HG/T 2076-1991 Phenylperisulfonic acid (1-phenylnaphthylamine-8-sulfonic acid)
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2076-91
Phenyl perisulfonic acid (1-phenylnaphthylamine-8-sulfonic acid) 1991-07-17 Issued
Ministry of Chemical Industry of the People's Republic of Chinawww.bzxz.net
1992-01-01 Implementation
Chemical Industry Standard of the People's Republic of China
Phenyl perisulfonic acid (1-phenylnaphthylamine-8-sulfonic acid) Subject content and scope of application
HG2076-91
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of phenyl perisulfonic acid. This standard applies to phenyl perisulfonic acid prepared from perisulfonic acid and aniline by aromatic amination. This product is used as a dye intermediate. Structural formula:
Molecular formula: Ci6HisNOsS
Relative molecular mass: 299.35 (according to the international relative atomic mass in 1987) 2 Reference standards
Chemical reagents
3 Technical requirements
The mass of phenylperiodic acid prepared by the standard solution for titration analysis (volumetric analysis) shall meet the requirements of the following table: %(m/m)
Phenylperiodic acid content (coupling value)
Periodic acid (1-naphthylamine-8-sulfonic acid) content (calculated as 100% of phenylperiodic acid) Ammonia insoluble matter content (calculated as 100% of phenylperiodic acid) Aniline content (calculated as 100% of phenylperiodic acid) 4 Test method
4.1 Determination of appearance
Visual determination method shall be adopted.
4.2 Determination of phenylperiodic acid content (coupling value) 4.2.1 Principle of the method
Superior grade
Green-brown to brown-green crystals
In a weakly acidic medium, phenylperiodic acid undergoes a quantitative coupling reaction with a standard solution of p-nitroaniline diazonium salt of known concentration. 4.2.2 Reagents and solutions
4.2.2.1 Hydrochloric acid (GB622) solution: chemically pure, 1+1 solution; approved by the Ministry of Chemical Industry of the People's Republic of China on July 17, 1991 and implemented on January 1, 1992
HG2076-91
4.2.2.2 Sodium hydroxide (GB629) solution: chemically pure, 500g/L solution; 4.2.2.3 Ammonia water (GB631): chemically pure; 4.2.2.4 Sodium nitrite (GB633) standard titration solution: chemically pure, c(NaNO2)=0.25 mol/L; 4.2.2.5 Sodium acetate (GB693) solution; chemically pure, 200g/solution, 4.2.2.6 30% acetic acid (HG3-1095): chemically pure; 4.2.2.7 Starch-potassium iodide test solution:
Weigh 0.5g starch (chemically pure), add 5mL water to make a paste, add the paste to 90mL boiling water under stirring, boil for 1-2min, cool, dilute to 1000mL, add 0.5g potassium iodide (GB1272), stir and dissolve for use (this solution is prepared before use, if turbidity is found, it should be re-prepared).
4.2.2.8 p-Nitroaniline standard solution: c(NO2CgH,NH)=0.2mol/L. Preparation:
Weigh 27.6g of p-nitroaniline into a 1000mL beaker, add 100mL of water to make a paste, add 180mL of hydrochloric acid, heat to dissolve, dilute to 1000mL with water, mix well, let stand overnight, filter and calibrate. Calibration:
Take 25mL of p-nitroaniline solution, place it in a 500mL beaker with 8~10mL of hydrochloric acid (4.2.2.1), cool to 0~9℃, add water cooled to 0~5℃, dilute to 100mL, then titrate with sodium nitrite standard titration solution (4.2.2.4) under stirring, insert the tip of the burette below the liquid surface, and when the titration is close to the end point of 1mL, lift the burette out of the liquid surface, and then add drop by drop, When the sample solution is titrated to the newly prepared starch-potassium iodide test solution (4.2.2.7) and turns slightly blue, repeat the test after 5 minutes. If it still turns slightly blue, it is the end point. At the same time, do a blank test.
