Some standard content:
GB5452—2001
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. Introduction
This standard is a revised version of the mandatory national standard GB 5452—1985 56% aluminum phosphide tablets. The main differences between this standard and GB5452—1985 56% aluminum phosphide tablets are: 1. Add two control specifications of (2.5±0.1)g and (0.6±0.03)g per tablet in Section 3.2. 2 In the chapter "Test Methods", the test method reduces the amount of reagents and liquid used and the amount of sample weighing. 35.2 In the tinplate cylinder with a layer of plastic bag inside the packaging, put a bag of adsorbent in each cylinder (aluminum bottle is optional) and test it. This standard is recommended to replace GB5452-1985 from the date of implementation. This standard is proposed by the State Petroleum and Chemical Industry Bureau. This standard is under the jurisdiction of the National Pesticide Standardization Technical Committee. The responsible drafting unit of this standard is: Shuoyang Chemical Research Institute. The participating drafting units of this standard are Jiangsu Shuangling Chemical Group Co., Ltd. Co., Ltd., Jining Chemical Experimental Plant, Shenyang Pesticide Factory, Anhui Ningguo Pesticide Chemical General Factory, Jining Yimin Chemical Factory. The main drafters of this standard are: Zhang Pilong, Ti Yankun, Zhou Shisheng, Wei Luyuan, Cheng Jinlong, Yue Xianping. This standard was first issued on October 4, 1985. This standard is the first revision.
This standard is entrusted to the Secretariat of the National Pesticide Standardization Technical Committee for interpretation. National Standard of the People's Republic of China
56% Aluminum phosphide tablets
56% Aluminum phosphidetablets Other names, structures and basic physical and chemical parameters of the active ingredient aluminum phosphide of this product are as follows: ISO common name: Aluminium PhosphideCIPAC digital code 227
Chemical name, aluminum phosphide
Structural formula: AIP
Experimental formula: AIP
Relative molecular mass: 57.96 (according to the 1997 international relative atomic mass) Biological activity: insecticide
Melting point>1000℃
Vapor pressure is very small below 1000℃ and sublimates at 1100℃. GB5452—2001
Reputation GB5452-1985
Stability: Stable when dry, easy to absorb moisture and decompose, the released phosphine gas has a bad garlic or calcium carbide smell. It reacts violently with acid and explodes and catches fire when it comes into contact with aqua regia. It can spontaneously combust in humid air. 1 Specification
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of 56% aluminum phosphide tablets. This standard applies to 56% aluminum phosphide tablets pressed from aluminum phosphide technical and ammonium carbamate and other fillers that meet the standards. 2 Cited standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard was published, the versions shown were valid. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T 601—1988 Preparation of standard solutions for chemical reagent titration analysis (volume analysis) GB/T603—1988 Preparation of preparations and products used in chemical reagent test methods GB/T1604—1995 Acceptance rules for commercial pesticides GB/T1605—2001 Sampling methods for commercial pesticides CB3796—1999 General rules for pesticide packaging
3 Requirements
3.1 Appearance: gray-green or yellow-green round tablets. 3.256% aluminum phosphide tablets should meet the requirements of Table 1. Approved by the State Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on 20D1-09-04 Implementation on 2002-03-01
Mass fraction of aluminum phosphide/%
Mass of each tablet/g
Vertical strength/MPa
Powder and fragments/%
GB 5452-2001
Table 1 Control items of 56% aluminum phosphide tablets 3.2±0.1
Note: Fragments shall be regarded as those not exceeding 1/4 of the tablet mass. 4 Test method
4.1 Sampling
2.5±0.1
0.60±0.03
Perform according to 5.3.4 of GB/T1605-2001. The sampled packages are determined by the random number table method, and the final sample size should be no less than 600g.
