Some standard content:
Chemical Industry Standard of the People's Republic of China
Triphenyl phosphate
1 Subject content and scope of application
HG/T 2688—1995
Replaces HC2-528—1.983
This standard specifies the technical requirements, test methods, inspection rules and markings, packaging, transportation, storage, etc. of triphenyl phosphate. This standard applies to triphenyl phosphate obtained by chlorination and hydrolysis of phenol and blue phosphorus chloride and vacuum distillation. This product is mainly used as a plasticizer for cellulose acetate, nitrocellulose, viscose cellulose and plastics or a flame retardant for insulating materials. Molecular formula: (CH,O),PO)
Relative molecular mass: 326.29 (according to the international relative atomic mass in 1991) 2 Reference standards
GB/T 601
Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T 603
GB/T 618
GB/T 1250
GB/T 1664
GB/T 1670
GB/T 3723
Preparation of preparations and products used in test methods for chemical reagents General method for determination of crystallization point of chemical reagents
Expression and determination method of limit values Determination of appearance color of additives (platinum-cobalt colorimetry) Thermal stability test of plasticizers
General safety rules for sampling of chemical products for Jiangye General rules for sampling of chemical products
GB/T 6678
CB/T6682
3 Technical requirements
Specifications and test methods for water used in analytical laboratories 3.1 Appearance: White crystalline powder or flakes. 3.2 Triphenyl phosphate shall meet the requirements of the following table:
Chroma (platinum-cobalt), No.
Chroma after thermal treatment (platinum-), No.
Crystallization point, ℃
Acidity (calculated as phosphoric acid), §
Free phenol (calculated as phenol), %
Water-soluble impurities
Chloride
Sulfate
Phosphate
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 360
Superior product
First-class product
Qualified product
Implemented on January 1, 1996
4 Test method
HG/T 2688—1995
The reagents used in this test method are all analytically pure reagents. Water should comply with the blue grade water in G3/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. When the instrument is not specified, it is a general experimental instrument. 4.1 Determination of chromaticity
4.1.1 Reagents and solutions
Acetone (GB/T 686).
4.1.2 Test steps
Weigh 28g of the sample (accurate to 0.5 brightness), dissolve it in 28mL of acetone, and proceed according to the provisions of GB/T1664. 4.2 Determination of chromaticity after heat treatment
4.2.1 Reagents and solutions
Acetone (GB/T686).
4.2.2 Test steps
Weigh 28g of sample (accurate to 0.5g), and perform the test according to GB/T1670. Keep the test chamber at 180℃±2℃ for 15min. Take out the heating tube containing the sample and let it cool in the air. The cooling temperature is above the crystallization point, and then dilute it with acetone to 50ml-. Perform the test according to GB/T1664.
4.3 Determination of crystallization point
Perform the test according to GB/1618.
4.4 Determination of acidity
4.4.1 Reagents and solutions
4.4.1.1 95% ethanol (GB/T 679)4.4.1.2 Sodium hydroxide (GB/T629) standard titration solution: c(Na0H)=0.1nul/L. 4.4.1.3 Phenol red indicator solution (0.2 g/L): Take 50 mg of phenol red, 2.85 mL of 0.05 mol/L sodium cyanide solution and 5 mL of 95% ethanol. Warm it up. Then add 5 mL of 95% ethanol and dilute it to 250 mL with water. 4.4.2 Test steps
Take 50 mL of 95% ethanol, add 0.5 mL of phenol red indicator solution and neutralize it with sodium cyanide standard titration solution until it turns slightly pink. Then add 25 g of the sample (accurately 0.5 g) and titrate it with sodium oxychloride standard titration solution until it turns slightly pink and keeps for 5 minutes. 5.4.4.3 Calculation of results
The acidity (in terms of phosphoric acid) fraction (X,) is calculated according to formula (1): X,=cVX0.049×100
The actual concentration of the standard titration solution of sodium fluoride, mol/L; I:
The volume of the standard titration solution of sodium hydroxide consumed by the titration sample, mL.: m
The mass of the sample, g;
The mass of phosphoric acid in grams equivalent to 1.00ml of the standard titration solution of sodium hydroxide [c(NaOH)=1.000mol/1].
4.5 Determination of free phenol
4.5.1 Principle
Phenol reacts with nitrous acid in the presence of sulfuric acid to form a nitroso compound. When treated with ammonia-ethanol solution, the color of the compound undergoes interconversion to form an aldehyde compound, which is determined by spectrophotometry. 4.5.2 Instruments
Spectrophotometer.