Calculate:
Ci(V1-V2)
Where: ci——concentration of sodium nitrite standard titration solution, mol/L; C2—concentration of p-nitroaniline standard solution, mol/L; V—concentration of p-nitroaniline standard solution, mol/L Volume of quasi-solution, mL; V1——Volume of sodium nitrite standard solution consumed in titration, mL; V2 Volume of sodium nitrite standard titration solution consumed in blank titration, mL. 4.2.2.9 Standard titration solution of p-nitroaniline diazonium salt: c(NO2CcH,NH2)=0.04mol/L. Preparation:
Use a pipette to accurately pipette 50mL of p-nitroaniline standard solution (4.2.2.8) into a 250mL brown volumetric flask to which 30mL of hydrochloric acid (4.2.2.1) has been added, add about 20mL of 0-5℃ water, and under shaking, use a burette to quickly add the calculated amount of sodium nitrite standard titration solution (4.2.2.4) so that the solution shows a microscopic blue color when tested with starch-potassium iodide test solution (4.2.2.7), and after maintaining for 5 minutes, it still shows a microscopic blue color, then add 0.1mL of excess sodium nitrite standard titration solution, dilute to the mark with water, and then After that, place the solution in an ice bath, cool it, and set it aside. This standard solution can only be used for 4 hours. Calculation:
Wherein: c2——concentration of p-nitroaniline standard solution, mol/L; Cs—concentration of p-nitroaniline diazonium salt standard titration solution, mol/L. 4.2.3 Analysis steps
Weigh 3-4g of wet sample or 2g of dry sample (accurate to 0.0002g) in a 150mL beaker. Add 5m 1 L ammonia water (4.2.2.3) and 80 mL water to fully dissolve (slightly heat), transfer the solution into a 500 mL volumetric flask, dilute to scale with water, shake well and set aside. Use a pipette to draw 50.0 mL of the above sample solution into a 600 mL beaker, add 300 mL of water, add about 3 mL of acetic acid solution (4.2.2.6), acidify to pH 5-6, Then add 30mL of sodium acetate solution (4.2.2.5), and then titrate with p-nitroaniline diazonium salt standard titration solution (4.2.2.9) at 5~10℃ (the standard solution should be placed in a brown burette with an ice sleeve). When titrating, first add about 2mL less than the estimated amount of p-nitroaniline diazonium salt standard titration solution, and then slowly titrate until the infiltration circle on the filter paper and the 1+1 infiltration circle of p-nitroaniline diazonium salt standard titration solution are at the same level. After it turns slightly purple, add 12 mL of sodium hydroxide solution (4.2.2.2) to alkalize the sample solution under significant alkalinity and maintain for 5 minutes. Then acidify it with acetic acid to make the sample solution weakly acidic (pH=5-6). Then titrate it with p-nitroaniline diazonium salt standard titration solution. Repeat this process several times (about 3 times) until the purple color disappears at the junction of the seepage circle of the coupled sample drop on the filter paper and the seepage circle of the 1+1 p-nitroaniline diazonium salt standard titration solution. The percentage of phenyl peri-acid (a1) is calculated according to formula (3): 21 = :: X0.299 4x
m?50/500
Where:
Cs——concentration of p-nitroaniline diazonium salt standard titration solution, mol/L; Vs——volume of p-nitroaniline diazonium salt standard titration solution consumed, mL; m——mass of sample, g;
(3)
0.2994——mass of phenyl peri-acid equivalent to 1.00mL p-nitroaniline diazonium salt standard titration solution Lc(NO2CH,NH2)=1.000mol/L), expressed in grams. The difference between the results of two parallel determinations is not greater than 1%, and the arithmetic mean is taken as the determination result. 4.3 Determination of pericentric acid content
