Some standard content:
Chemical Industry Standard of the People's Republic of China
HG3291~3297—2001
(2001)
Published on January 24, 2002
Implementation on July 1, 2002
Published by the State Economic and Trade Commission
Reference number: 10083—2002
1G3296—2001
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard is a revision of the original HG3296-1989-1989 standard. The main technical differences between this standard and H3286-1989 are: adding phosphite and desiccant control spray, deleting acidity and moisture control, adding pulp test. The analytical method of diethyl ether is equivalent to the International Pesticide Analysis Cooperative Committee C1PAC:384/FC/V/- (1993) method. Added phosphite and olefin measurement method. Deleted the carrier and moisture measurement method. This standard is proposed by the National Pesticide Standardization Technical Committee from the date of implementation. The sponsor of this project is: Biyang Chemical Research Institute, the sponsor is: Zhenjiang Jiangnan Chemical Industry Co., Ltd. The main contributors of this project are Zhang Gelong, Ti Yandan, Tu Baojie and Ji Dafang. This standard was first issued as a professional standard in 1985, and was converted into a mandatory chemical industry standard in 1999, and was re-edited as JIG3291Se9. The editorial committee of this standard approved the interpretation of the National Pesticide Standardization Technical Committee, 15 Chemical Industry Standard of the People's Republic of China. The name, structure and basic chemical properties of the product are as follows: Isu Applicable name: rosetylaluminium tfoactyl-Al) Common name, diethyl phosphine. CIPAC number: 384 t||Chemical name: di(ethyl acetate) t
Structural formula:
Empirical formula: CHiaAlO,P
Relative molecular weight, 354.11 (according to the atomic mass of 1997) Physical Standard: chlorinated
Melting point: 200 Decomposition
Benzene gas (25), ≤10-Pa
HG3296-2001
Solubility (20℃, /.) In water 120, methanol 920, in methanol 45 ethyl acetate, in acetic acid, in chloroform 5X102
Stability: Stable in the range of 1 under normal storage conditions
This standard specifies the requirements, test methods, as well as marking, labeling, packaging and transportation of aluminum triacetate technical. This standard is used to prepare triethylamine technical pesticides produced by various processes. 2 Referenced standards
The provisions of the following standards are all cited in this standard and become the main text of this standard. The versions shown in this standard are valid. All standards will be revised. When using this standard, the latest versions of the following standards should be used. GB/T6U1-1938 Preparation of standard titration solution for chemical test titration analysis (content analysis) GB/T93-19 Preparation of preparations and products used in chemical reagent test GB/T1634-1995 Acceptance plan for product coating GH/11605--1979 (1989) Product packaging sampling: GB3795--1999 Pesticide packaging standard
3 Requirements
3.1 Appearance: white powder.
3.2 The composition of triethylamine technical pesticide shall meet the requirements of Table 1.
National Economic and Trade Commission 2002-1-24 approved 2002-07-01 implementation
[Huanchengyue
Yarongdong to request inspection of the city
4 Let the riding method
4.1 Sampling
TIG3296-2001
Table 1 Triethylhexanoic acid original drug preparation index
Combined storage product
Method (E/16u5199G\Original inspection group" force method: Use a random number table to determine the sampling of packaging, the final sample single ratio is not less than 200.
4. 2.2 Test Procedures 4.2.1 Commercial Chromatography Using a liquid chromatograph with a neutral conductivity detector and an ion exchanger, under the same chromatographic conditions, the retention time of a peak in the sample and the retention time of an acetic acid peak in the standard liquid are within 1.5 relative values. Operating Conditions: Sample: a 100 mL column containing approximately 1% acetic acid, in a narrow base flask, add 20 mL of water, and sonicate for 3 h. Cool to room temperature, use flow and phase. Before analysis, use 3.2m filter to filter, standard solution: weigh 0.18+100ml of lead monoacetate, other solutions are the same as the test details: 0.1425NHC, 9.18uCO1T.