4.5.3 Reagents and solutions
1IG/T 2688—1995
4.5.3.11.2-Chloroethane (HG/T31117). 4.5.3.2 98% sulfuric acid (GB/T 625)
4.5.3.3 Glacial acid (GB/T 676).
4.5.3.4 Acetic acid grade solution: Mix 150mL of 100mol/L potassium hydroxide solution and 800ml of glacial acetic acid, and dilute with water to 1000ml.
4.5.3.5 Hydrogenated ethanol solution: Mix 450mL of 75% ethanol and 120mL of 25% ammonia paint solution. Then add 130mL of water. 4.5.3.6 Sodium nitrite (B633): Saturated solution. Sodium hydroxide standard titration solution: c(NaOH)=0.1mol/L.4. 5. 3.7
4.5.3.8 Phenol standard solution:
Accurately weigh 1.00g of phenol and dissolve it in water, then dilute it with water to 100ml., shake well, this solution contains 1mg of phenol in 1mL. This solution is solution A.
Take 10.0mlL of solution A and dilute it with water to 10)ml.. This solution contains 0.1mg of phenol in 1mL. This solution is bath solution R (this solution is valid for the day
4.5.3.9], Preparation of 2-dichloroethane: In a separatory funnel, use 0.1mol/L sodium hydroxide Wash 1,2-dichloroethane with solution (add 0.1mnl/l. sodium hydroxide solution 5ml. for every 10mL 1,2-dichloroethane), then separate the lower solvent layer, wash it once with water in the same ratio, separate the lower 1,2-dichloroethane for later use. 4.5.4 Experimental stepswww.bzxz.net
4.5.4.1 Drawing of standard curve
In each 50ml volumetric flask, add 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL) of phenol standard solution B, which is equivalent to 0.1 butylphenol content. mg, 0.2mg+0.3tg, 0.4ng, 0.5ng, then add 0.5mL of glacial acetic acid, 10mL of acetic acid buffer solution and 0.2mL of sodium nitrate solution, and mix well. Then add 0.3ml of concentrated sulfuric acid. After mixing, let it stand for 30 minutes, place the volumetric flask in an ice-water bath, cool it to 3°C, and slowly add ammonia-ethanol solution while rubbing until the liquid level just reaches below the scale. After 10 minutes, take it out of the ice-water bath, wait until it reaches room temperature, and dilute it to the scale with ammonia-ethanol solution. Determine the absorbance according to the following steps: select 10mm colorimetric blood, at a wavelength of 420nm, use water as a reference, and then perform absorbance determination of the standard color, with phenol content as the horizontal coordinate and the corresponding absorbance as the vertical coordinate, and draw a standard curve. 4.5.4.2 Determination
Put 10mL of washed 1,2-dichloroethane into a 100mL separatory funnel, add 1.0g of sample and shake to dissolve, then add 10ml of 1mol/l sodium hydroxide solution, stir thoroughly for 1 til, after separation, transfer the upper aqueous phase into a 50mL volumetric flask, then add 0.5ml of glacial acetic acid, 10ml of acetic acid buffer solution and 0.2ml of sodium nitrite solution, mix well, and then add 0.3mL, shake and let stand for 30min, cool the volumetric flask in an ice-water bath to 5℃, slowly add ammonia-ethanol solution while stirring until the liquid level just reaches the scale line, remove from the ice-water bath after 10min, warm to room temperature, and dilute to the scale with ammonia-ethanol solution. Synchronize with the above standard curve preparation, the wavelength is 42)nm, and water is used as a reference to measure the absorbance of the test solution. 4.5.4.3 Result expression
According to the absorbance of the sample, the phenol content is found on the standard curve. The free acid (in terms of phenol) content (X2) in the sample is calculated according to (2):
X2-mz×10-1
Where: m2 phenol mass in the test solution.mg:
ms—sample mass.
4.6 Determination of water-soluble impurities
4.6.1 Reagents and solutions
4.6.1.1 Hydrochloric acid (GB/T 622).
4.6.1.2 Nitric acid (G1/T 626),
IIG/T 2688-1995
4.6.1.3 Silver nitrate (GB/T670) solution: 50 g/L,
IIG/T 2688-1995
4.6.1.4 Barium chloride (GB/T 652) solution: 100 g/L4.6.1.5 Nitric acid (G13/T 626) solution; 1|2.4.6.1.6 Ammonium chloride (GB/T 657) solution: dissolve 15 g of ammonium chloride in 200 mL of water and 100 mL of nitric acid solution and saturate with ammonium nitrate.