4.3.1 Instruments and materials
4.3.1.1 Chromatography cylinder; 20cmX20cm×20cm; 4.3.1.2 Micro syringe: 5uL;
4.3.1.3 UV analyzer: wavelength 254nm; 4.3.1.4 Chromatography paper, No. 1.
4.3.2 Reagents and solutions
4.3.2.1 Ammonia water (GB631): chemically pure 1+1 solution 4.3.2.2 n-Butanol (HG3-1012): chemically pure, 4.3.2.3 Developing solvent: n-Butanol is saturated with 1+1 ammonia water; 4.3.2.4 Refined product of perithionic acid: Take about 200g of dry perithionic acid (industrial product), put it in a 2000mL beaker, add 800mL of water, add ammonia water (4.3.2.1) and heat to dissolve until pH=8~9, and filter it while hot. Use 10% sulfuric acid to acidify the filtrate to pH-4, filter and wash with water twice, repeat the above method 3~4 times until no Laurentide spots are found on the chromatography paper with 2% perithionic acid solution. Place in an oven to dry for later use;
4.3.2.5 Peripheral acid standard solution: weigh the refined peripheral acid product calculated by 100% (4.3.2.4) 1g (accurate to 0.0001g), placed in a 150mL beaker, add 4mL ammonia water (4.3.2.1) and 50mL water to dissolve, transfer to a 250mL volumetric flask, dilute to scale with water and mix well. The concentration of this solution is 0.4% (m/m), stored at room temperature away from light, and the validity period is two weeks. 4.3.3 Preparation of standard color scale of hydroxyl acid
Put 2.50, 3.75, 5.00, and 6.25mL of the above standard solution (4.3.2.5) in four 100mL volumetric flasks, dilute to scale with water, shake well, and the concentrations are 0.01, 0.015, 0.02, and 0.025% (m/m) respectively. The standard color scale is valid for 7 days. 4.3.4 Analysis steps
Weigh 1g of phenylperiodic acid sample (accurate to 0.02g) calculated by folding into a 150mL beaker, add 4mL of ammonia water (4.3.2.1), dissolve in hot water, and then transfer to a 100mL volumetric flask and dilute to the scale. Take a 160mm×250mm chromatography paper (4.3.1.4), and draw three lines with a pencil at 1, 2, and 18cm from the bottom of the chromatography paper, namely, the immersion line, the spot line, and the front line. Use a pencil to make a point every 2cm on the spot line. At the pencil point, use a micro syringe to apply 2uL of phenylperiodic acid sample solution and periic acid standard color scale solution respectively as shown in the figure (three times, so that the diameter of the origin does not exceed 5mm), blow dry, put the chromatography paper into the chromatography tank, and develop it at 20-30℃ using the ascending method. When the solvent ascends to the front line, take it out and blow dry. Under the UV analyzer, 3
HG2076—91
compare the size and intensity of the peri-acid fluorescence spot in the sample with the standard fluorescence spot, and determine the color scale number corresponding to the sample. The percentage of peri-acid in the sample (r2) is calculated according to formula (4): W1×100
where: 01
mass percentage of peri-acid in the standard color scale corresponding to the sample, % (m/m); mass percentage of phenyl peri-acid sample solution, % (m/m). The difference between the two parallel determination results is not greater than 0.5%, and the arithmetic mean is taken as the determination result. Front line of the agonist
DOODODE
A2BSCA
Schematic diagram of peri-acid chromatography in phenyl peri-acid (4)
2uL of peri-acid standard color scale solution is applied at 1, 2, 3, and 4 in the figure, and its mass percentage is 0.01%, 0.015%, 0.02%, and 0.025% (m/m), respectively.
2uL of phenyl peri-acid sample solution is applied at A, B, and C, respectively. E and D represent peri-acid spots and phenyl peri-acid spots, respectively. 4.4 Determination of ammonia insoluble matter content
4.4.1 Reagents and solutions
Ammonia (GB631: chemically pure.
4.4.2 Analysis steps
Weigh 2g of the sample (accurate to 0.002g) and put it into a 150mL beaker, add 10mL of ammonia (4.4.1.1) and 80mL of water, stir and heat until the sample is completely dissolved, filter it while hot through a G3 crucible filter that has been constant weight at 100~105℃, wash it with hot water until the solution is colorless, drain it and place it in a 100~105℃ oven to dry it to constant weight. The percentage of ammonia insoluble matter (r:) is calculated according to formula (5): 3
Where: m
Mass of empty crucible filter, g;
X100... ...
Total mass of crucible filter and insoluble residue after drying, g; mass of sample, ;
Content of phenyl pericyclic acid determined in Article 4.2, %. 4.5 Determination of aniline content
4.5.1 Reagents and solutions
4.5.1.1 Hydrochloric acid (GB622) solution: chemically pure, 1+1 solution; 4.5.1.2 Sodium nitrite (GB633) standard titration solution: chemically pure, c(NaNO,)=0.1mol/L; 4
HG207691
4.5.1.3 Anhydrous sodium carbonate (GB639) solution: 100g/L solution; 4.5.1.4 Potassium bromide (GB649) solution: chemically pure, 200g/solution; 4.5.1.5 Starch-iodide Potassium test solution: (same as 4.2.2.7). 4.5.2 Analysis steps
Weigh 10g (accurate to 0.02g) of the sample into a 500mL flask with 30mL of sodium carbonate solution (4.5.1.3) and 100mL of water, shake to dissolve the sample completely, add water to a total volume of 250mL, add a few zeolites for distillation, and collect the distillate in a 500mL beaker filled with 50mL of hydrochloric acid (4.5.1.1) and 100mL of water until the total volume of the solution in the receiving flask reaches more than 380mL, which is the end point of the distillation. After the distillation is completed, add 10mL of potassium bromide solution (4.5.1.4) to the distillate, and titrate with sodium nitrite standard titration solution (4.5.1.2) until the starch-potassium iodide test solution (4.5.1.5) turns slightly blue. The end point is when the color of the sample is still slightly blue to the starch-potassium iodide solution after 5 minutes. A blank test is performed at the same time.
