Some standard content:
Chemical Industry Standard of the People's Republic of China
Subject Content and Applicable Scope
HG/T 2689
Replaces HG2-5291967
The small standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation, storage, etc. of cresol phosphate. This standard applies to tricresyl phosphate obtained by reacting cresol with phosphorus dichloride or "chlorophosphorus", then nitrogenating and hydrolyzing it, and vacuuming it. This product mainly uses plasticizers such as butyl polyvinyl chloride and nitrocellulose. Molecular formula: (CH, CH, O), PO
Relative molecular weight: 368.37 (International relative atomic mass in 1991) 2 Reference standards
GB/T 501
GB/T 603
GB/T 1250
GB/T 1664
GB/T 1669
:GB/T 1671
G3/T [672
GB/T3723
GB/T 4472
GB/T 6678
GB/T 6682
3 Technical requirements
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents Preparation of preparations and products used in test methods for chemical reagents Methods of expressing and determining limit values Determination of the appearance color of plasticizers (platinum-cobalt colorimetry) Determination of heating loss of plasticizers
Determination of the flash point of plasticizers
Cleveland open cup method
Determination of the volume resistivity of plasticizers
Safety information for samples of industrial chemical products General rules for determination of density and relative density of chemical products General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories 3. 1 Appearance: Yellow transparent oily liquid. 3.2 Cresyl phosphate shall meet the requirements of the following table: Item
Chroma (platinum-cobalt), No.
Density (o), g/cma
Acidity (calculated as phosphoric acid), not reduced by heating, %
Free phenol (calculated as phenol), %
Product resistivity.n·cm
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995, etc.
Qualified products
Implemented on January 1, 1996
Test method
HG/T 2689—1995
The reagents used in this test method are all analytically pure reagents. Water should comply with the third-grade water specified in GB/T6682. Unless otherwise specified, the standard titration solutions and preparations used in this test method are prepared in accordance with GB/T601 and GB/T603: General laboratory instruments are used when no instrument requirements are specified.
4.1 Determination of chromaticity
Perform in accordance with GB/T 1664.
4.2 Determination of density
Perform in accordance with 2.3.2 Wei's balance method in GB/T4472: 4. 3 Determination of acidity
4. 3.1 Reagents and solutions
4.3.1.195 Ethanol (GB/T679).
4.3.1.2 Sodium hydroxide (GB/T 629) standard titration solution: r(NaOH)—0.1 mol/L4.3.1.3 Phenol red indicator (0.2 g/L): Take 50 Img of phenol red and mix it with 2.85 ml. 2g/L sodium hydroxide solution and 5 mL of 95% ethanol. After warming, dilute it to 250 mL with 20% ethanol. 4.3.2 Test steps
Take 12.5 ml of 95% ethanol, add 0.5 tmT of phenol red indicator solution, neutralize it with sodium hydroxide standard titration solution until it turns slightly pink, then add 25 g of the sample (accurate to (.5 g), and titrate it with sodium hydroxide standard titration solution until it turns slightly pink. Keep for 5 seconds. 4.3.3 Result calculationbZxz.net
The mass fraction (X1) of acidity (in terms of phosphoric acid) is calculated according to formula (1): XI+VX0. 019x
Wherein: .-actual concentration of sodium hydroxide standard titration solution, mal/IV—volume of sodium hydroxide standard titration solution consumed by titrating the sample, mL; sample mass, ;
0.049---mass of phosphoric acid in grams equivalent to 1.00ml sodium hydroxide standard titration solution Cc(NaOH)=1.000Iol/LJ.
4.4 Determination of heating loss
Weigh 10 g of sample (accurate to 0.0002g) and measure according to GB/T1669. 4.5 Determination of flash point
Carry out according to GB/T 1671.
4. 6 Determination of free phenol
4.6.1 Reagents and solutions
4. 6. 1. 1
4. 6. 1. 2
4. 6. 1. 3
Methyl chloride (GB/T682).
Hydrochloric acid (GB/T 622).
Sodium hydroxide (GB/T629) solution: 25\/1. 4. 6. 1. 4
Potassium iodide (GB/T1272) solution: 190g/L 4.6.1.5 Potassium bromide (GB/T649)-potassium bromate (GB3/T650) solution: dissolve 0.6 mol of potassium bromate and 3.0 mol of potassium bromate in water, and dilute to 1000mL with water
4.6.1.6 Sodium thiosulfate (GB/T637) standard titration solution: c(NaS,O:)=0.02mol/L, 4.6.1.7 Starch indicator solution: 2.5g/L.