Hydrochloric acid (GB/T622) standard titration solution: (HCI)*0.001mol/L4.6. 1. 7
4.6.2 Test steps
4.6.2.1 Preparation of water-benzene extract
Weigh 25g of the sample (accurate to 0.1) and put it into a 250mL conical flask. Then add 50ml of 80℃ water. After the sample is dissolved, continue to shake for 1 tmil, cool to room temperature, and then filter with dry quantitative filter paper. Collect the filtrate for later use. 4.6.2.2 Determination of chloride
Standard preparation: In a test tube, add 9.0InL water and 1ml of 0.00lmol/1 hydrochloric acid solution, and add 2ml of nitric acid solution and 1mL of silver nitrate solution. Mix and let stand in the dark for 5 minutes. Preparation of sample: Pipette 19.0 mL of filtrate into a test tube, add 2 mL of nitric acid solution and 1 mL of silver nitrate solution, mix and let stand for 6 min in a dark place, the floating matter generated should be less than the standard. 4.6.2.3 Determination of sulfate
Pipette 10.0 mL of filtrate into a test tube, add 0.5 mL of hydrochloric acid, then add 1 mL of chlorinated solution, mix and let stand for 5 min, there should be no floating matter or precipitation.
4.6.2.4 Determination of phosphate
Pipette 1.00 mL of filtrate into a test tube, add 1 mL of nitric acid and 1 mL of ammonium chloride solution, heat to 70 ℃, there should be no floating matter or yellow precipitation generated.
5 Inspection rules
5.1 Triphenyl phosphine should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all products shipped meet the requirements of this standard. Each batch of Shanchang products shall be accompanied by a quality certificate in a certain format. The content shall include the manufacturer name, product name, grade, batch number, net weight, trademark and standard number.
5.2 The user has the right to inspect the quality of the triphenyl phosphate received in accordance with this standard to check whether its indicators meet the requirements of this standard.
5.3 The net weight of each batch of products shall not exceed 1 t. 5.4 The sampling method shall comply with the requirements of GB/T3723. The number of samples shall be in accordance with the provisions of Table (2) of GB/T6678. When sampling, a stainless steel sampling tube shall be quickly inserted into the upper, middle and lower parts of the packaging container to sample evenly. Each sample shall not be less than 50g. The total amount after mixing and shrinking shall not be less than 800g. They shall be placed in two clean and dry bottles with grinding stoppers. Bottle 1 shall be labeled and marked with: manufacturer name, product name, batch number, etc. Bottle 1 is for inspection by the inspection department: Bottle 2 is sealed and kept for future reference. 5.5 If any of the indicators in the test results do not meet the requirements of this standard, re-sampling should be carried out from twice the number of samples. If any of the indicators in the test results do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.7 The judgment of the test results shall be carried out in accordance with the rounded value comparison method of C:B/T1250. 6 Marking, packaging, transportation and storage
6.1 A firm mark shall be applied on the outer packaging, and its contents shall include: manufacturer name, product name, grade, batch number, net weight, etc. 6.2 Each packaged product is accompanied by a factory certificate, which includes: manufacturer name, product name, grade, batch number, net weight, trademark, quality indicators that meet the requirements of this standard, and the number of this standard. 363
HG/T2688—1995
6.3 The packaging bags of triphenyl phosphate shall not be less than 3 layers, the outer layer is white polypropylene woven bag, the middle layer is black polyethylene bag, and the inner layer is colorless polyethylene bag. After the product is packed, it shall be sealed separately to avoid moisture. The net weight of each bag is 25kg. 6.4 This product should be protected from sunlight and moisture during transportation. It should be loaded and unloaded gently during transportation. It is strictly forbidden to use iron hand hooks. 6.5 This product should be stored in a ventilated, cool and dry warehouse, and the packaging height shall not exceed 10. 6.6 Under the specified transportation conditions, the shelf life is 6 months. 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 Shanghai Zhangyong Chemical Plant, and the main drafters of this standard were Chen Yong and Zheng Xurong. From the date of implementation of this standard, the original standard HG2-528-1983 "Lanthate Phosphate" issued by the Ministry of Chemical Industry of the People's Republic of China will be invalidated.1 Triphenyl phosphate should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all products leaving the factory meet the requirements of this standard. Each batch of factory products should be accompanied by a quality certificate in a certain format. The content includes the manufacturer's name, product name, grade, batch number, net weight, trademark and standard number.