The percentage of aniline (α) is calculated according to formula (6): _c(V/-Ve)×0.0931
Wherein:
c——concentration of sodium nitrite standard solution, mol/L; V——volume of sodium nitrite standard solution consumed in titration, mL; Vs——volume of sodium nitrite standard solution consumed in blank titration, mLm—mass of the sample,,
21——content of phenyl peri-acid determined in Article 4.2,%; (6)
0.0931——mass of aniline in grams equivalent to 1.00mL sodium nitrite standard titration solution (Cc(NaNO2)=1.000mol/L).
5 Inspection rules
5.1 Phenylperiodic acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all phenylperiodic acid shipped out of the factory meets the requirements of this standard. Each batch of phenylperiodic acid shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Aniline content is a type inspection item, and type inspection shall be conducted no less than twice a year. 5.3 The user shall conduct quality inspection on the received phenylperiodic acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each barrel of each batch of products, insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts and put them into a pond porcelain plate, and mix the samples carefully. The total amount of the sample taken shall not be less than 200g, and it shall be divided into two clean, dry wide-mouth bottles with ground stoppers. Labels shall be affixed to the bottles, indicating the manufacturer name, product name, batch number, and sampling date. One bottle is used for inspection and the other is kept for future reference. 5.5 If any of the test results do not meet the requirements of the standard, re-sampling and re-testing shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of phenylperiodic acid cannot be accepted.
5.6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the issue, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenylperiodic acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional Notes:
HG2076—91
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Factory. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard refers to the Indian standard IS8233—76 "Industrial Phenyl Peri-Acid".1), after dissolving in hot water, transfer to a 100mL volumetric flask and dilute to the scale. Take a 160mm×250mm chromatography paper (4.3.1.4), and draw three lines with a pencil at 1, 2, and 18cm from the bottom of the chromatography paper, namely the immersion line, the spot line, and the front line. Use a pencil to make a point every 2cm on the spot line. At the pencil point, use a micro-syringe to apply 2uL of the phenylperi-acid sample solution and the peri-acid standard color scale solution respectively as shown in the figure (three times, so that the origin diameter does not exceed 5mm), blow dry, put the chromatography paper into the chromatography cylinder, and develop it at 20-30℃ using the ascending method. When the solvent ascends to the front line, take it out and blow dry. Under the UV analyzer, 3
HG2076—91
compare the size and intensity of the peri-acid fluorescence spot in the sample with the standard fluorescence spot, and determine the color scale number corresponding to the sample. The percentage of peri-acid in the sample (r2) is calculated according to formula (4): W1×100
where: 01
mass percentage of peri-acid in the standard color scale corresponding to the sample, % (m/m); mass percentage of phenyl peri-acid sample solution, % (m/m). The difference between the two parallel determination results is not greater than 0.5%, and the arithmetic mean is taken as the determination result. Front line of the agonist
DOODODE
A2BSCA
Schematic diagram of the chromatography of peri-acid in phenyl peri-acid (4)
In the figure, 2uL of the peri-acid standard color scale solution is applied at 1, 2, 3, and 4, and its mass percentage is 0.01%, 0.015%, 0.02%, and 0.025% (m/m), respectively.
2uL of the phenyl peri-acid sample solution is applied at A, B, and C, respectively. E and D represent the peri-acid spot and the phenyl peri-acid spot, respectively. 4.4 Determination of ammonia insoluble matter content
4.4.1 Reagents and solutions
Ammonia (GB631: chemically pure.
4.4.2 Analysis steps
Weigh 2g of the sample (accurate to 0.002g) and put it into a 150mL beaker, add 10mL of ammonia (4.4.1.1) and 80mL of water, stir and heat until the sample is completely dissolved, filter it while hot through a G3 crucible filter that has been constant weight at 100~105℃, wash it with hot water until the solution is colorless, drain it and place it in a 100~105℃ oven to dry it to constant weight. The percentage of ammonia insoluble matter (r:) is calculated according to formula (5): 3
Where: m
Mass of empty crucible filter, g;
X100... ...