4.6.2 Test steps
Preparation of test solution
HG/T2689--1995
Weigh 10g of the sample (accurate to 0.01g) into a 100ml volumetric flask, add 50.11L of caustic soda solution, shake for 3min, and dilute to the mark with water. Filter with wet filter paper and take the filtered clear liquid. 4.6.2.2 Determination
Absorb 50.6ml of the filtered clear liquid and put it into a 500ml iodine volumetric flask, add 20.0mL of potassium bromide-bromic acid solution, add 5ml of hydrochloric acid, immediately cover the bottle stopper and shake well, add water to the mouth of the iodine volumetric flask to seal it. Place it in a dark place and let it stand for 15min. Carefully remove the bottle, add 10mL of potassium iodide solution and rinse the bottle stopper and the inner wall of the bottle with water. If there is white precipitate, add 1 mL of chloroform and titrate with sodium thiosulfate standard titration solution. When it is close to the end point, add 2 mL of starch indicator solution. The end point is when the blue color disappears. At the same time, take 50 mL of water instead of the filtered clear liquid for a blank test. 4.6.3 Calculation of results
The mass content of free phenol (in terms of phenol) (X) is calculated according to formula (2) X c(Vl-Vox0.015 67×100
Wherein: VI—··The volume of sodium thiosulfate standard titration solution consumed in the blank test. IL; V: The volume of sodium thiosulfate standard titration solution consumed by the titration sample. mL; -The actual concentration of sodium thiosulfate standard titration solution, mol/L! Sample mass · +
0.015 67-
The mass of phenol in grams equivalent to 1.00 ml of sodium thiosulfate standard titration solution [c(NazS2U:—1.000 mal/L),
4.7 Determination of volume resistivity
According to GB/T 1672,
5 Inspection rules
5.1 Triphenyl phosphate should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all products of the manufacturer meet the requirements of the standard. Each batch of products leaving the factory should be accompanied by a quality certificate in a certain format. The content includes: manufacturer name, product name, grade, batch number, net weight, trademark and label number.
5.2 The user unit has the right to inspect the quality of the received triphenyl phosphate according to this standard to check whether its indicators meet the requirements of this standard.
5.3 The net weight of the product to be approved shall not exceed 8 t. 5.4 Sampling method
Sampling must comply with the requirements of GB/T3723. The number of samples shall be in accordance with the provisions of GB/T6678 Table (2). When sampling, use a dry glass sampling tube. Sampling is evenly carried out on the upper, middle and lower parts of the packaging container. The sample volume of each sample shall not be less than 50ml, and the total volume shall not be less than 800ml. The samples shall be placed in two clean, dry bottles with ground stoppers. Labels shall be affixed and the following shall be marked: manufacturer name, product name, batch number, etc. One bottle shall be inspected by the inspection department, and the other bottle shall be sealed and kept for future reference. 5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling shall be carried out from twice the number of samples: If even one of the indicators in the inspection results does not meet the requirements of this standard, the entire batch of products shall be deemed unqualified. 5.6 When the supply and demand parties have objections to the product quality.Handle in accordance with the provisions of the "Production Quality Law of the People's Republic of China". 5.7 The judgment of the inspection results shall be carried out in accordance with the rounded value comparison method in GT3/T 1250. 6 Marking, packaging, transportation, storage and safety 6.1 The packaging iron drum shall be painted with a firm mark, which includes: the name of the manufacturer, product name, grade, batch number, net weight and toxic substances, etc. 6.2 Each packaged product shall be accompanied by a factory certificate, which includes: the name of the manufacturer, product name, grade, batch number, net weight. Trademark, product quality indicators and this standard number. 367
HG/T 2689—1995
6.3 The product is packed in round iron drums with a standard weight of 200kg. The drums should be tight and leak-proof. 6.4 The product should be protected from sunlight and moisture during transportation. It should be handled with care. 6.5 The product should be stored in a ventilated, cool and dry warehouse, neatly arranged, and the height of the packaging should not exceed 2. 6.6 Under the specified storage and transportation conditions, the shelf life is 6 months. 6.7 If the product leaks out, it should be covered with sand for adsorption. If it comes into contact with the skin, it should be rinsed with plenty of water first, and then cleaned with ethanol.
Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shanxi Chemical Research Institute. This standard was drafted by "Hai Pengpu Chemical". The main drafters of this standard are Chen and Zheng Xulai. From the date of implementation of this standard, the standard HG2-5291967 "Tris-phosphate" issued by the Ministry of Chemical Industry of the People's Republic of China will be invalidated.
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