Liquid chromatograph: equipped with ion exchange chromatographic hanger and electronic controller: chromatographic column: StarmA800um195mmx4.stmi.d, equipped with pre-supersonic water bath.
Control line energy: o.2m i.
Clean, J3mL/min
Temperature; room overflow.
Phase preparation: Inhibition or chemical inhibition method [e (HS) = 0.U25mol/, sulfuric acid inhibition at a flow rate of 4ml/mi] injection. 101..
Maintain time S
4.2.2 Infrared spectroscopy
Prepare the sample and standard sample and KHr pressure respectively (acetic acid sample or standard sample 1mg and KHr 8mmg), scan from 000-430 Scan the compressed film, and the infrared spectrum of the sample should not show obvious differences (see Figure 1). 4.3 Determination of triethyl aluminum content 4.3.1 Method summary HG3296-2001 Figure 1 Infrared spectrum of triethyl aluminum 7-hydroxy-1-nitropropene is heated in a hydrogen peroxide solution and decomposed. The resulting salt is oxidized and the excess sulfhydryl reacts to form a volatile organic compound, C,H,A1O.P: rEOH
+3ITP(-+3C,H,OH+AF+
HPO+1H
+HP0-+21
4. 3.2 Reagents and solvents
Potassium iodide.
Acidity: 805%.
+H,S0= mol/L
Sulfuric acid quotient:
Hydrogen hydration solution: c(NeOH>一1mol/l. Oxidation solution N 2 H)=.1c/
Iodine standard solution:
+S(%-+21
12)=0.1mol/L..Prepare according to GB/T6u=. Standard solution of cable acid: c(N%u)-0.1mol/L, prepared according to (B/T61). Energy aging indicator: 1g/L, 1g/L starch indicator, 1.5R/L (freshly prepared), prepared according to GB/T603. Differential flushing solution. FH=7.3=U.2. Weigh 10μ sodium hydroxide (accurate to 0.000) 2g) in 1.8L water and neutralize to nH8 with iodine. After cooling to room temperature, add acid to H7.3-.2. Add 20ml of standard solution with water and dilute to 2L, store in a dark room. Before use, add sodium cyclosulfate standard titration until the solution is slightly yellow.
4.3.3 Only the electric clearing instrument with a locking electrode.
Supermarket wave water edge
pII meter.
Waterproof material.
Adjustable electric heating jacket: 1200w,
Spherical condensation,
Body plate: 25omL tool:
Dissipation tube: 25tnJ. Brown,
4.3.4 Test step ticket
4. 3.4. 1 Sample flow reduction
HE 32962001
Weigh the aluminum-containing 3-aldehyde sample (with a concentration of 0.000), put it into a volumetric flask, add 200ml of oxygen, and place it in a supernatant for 1 minute. Control the temperature to 1:1: add sodium hydroxide to make up to volume and mix well. Use liquid to transfer the sample to a 1/4 flask, add 4% chlorine ion solution, connect it to a reflux condenser, and evaporate for 1 minute. Rinse the condenser with a small amount of water, cool it to room temperature, neutralize it with thialdehyde solution, add 2% phenol indicator, and continue dripping until the red color disappears.
4. 3. 4.2. Transfer the tubes to the deep dripping tubes and add 20 ml of standard solution. Seal the tubes with water and place them in a dark place. Add 3 mL of acetic acid to acidify the tubes. When the end point is close to the end point, add 3 mL of liquid powder and continue to titrate until the color disappears. The end point can be determined by a potentiometric titrator. 4.3.4.3 Determination of tt||Under the condition of scanning, replace the sample with 10% hydrogen peroxide and perform the same determination on the other samples. 4.3.5 Calculation of the mass fraction of tt|| in the sample: (%): Calculate according to formula (1): X, sVmXx2.09 02 x100 9
c(VV) x295-1
m10/505
Wherein: V·-the volume of sodium thiosulfate standard titration solution consumed in the titration, mL; -the actual concentration of sodium thiosulfate standard titration solution, mal/lt;
the mass of the sample: 8:
-with 1.uL sodium thiosulfate standard titration solution NS-1.Kmt/L! half 4.3.6 Allowable difference between the results of two parallel determinations shall not exceed 1%. The arithmetic half mean shall be taken as the determination result. 4.4 Determination of phosphite 4.4.1 The storage method shall be the same as that of iodine oxidation. 4.4.2 Test in a new fall tank shall be the same as that of 4.3.2. 4.4.3 Night apparatus) 4.3.3.