Total mass of crucible filter and insoluble residue after drying, g; mass of sample, ;
Content of phenyl pericyclic acid determined in Article 4.2, %. 4.5 Determination of aniline content
4.5.1 Reagents and solutions
4.5.1.1 Hydrochloric acid (GB622) solution: chemically pure, 1+1 solution; 4.5.1.2 Sodium nitrite (GB633) standard titration solution: chemically pure, c(NaNO,)=0.1mol/L; 4
HG207691
4.5.1.3 Anhydrous sodium carbonate (GB639) solution: 100g/L solution; 4.5.1.4 Potassium bromide (GB649) solution: chemically pure, 200g/solution; 4.5.1.5 Starch-iodide Potassium test solution: (same as 4.2.2.7). 4.5.2 Analysis steps
Weigh 10g (accurate to 0.02g) of the sample into a 500mL flask with 30mL of sodium carbonate solution (4.5.1.3) and 100mL of water, shake to dissolve the sample completely, add water to a total volume of 250mL, add a few zeolites for distillation, and collect the distillate in a 500mL beaker filled with 50mL of hydrochloric acid (4.5.1.1) and 100mL of water until the total volume of the solution in the receiving flask reaches more than 380mL, which is the end point of the distillation. After the distillation is completed, add 10mL of potassium bromide solution (4.5.1.4) to the distillate, and titrate with sodium nitrite standard titration solution (4.5.1.2) until the starch-potassium iodide test solution (4.5.1.5) turns slightly blue. The end point is when the color of the sample is still slightly blue to the starch-potassium iodide solution after 5 minutes. A blank test is performed at the same time.
The percentage of aniline (α) is calculated according to formula (6): _c(V/-Ve)×0.0931
Wherein:
c——concentration of sodium nitrite standard solution, mol/L; V——volume of sodium nitrite standard solution consumed in titration, mL; Vs——volume of sodium nitrite standard solution consumed in blank titration, mLm—mass of the sample,,
21——content of phenyl pericyclic acid determined in Article 4.2,%; (6)
0.0931——mass of aniline expressed in grams equivalent to 1.00mL sodium nitrite standard titration solution (Cc(NaNO2)=1.000mol/L).
5 Inspection rules
5.1 Phenylperiodic acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all phenylperiodic acid shipped out of the factory meets the requirements of this standard. Each batch of phenylperiodic acid shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Aniline content is a type inspection item, and type inspection shall be conducted no less than twice a year. 5.3 The user shall conduct quality inspection on the received phenylperiodic acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each barrel of each batch of products, insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts and put them into a pond porcelain plate, and mix the samples carefully. The total amount of the sample taken shall not be less than 200g, and it shall be divided into two clean, dry wide-mouth bottles with ground stoppers. Labels shall be affixed to the bottles, indicating the manufacturer name, product name, batch number, and sampling date. One bottle is used for inspection and the other is kept for future reference. 5.5 If one of the test results does not meet the standard requirements, re-sampling and re-testing should be carried out. If the results still do not meet the requirements of this standard, the entire batch of phenylperiodic acid cannot be accepted.
5.6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the issue, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenylperiodic acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional Notes:
HG2076—91
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Factory. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard refers to the Indian standard IS8233—76 "Industrial Phenyl Peri-Acid".1), after dissolving in hot water, transfer to a 100mL volumetric flask and dilute to the scale. Take a 160mm×250mm chromatography paper (4.3.1.4), and draw three lines with a pencil at 1, 2, and 18cm from the bottom of the chromatography paper, namely the immersion line, the spot line, and the front line. Use a pencil to make a point every 2cm on the spot line. At the pencil point, use a micro-syringe to apply 2uL of the phenylperi-acid sample solution and the peri-acid standard color scale solution respectively as shown in the figure (three times, so that the origin diameter does not exceed 5mm), blow dry, put the chromatography paper into the chromatography cylinder, and develop it at 20-30℃ using the ascending method. When the solvent ascends to the front line, take it out and blow dry. Under the UV analyzer, 3
HG2076—91
compare the size and intensity of the peri-acid fluorescence spot in the sample with the standard fluorescence spot, and determine the color scale number corresponding to the sample. The percentage of peri-acid in the sample (r2) is calculated according to formula (4): W1×100
where: 01
mass percentage of peri-acid in the standard color scale corresponding to the sample, % (m/m); mass percentage of phenyl peri-acid sample solution, % (m/m). The difference between the two parallel determination results is not greater than 0.5%, and the arithmetic mean is taken as the determination result. Front line of the agonist
DOODODE
A2BSCA
Schematic diagram of peri-acid chromatography in phenyl peri-acid (4)
2uL of peri-acid standard color scale solution is applied at 1, 2, 3, and 4 in the figure, and its mass percentage is 0.01%, 0.015%, 0.02%, and 0.025% (m/m), respectively.