5.2 The user 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 each batch of products shall not exceed 1 t. 5.4 The sampling method shall comply with the requirements of GB/T3723. The number of samples shall be in accordance with the provisions of Table (2) of GB/T6678. When sampling, use a stainless steel sampling tube to quickly insert into the upper, middle and lower parts of the packaging container, and evenly sample. Each sample should be no less than 50g, and the total amount after mixing and shrinking should be no less than 800g. They should be placed in two clean and dry bottles with grinding stoppers. Bottle 1 should be labeled and marked with: manufacturer name, product name, batch number, etc. Bottle 1 is for inspection by the inspection department: one bottle should be sealed and kept for future reference. 5.5 If any index does not meet the requirements of this standard in the inspection results, re-sampling should be carried out from twice the number of sampling pieces. If any index does not meet the requirements of this standard in the inspection results, the entire batch of products shall be unqualified. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.7 The judgment of the inspection results shall be carried out according to the comparison method of rounded values in C:B/T1250. 6 Marking, packaging, transportation and storage
6.1 The outer packaging should be painted with a firm mark, which includes: manufacturer name, product name, grade, batch number, net weight, etc. 6.2 Each packaged product is accompanied by a factory certificate, which includes: manufacturer name, product name, grade, batch number, net weight, trademark, product quality meets the quality indicators required by this standard and the number of this standard. 363
HG/T2688—1995
6.3 The packaging bag of triphenyl phosphate shall not be less than 3 layers, the outer layer is a white polypropylene woven bag, the middle layer is a black polyethylene bag, and the inner layer is a colorless polyethylene bag. After the product is packed, it should be sealed separately to prevent moisture. The net weight of each bag is 25kg. 6.4 This product should be transported away from sunlight and moisture. It should be loaded and unloaded gently during transportation. It is strictly forbidden to use iron hand hooks. 6. 5 This product should be stored in a ventilated, cool and dry warehouse, and the packaging height should not exceed 10. 6.6 Under the specified operating conditions, the shelf life is 6 months. 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 the Shanxi Chemical Research Institute. This standard was drafted by Shanghai Zhangyong Chemical Plant, and the main drafters of this standard were Chen Yong and Zheng Xurong. From the date of implementation of this standard, the original standard HG2-528-1983 "Phosphate of Phosphate" issued by the Ministry of Chemical Industry of the People's Republic of China will be invalidated.1 Triphenyl phosphate should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all products leaving the factory meet the requirements of this standard. Each batch of factory products should be accompanied by a quality certificate in a certain format. The content includes the manufacturer's name, product name, grade, batch number, net weight, trademark and standard number.
5.2 The user 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 each batch of products shall not exceed 1 t. 5.4 The sampling method shall comply with the requirements of GB/T3723. The number of samples shall be in accordance with the provisions of Table (2) of GB/T6678. When sampling, use a stainless steel sampling tube to quickly insert it into the upper, middle and lower parts of the packaging container, and evenly sample. Each sample should be no less than 50g, and the total amount after mixing and shrinking should be no less than 800g. They should be placed in two clean and dry bottles with grinding stoppers. Bottle 1 should be labeled and marked with: manufacturer name, product name, batch number, etc. Bottle 1 is for inspection by the inspection department: one bottle should be sealed and kept for future reference. 5.5 If any index does not meet the requirements of this standard in the inspection results, re-sampling should be carried out from twice the number of sampling pieces. If any index does not meet the requirements of this standard in the inspection results, the entire batch of products shall be unqualified. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.7 The judgment of the inspection results shall be carried out according to the rounded value comparison method of C:B/T1250. 6 Marking, packaging, transportation and storage
6.1 The outer packaging should be painted with a firm mark, which includes: manufacturer name, product name, grade, batch number, net weight, etc. 6.2 Each packaged product is accompanied by a factory certificate, which includes: manufacturer name, product name, grade, batch number, net weight, trademark, product quality meets the quality indicators required by this standard and the number of this standard. 363
HG/T2688—1995
6.3 The packaging bag of triphenyl phosphate shall not be less than 3 layers, the outer layer is a white polypropylene woven bag, the middle layer is a black polyethylene bag, and the inner layer is a colorless polyethylene bag. After the product is packed, it should be sealed separately to prevent moisture. The net weight of each bag is 25kg. 6.4 This product should be transported away from sunlight and moisture. It should be loaded and unloaded gently during transportation. It is strictly forbidden to use iron hand hooks. 6. 5 This product should be stored in a ventilated, cool and dry warehouse, and the packaging height should not exceed 10. 6.6 Under the specified operating conditions, the shelf life is 6 months. 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 the Shanxi Chemical Research Institute. This standard was drafted by Shanghai Zhangyong Chemical Plant, and the main drafters of this standard were Chen Yong and Zheng Xurong. From the date of implementation of this standard, the original standard HG2-528-1983 "Phosphate of Phosphate" issued by the Ministry of Chemical Industry of the People's Republic of China will be invalidated.
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