4.4.4.1 Sample preparation
The sample with the maximum concentration of 0.8% (correct to 0%) should be placed in 1% water at 1°C, stirred for 1 hour, and placed in supernatant water with a concentration of 10 ml of sodium hydroxide (A) at a level of about 5 l under colorimeter control until the concentration of hydrogen is estimated to be 7. 510.2 (a small amount of about me chemical sodium certificate. An impact determination!, use water transfer car and dense 2Cm1. Change the bottle user. 4.4.4.2 Special determination
return 4.3.4.2.
4.4.4.3 room self determination
J [G3296—2001
Under the same conditions, replace the sample liquid with 0mL water, implement the same sample 4.3.4.2.44.5 etc.
academic light salt (with the acidity of the mass fraction X. (%). Calculate V-Vx0.n52 according to the formula ()
Formula:
The volume of the standard titration potential consumed by the titration sample, ml-the volume of the standard sodium thiosulfate consumed by the titration sample, L: The actual concentration of the standard drop of sodium thiosulfate, (?)
The standard titration value of 1.00mL of thiosulfate expressed in grams (N, S, 0) = 1.U00o1/L 4. 5 Determination of olefin reduction
4. 5. 1 Apparatus
Quick box: 1
Additional volume, diameter m, height mm
Flat beam apparatus
4. 5. 2. Test steps Www.bzxZ.net
Weigh the pan and bake at (100+1)°C for 1h (accurate to 0.02°C), put in 5°C sample and weigh the air to 300°C (accurate to 0.300°C). Spread the sample into a thin layer and put it in the oven without adding any heat. Cool to 7°C at 101±1°C. Measure and check if the temperature reaches 0.2°C.
4. 5. 3 Calculation
The decomposition amount of the sample expressed as a fraction of the amount of light, X, <%", is calculated according to formula (3):-
Where:
Sample flow quality · E1
Test bottle use benefit · more:
Sample is the same as the quality inspection of the bureau version,:
The purity of the two parallel measurements should not be less than 15%, and the arithmetic mean value is taken as the full result. 4.6 Product inspection and acceptance
The inspection and acceptance of the product shall comply with the provisions of (Normal/T104), and the limit value shall be processed by the rounded value comparison method. 5 Marking, labeling, packaging, storage
5.1-. The marking, labeling, packaging and filling of the copper raw material shall be It should comply with the provisions of GB3735. (3)
5.2 The packaging of aluminum triethyl ester should be made of PVC iron drum with a dry inner seal. The aluminum triethyl ester content in each iron drum should not exceed 0%. It can also be packed in a double-layer plastic bag with a propylene outer layer and a high-pressure ethylene inner layer. The aluminum triethyl ester content in each bag should not exceed 55k. The aluminum triethyl ester content in the small package and plastic pad should not exceed 1.