2uL of phenyl peri-acid sample solution is applied at A, B, and C, respectively. E and D represent peri-acid spots and phenyl peri-acid spots, respectively. 4.4 Determination of ammonia insoluble matter content
4.4.1 Reagents and solutions
Ammonia (GB631: chemically pure.
4.4.2 Analysis steps
Weigh 2g of the sample (accurate to 0.002g) and put it into a 150mL beaker, add 10mL of ammonia (4.4.1.1) and 80mL of water, stir and heat until the sample is completely dissolved, filter it while hot through a G3 crucible filter that has been constant weight at 100~105℃, wash it with hot water until the solution is colorless, drain it and place it in a 100~105℃ oven to dry it to constant weight. The percentage of ammonia insoluble matter (r:) is calculated according to formula (5): 3
Where: m
Mass of empty crucible filter, g;
X100... ...
Total mass of crucible filter and insoluble residue after drying, g; mass of sample, ;
Content of phenyl pericyclic acid determined in Article 4.2, %. 4.5 Determination of aniline content
4.5.1 Reagents and solutions
4.5.1.1 Hydrochloric acid (GB622) solution: chemically pure, 1+1 solution; 4.5.1.2 Sodium nitrite (GB633) standard titration solution: chemically pure, c(NaNO,)=0.1mol/L; 4
HG207691
4.5.1.3 Anhydrous sodium carbonate (GB639) solution: 100g/L solution; 4.5.1.4 Potassium bromide (GB649) solution: chemically pure, 200g/solution; 4.5.1.5 Starch-iodide Potassium test solution: (same as 4.2.2.7). 4.5.2 Analysis steps
Weigh 10g (accurate to 0.02g) of the sample into a 500mL flask with 30mL of sodium carbonate solution (4.5.1.3) and 100mL of water, shake to dissolve the sample completely, add water to a total volume of 250mL, add a few zeolites for distillation, and collect the distillate in a 500mL beaker filled with 50mL of hydrochloric acid (4.5.1.1) and 100mL of water until the total volume of the solution in the receiving flask reaches more than 380mL, which is the end point of the distillation. After the distillation is completed, add 10mL of potassium bromide solution (4.5.1.4) to the distillate, and titrate with sodium nitrite standard titration solution (4.5.1.2) until the starch-potassium iodide test solution (4.5.1.5) turns slightly blue. The end point is when the color of the sample is still slightly blue to the starch-potassium iodide solution after 5 minutes. A blank test is performed at the same time.
The percentage of aniline (α) is calculated according to formula (6): _c(V/-Ve)×0.0931
Wherein:
c——concentration of sodium nitrite standard solution, mol/L; V——volume of sodium nitrite standard solution consumed in titration, mL; Vs——volume of sodium nitrite standard solution consumed in blank titration, mLm—mass of the sample,,
21——content of phenyl pericyclic acid determined in Article 4.2,%; (6)
0.0931——mass of aniline expressed in grams equivalent to 1.00mL sodium nitrite standard titration solution (Cc(NaNO2)=1.000mol/L).
5 Inspection rules
5.1 Phenylperiodic acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all phenylperiodic acid shipped out of the factory meets the requirements of this standard. Each batch of phenylperiodic acid shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Aniline content is a type inspection item, and type inspection shall be conducted no less than twice a year. 5.3 The user shall conduct quality inspection on the received phenylperiodic acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each barrel of each batch of products, insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts and put them into a pond porcelain plate, and mix the samples carefully. The total amount of the sample taken shall not be less than 200g, and it shall be divided into two clean, dry wide-mouth bottles with ground stoppers. Labels shall be affixed to the bottles, indicating the manufacturer name, product name, batch number, and sampling date. One bottle is used for inspection and the other is kept for future reference. 5.5 If one of the test results does not meet the standard requirements, re-sampling and re-testing should be carried out. If the results still do not meet the requirements of this standard, the entire batch of phenylperiodic acid cannot be accepted.