4.2 Identification test
Weigh a small amount of sample into a beaker, add an appropriate amount of water, and then slowly add an excess of 40% sulfuric acid. Use silver nitrate test paper to contact the generated gas, and the filter paper will turn black. Heat to a slight boil until there are no bubbles, cool to room temperature, add 8g/L sodium hydroxide solution to adjust the pH value to about 12 and filter. Use 40% sulfuric acid solution to adjust the filter until a large amount of white precipitate is produced, then add alizarin-S, and the solution will turn into rose red. 4.3 Determination of aluminum phosphide content
4. 3.1 Summary of the method
Aluminum phosphide generates phosphine gas with acid, which is oxidized and absorbed with an excess of potassium permanganate solution, and then an excess of oxalic acid solution is added, and the oxalic acid is back-titrated with potassium permanganate solution. The reaction equation is as follows: AIP+3H-→+H,P + +A13 1
5H,P+8MnO, +9H+→5PO}-+8Mn*I +12H,02Mn0++5C,O-+16H+—2Mnz1+10CO.t+8H,04.3.2 Reagents and solutions
Potassium permanganate standard titration solution: c(—KMnO,)=0.5mol/L solution, prepared according to GB/T 601: Oxalic acid standard solution: c(
H,C0,)=0.5mol/L bath solution, prepared according to GB/T601, sulfuric acid solution: w(H,SO)=40%, prepared according to GB/T603. 4.3.3 Instruments
Electric oscillator: international type, 100 times/min 4.3.4 Determination steps
Pour out all the extracted samples, mix gently, and quickly select about 100 samples by quartering method, and put them into plastic bags. Smash the samples to a particle size of no more than 3mm, transfer them into a 250mL ground-mouth bottle, and mix them. Select about 10g of the sample, put it in a mortar and grind it quickly, and put it into a ground-mouth bottle. Use a weighing bottle to quickly weigh 0.14g~0.16g (accurate to 0.0002g) of the sample, and place it in a 500ml conical flask with a ground-mouth stopper that has been accurately added with 50mL of potassium permanganate standard titration solution. Add 25mL of sulfuric acid solution, immediately seal it tightly, put it on a shaker, shake it for 25min, remove the bottle, accurately add 30mL of oxalic acid standard solution until the purple color disappears, and immediately titrate the excess oxalic acid with potassium permanganate standard titration solution. Heat to 70℃ when it is close to the point, and continue titrating until it turns slightly red, which is the end point. Residue and blank determination: Under opposite conditions, quickly weigh 0.14E~0.16g (accurate to 0.0002g) of finely ground aluminum phosphide, place it in a 200mL beaker, add 5ml of water in a fume hood, and then slowly add 25mL of sulfuric acid solution. Stir until no bubbles occur, heat to a slight boil (2~3) minutes, take out and cool, and transfer all to a 500mL conical flask with a ground stopper that has been accurately added with 50mL of potassium permanganate standard titration solution in advance. Other operations are the same as the sample determination, and 60mL of oxalic acid standard solution is accurately added. 4.3.5 Calculation
GB 5452—2001
The mass fraction X(%) of aluminum phosphide in the sample is calculated according to formula (1): X, =
Where: c
(eVi-eV- V, -eV4
X0.007244X100
-The actual concentration of potassium permanganate standard titration solution: mol/L: The actual concentration of oxalic acid standard solution, mol/L; The total volume of potassium permanganate standard titration solution added and consumed in titration when measuring the sample, InL; V,---The volume of oxalic acid standard solution added and consumed in titration of the sample, mL; V
The total volume of potassium permanganate solution added and consumed in titration of the residue and blank, mL! V,--The volume of oxalic acid solution added in titration of the residue and blank, mL; mt--Sample mass, g,
Residue and blank sample mass, g:
-With 1.00mL potassium permanganate standard titration solution [c00. 007 244 -
Mass of aluminum.
4.3.6 Allowable errorbZxz.net
KMnO,)=1.000 mgl/L1 equivalent in grams. The difference between the results of two parallel determinations shall not exceed 0.8%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of the mass of each piece
4.4.1 Instrument
Industrial balance, sensitivity 0.01g.