5.3 According to user requirements or design agreements, other types of packaging can be used, but they must comply with the provisions of GB379G. 5.4 The packaging should be placed in a ventilated and dry warehouse. 3296—2001
5.5 During transportation, keep the product away from moisture, rain and moisture, keep the room well ventilated, do not mix with food, seeds and products, and avoid contact with skin. Use a nose spray before use
5.6 This product is an organic systemic killer, which is mild to humans and plants, and safe to plants. It is non-irritating and non-corrosive to skin and skin. Generally, no poisoning accidents occur. If poisoning occurs, go to the hospital for examination and treatment in time. Use this product with caution. Wear protective gloves, masks and clean protective belts. Wash with soap and water after use. 523 Calculation
The decomposition amount of the sample expressed as a fraction of the amount of light, X, <%", is calculated according to formula (3):-
Where:
Sample flow quality · E1
Test bottle use benefit · more:
Sample is the same as the quality inspection of the bureau version,:
The purity of the two parallel measurements should not be less than 15%, and the arithmetic mean value is taken as the full result. 4.6 Product inspection and acceptance
The inspection and acceptance of the product shall comply with the provisions of (Normal/T104), and the limit value shall be processed by the rounded value comparison method. 5 Marking, labeling, packaging, storage
5.1-. The marking, labeling, packaging and filling of the copper raw material shall be It should comply with the provisions of GB3735. (3)
5.2 The packaging of aluminum triethyl ester should be made of PVC iron drum with a dry inner seal. The aluminum triethyl ester content in each iron drum should not exceed 0%. It can also be packed in a double-layer plastic bag with a propylene outer layer and a high-pressure ethylene inner layer. The aluminum triethyl ester content in each bag should not exceed 55k. The aluminum triethyl ester content in the small package and plastic pad should not exceed 1.
5.3 According to user requirements or design agreements, other types of packaging can be used, but they must comply with the provisions of GB379G. 5.4 The packaging should be placed in a ventilated and dry warehouse. 3296—2001
5.5 During transportation, keep the product away from moisture, rain and moisture, keep the room well ventilated, do not mix with food, seeds and products, and avoid contact with skin. Use a nose spray before use
5.6 This product is an organic systemic killer, which is mild to humans and plants, and safe to plants. It is non-irritating and non-corrosive to skin and skin. Generally, no poisoning accidents occur. If poisoning occurs, go to the hospital for examination and treatment in time. Use this product with caution. Wear protective gloves, masks, and clean protective belts. Wash with soap and water after use. 523 Calculation
The decomposition amount of the sample expressed as a fraction of the amount of light, X, <%", is calculated according to formula (3):-
Where:
Sample flow quality · E1
Test bottle use benefit · more:
Sample is the same as the quality inspection of the bureau version,:
The purity of the two parallel measurements should not be less than 15%, and the arithmetic mean value is taken as the full result. 4.6 Product inspection and acceptance
The inspection and acceptance of the product shall comply with the provisions of (Normal/T104), and the limit value shall be processed by the rounded value comparison method. 5 Marking, labeling, packaging, storage
5.1-. The marking, labeling, packaging and filling of the copper raw material shall be It should comply with the provisions of GB3735. (3)
5.2 The packaging of aluminum triethyl ester should be made of PVC iron drum with a dry inner seal. The aluminum triethyl ester content in each iron drum should not exceed 0%. It can also be packed in a double-layer plastic bag with a propylene outer layer and a high-pressure ethylene inner layer. The aluminum triethyl ester content in each bag should not exceed 55k. The aluminum triethyl ester content in the small package and plastic pad should not exceed 1.
5.3 According to user requirements or design agreements, other types of packaging can be used, but they must comply with the provisions of GB379G. 5.4 The packaging should be placed in a ventilated and dry warehouse. 3296—2001
5.5 During transportation, keep the product away from moisture, rain and moisture, keep the room well ventilated, do not mix with food, seeds and products, and avoid contact with skin. Use a nose spray before use
5.6 This product is an organic systemic killer, which is mild to humans and plants, and safe to plants. It is non-irritating and non-corrosive to skin and skin. Generally, no poisoning accidents occur. If poisoning occurs, go to the hospital for examination and treatment in time. Use this product with caution. Wear protective gloves, masks, and clean protective belts. Wash with soap and water after use. 52
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