5.6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the issue, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenylperiodic acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional Notes:
HG2076—91
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Factory. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard refers to the Indian standard IS8233—76 "Industrial Phenyl Peri-Acid".002g) is placed in a 150mL beaker, 10mL ammonia water (4.4.1.1) and 80mL water are added, and the sample is stirred and heated until it is completely dissolved. Then, it is filtered while hot through a G3 crucible filter that has been constant weight at 100-105℃, and washed with hot water until the solution is colorless. After being drained, it is taken out and placed in a 100-105℃ oven and dried to constant weight. The percentage content of ammonia water insoluble matter (r:) is calculated according to formula (5): 3
In the formula: m
Mass of empty crucible filter, g;
X100......
Total mass of crucible filter and insoluble residue after drying, g; Mass of sample,;
Content of phenyl pericyclic acid determined in Article 4.2, %. 4.5 Determination of aniline content
4.5.1 Reagents and solutions
4.5.1.1 Hydrochloric acid (GB622) solution: chemically pure, 1+1 solution; 4.5.1.2 Sodium nitrite (GB633) standard titration solution: chemically pure, c(NaNO,)=0.1mol/L; 4
HG207691
4.5.1.3 Anhydrous sodium carbonate (GB639) solution: 100g/L solution; 4.5.1.4 Potassium bromide (GB649) solution: chemically pure, 200g/solution; 4.5.1.5 Starch-potassium iodide test solution: (same as 4.2.2.7). 4.5.2 Analysis steps
Weigh 10g (accurate to 0.02g) of the sample into a 500mL flask with 30mL of sodium carbonate solution (4.5.1.3) and 100mL of water. Shake to dissolve the sample completely. Add water to a total volume of 250mL. Add a few zeolites for distillation. Collect the distillate in a 500mL beaker with 50mL of hydrochloric acid (4.5.1.1) and 100mL of water. Collect the distillate until the total volume of the solution in the receiving flask reaches more than 380mL. This is the end point of the distillation. After the distillation is completed, add 10mL of potassium bromide solution (4.5.1.4) to the distillate and titrate with sodium nitrite standard titration solution (4.5.1.2) until the starch-potassium iodide test solution (4.5.1.5) is slightly blue. After maintaining for 5 minutes, the starch-potassium iodide test solution is still slightly blue. This is the end point. Perform a blank test at the same time.
The percentage of aniline (α) is calculated according to formula (6): _c(V/-Ve)×0.0931
Wherein:
c——concentration of sodium nitrite standard solution, mol/L; V——volume of sodium nitrite standard solution consumed in titration, mL; Vs——volume of sodium nitrite standard solution consumed in blank titration, mLm—mass of sample,,
21——phenyl peri-acid content determined in Article 4.2, %; (6)
0.0931——mass of aniline in grams equivalent to 1.00mL sodium nitrite standard titration solution (Cc(NaNO2)=1.000mol/L).
5 Inspection rules
5.1 Phenylperiodic acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all phenylperiodic acid shipped out of the factory meets the requirements of this standard. Each batch of phenylperiodic acid shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Aniline content is a type inspection item, and type inspection shall be conducted no less than twice a year. 5.3 The user shall conduct quality inspection on the received phenylperiodic acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each barrel of each batch of products, insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts and put them into a pond porcelain plate, and mix the samples carefully. The total amount of the sample taken shall not be less than 200g, and it shall be divided into two clean, dry wide-mouth bottles with ground stoppers. Labels shall be affixed to the bottles, indicating the manufacturer name, product name, batch number, and sampling date. One bottle is used for inspection and the other is kept for future reference. 5.5 If one of the test results does not meet the standard requirements, re-sampling and re-testing should be carried out. If the results still do not meet the requirements of this standard, the entire batch of phenylperiodic acid cannot be accepted.
5.6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the issue, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenylperiodic acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional Notes:
HG2076—91
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Factory. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard refers to the Indian standard IS8233—76 "Industrial Phenyl Peri-Acid".002g) is placed in a 150mL beaker, 10mL ammonia water (4.4.1.1) and 80mL water are added, and the sample is stirred and heated until it is completely dissolved. Then, it is filtered while hot through a G3 crucible filter that has been constant weight at 100-105℃, and washed with hot water until the solution is colorless. After being drained, it is taken out and placed in a 100-105℃ oven and dried to constant weight. The percentage content of ammonia water insoluble matter (r:) is calculated according to formula (5): 3
In the formula: m
Mass of empty crucible filter, g;
X100......