4. 4.2 Determination steps
Take 10 pieces of the sample at random and weigh them (accurate to 0. 01 g). 4.4.3 Calculate the mass X of each sample according to formula (2): X = 10
Where: m—mass of 10 samples, g;
10—number of samples.
4.5 Determination of vertical strength
4.5. 1 Instrument
Strength tester: accuracy 0.1N.
4.5. 2 Determination steps
Take 10 samples and use the strength tester to test the vertical pressure value of each lead phosphide tablet at room temperature, and then add them up (F). 4.5. 3 Calculate the vertical strength X of the sample: Calculate X according to formula (3): -
Where: F—the sum of the pressures borne by 10 samples, MPa: 10—number of samples.
4.6 Determination of powder and fragments
4.6.1 Instrument
Industrial balance
4. 6.2 Determination steps
Open the packaging can from which the sample was extracted, collect all the powder and fragments, and weigh them (accurate to 0.01g). (3)
4.6.3 Calculation
GB5452—2001
The powder and fragments in the sample expressed as mass fraction X. (%) is calculated according to formula (4): X-×100
Where: m1Mass of powder and fragments?gi
m2—Mass of aluminum phosphide sample in each packaging can. 4.7 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604, and the rounded value comparison method shall be used for limit value processing. 5 Safety
.. (4)
5.1 Aluminum phosphide is a highly toxic insecticide. It decomposes when it absorbs moisture or comes into contact with water. The released phosphine gas is extremely toxic to humans. When the phosphine gas content in the air reaches 0.14MR/L., it will cause breathing difficulties and even death. The explosion limit of phosphine gas is (26.1~27.1)MR/L. 5.2 Phosphine mainly damages the nervous system, heart and liver of the human body. Acute poisoning symptoms: Mildly poisoned patients have headaches, fatigue, nausea, insomnia, dry mouth, dry nasopharynx, chest tightness, cough and low fever. Moderately poisoned patients have mild consciousness disorders, breathing difficulties and myocardial damage. Severe poisoning will cause pulmonary edema, myocardial, liver and kidney damage. 5.3 The spraying personnel must undergo strict training and wear gas masks, protective clothing and protective gloves during the spraying process. The opening and inspection should be carried out in a fume hood away from people. Smoking, eating and drinking are prohibited at the work site. 5.4 In case of poisoning, leave the site quickly to a place with fresh air, keep breathing unobstructed, give oxygen in case of breathing difficulties and send to hospital for treatment quickly.
5.5 In case of fire, foam and carbon dioxide fire extinguishing agents should be used. It is prohibited to use fire extinguishing agents containing water. 6 Marking, labeling, packaging and transportation
6.156% aluminum phosphide tablets are Class 1 dangerous goods. Their marking, labeling, packaging and storage should comply with the provisions of GB3796. 6.2 The boxes and cylinders should be marked with "heat-resistant", "fireproof" and "flammable when wet". 6.3 56% aluminum phosphide tablets are packed in completely sealed tinplate cylinders with threaded covers and aluminum cylinders. The net weight of each cylinder is 16g, 32g, 250B500g, 1.0kg and 1.5kg. For cylinders below 100g, completely sealed threaded hard ester plastic cylinders can also be used. The outer packaging is made of moisture-proof and flame-retardant cartons, calcium plastic boxes, etc., and the middle is padded with shock-absorbing materials. The net weight of each box does not exceed 20kg. Each packaging unit and each tablet weight are clearly marked with
6.4 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 6.5 Packages should be stored in ventilated and dry warehouses, away from fire and heat sources. 6.6 During storage and transportation, prevent moisture and sun exposure, ensure good ventilation, keep away from fire sources, and do not mix with food, seeds and materials, avoid contact with skin, and prevent inhalation through the mouth and nose.
6.7 Under the specified storage and transportation conditions, the warranty period of 56% aluminum phosphide tablets is 2 years from the date of production.
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.