven for 11 days. After taking the container out of the oven, cool it and weigh it for testing (the weight should be the same as before hot storage, indicating no leakage). If there is no leakage, it can be tested as specified in Article 4.2. After hot storage, the content of the active ingredient of the insecticide is allowed to drop to 85% of the content measured before, which is qualified.
5 Inspection rules
5.1 Test of GR 1604 Near acceptance. The period for hot storage stability test is half a year. 5.2 Sampling shall be carried out in accordance with the provisions of GB1605.
5.3 The quality assurance period of insecticide water is two years. During the guarantee period, the content of insecticide active ingredients shall not be less than 16.0%. 6 Marking, packaging, transportation and storage
6.1 The marking of insecticide water shall comply with the provisions of CB3796. 6.2 Insecticide water is packaged in rubbed glass bottles, with a net weight of 1.6kg or 1kg per bottle, and the bottle is lined with straw, straw mat or powder paper. They are densely arranged in the packaging box, and the net weight of each box shall not exceed 15kg. Its outer packaging The packaging should be in plastic boxes or wooden boxes and should comply with the provisions of GB3796. 6.3 It must be carefully lifted and placed during transportation. It must not be inverted and avoid collision and heavy pressure. 6.4 It must be strictly protected from rain and vomiting. Keep a good headwind. It must not be mixed with food, seeds, feed, etc. to avoid contact with the skin and prevent oral inhalation.
Additional remarks:
This standard was proposed by the Ministry of Science and Technology of the Chemical Industry of the People's Republic of China. This standard was proposed by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shanghai Pesticide Research Institute, and Xinjiang Longyou Pesticide Factory and Hunan Pesticide participated in the drafting. The main drafters of this standard are Wen Shu, Chen Zhongmin, Shang Yonglan, Tong Bing, Chang Weiying,
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