Total mass of crucible filter and insoluble residue after drying, g; Mass of sample,;
Content of phenyl pericyclic acid determined in Article 4.2, %. 4.5 Determination of aniline content
4.5.1 Reagents and solutions
4.5.1.1 Hydrochloric acid (GB622) solution: chemically pure, 1+1 solution; 4.5.1.2 Sodium nitrite (GB633) standard titration solution: chemically pure, c(NaNO,)=0.1mol/L; 4
HG207691
4.5.1.3 Anhydrous sodium carbonate (GB639) solution: 100g/L solution; 4.5.1.4 Potassium bromide (GB649) solution: chemically pure, 200g/solution; 4.5.1.5 Starch-potassium iodide test solution: (same as 4.2.2.7). 4.5.2 Analysis steps
Weigh 10g (accurate to 0.02g) of the sample into a 500mL flask with 30mL of sodium carbonate solution (4.5.1.3) and 100mL of water. Shake to dissolve the sample completely. Add water to a total volume of 250mL. Add a few zeolites for distillation. Collect the distillate in a 500mL beaker with 50mL of hydrochloric acid (4.5.1.1) and 100mL of water. When the total volume of the solution in the receiving flask reaches more than 380mL, the end point of the distillation is reached. After the distillation is completed, add 10mL of potassium bromide solution (4.5.1.4) to the distillate, and titrate with sodium nitrite standard titration solution (4.5.1.2) until the starch-potassium iodide test solution (4.5.1.5) is slightly blue, and after maintaining for 5 minutes, the starch-potassium iodide test solution is still slightly blue. This is the end point. Perform a blank test at the same time.
The percentage of aniline (α) is calculated according to formula (6): _c(V/-Ve)×0.0931
Wherein:
c——concentration of sodium nitrite standard solution, mol/L; V——volume of sodium nitrite standard solution consumed in titration, mL; Vs——volume of sodium nitrite standard solution consumed in blank titration, mLm—mass of sample,,
21——phenyl pericyclic acid content determined in Article 4.2, %; (6)
0.0931——mass of aniline expressed in grams equivalent to 1.00mL of sodium nitrite standard titration solution (Cc(NaNO2)=1.000mol/L).
5 Inspection rules
5.1 Phenylperiodic acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all phenylperiodic acid shipped out of the factory meets the requirements of this standard. Each batch of phenylperiodic acid shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Aniline content is a type inspection item, and type inspection shall be conducted no less than twice a year. 5.3 The user shall conduct quality inspection on the received phenylperiodic acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each barrel of each batch of products, insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts and put them into a pond porcelain plate, and mix the samples carefully. The total amount of the sample taken shall not be less than 200g, and it shall be divided into two clean, dry wide-mouth bottles with ground stoppers. Labels shall be affixed to the bottles, indicating the manufacturer name, product name, batch number, and sampling date. One bottle is used for inspection and the other is kept for future reference. 5.5 If any of the test results do not meet the requirements of the standard, re-sampling and re-testing shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of phenylperiodic acid cannot be accepted.
5.6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the issue, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenylperiodic acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional Notes:
HG2076—91
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Factory. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard refers to the Indian standard IS8233—76 "Industrial Phenyl Peri-Acid".6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the dispute, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenyl peri-acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional instructions:
HG2076-91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Plant. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard adopts Indian Standard IS8233-76 "Industrial Phenyl Peri-Acid".6 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the dispute, or ask the arbitration institution to conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation, storage
6.1 The packaging barrel is marked with the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date with non-fading paint. 6.2 Phenyl peri-acid is packed in iron barrels or chemical fiber woven bags lined with plastic bags. The net weight of each barrel (bag) is 25kg or 50kg, and the bag mouth should be double-tied. 6.3 Prevent exposure to sunlight and rain during transportation. Be gentle when loading and unloading. 6.4 Store in a ventilated and dry place to avoid sunlight. 5
Additional instructions:
HG2076-91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Wujiang Dongfeng Chemical Plant. The main drafters of this standard are Wang Qiongxuan and Huang Yuxin. This standard adopts Indian Standard IS8233-76 "Industrial Phenyl Peri-Acid".
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