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Chemical Industry Standard of the People's Republic of China
HG2548—93
Published on September 25, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
W.bzsoso.cOI Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG2548—93
This standard specifies the technical conditions, test methods, inspection rules, and marking, packaging, storage, transportation, etc. of Tobias acid (2-amino-1-naphthalenesulfonic acid).
This standard applies to Tobias acid prepared from 2-naphthol by sulfonation, neutralization, and amination. Tobias acid is mainly used as a dye intermediate. Molecular formula: C10HgNOsS
Structural formula:
Relative molecular mass: 223.245 (according to the international relative atomic mass in 1989) 2 Reference standards
GB601 Preparation of standard solution for chemical reagent titration analysis (volumetric analysis) GB9722 General rules for gas chromatography of chemical reagents 3 Technical requirements
Tobiased acid should meet the requirements of Table 1
Total amino value (based on Tobiased acid dry product), %2-naphthylamine, %
Water, %
Test method
4.1 Appearance
Determine by visual method.
4.2 Determination of total amino value
4.2.1 Reagents and solutions
4.2.1.1 Potassium bromide (GB/T649);
Ammonia water (GB/T631) solution: 20%;
Hydrochloric acid (GB/T622) solution: (1+1):
Superior product
White to light red powder
Qualified product
Sodium nitrite (GB/T633) standard titration solution: c(N aNO2)=0.1mol/L, prepared and calibrated according to the provisions of GB601, approved by the Ministry of Chemical Industry of the People's Republic of China on September 25, 1993 and implemented on July 1, 1994
W.bzsoso:com During calibration, starch potassium iodide test paper is used to determine the end point; HG2548-93
4.2.1.5 Starch potassium iodide test paper: Add 0.5g potassium iodide to 100mL of newly prepared 0.5% starch solution, dissolve it, and mix it evenly. Soak the qualitative filter paper in the solution, take it out and dry it in the air or in the oven. Store it in a sealed brown bottle. 4.2.2 Determination steps
Weigh 5g of Tobias acid sample (accurate to 0.001g), add a small amount of water to moisten it, and then add 10mL of ammonia water (4.2.1.2). After the sample is completely dissolved, transfer it to a 250mL volumetric flask, add water to dilute to the scale, and shake it well. Take 25mL of the above test solution and place it in an 800mL beaker. Add 600mL of water, 40mL of hydrochloric acid (4.2.1.3) and 5g of potassium bromide (4.2.1.1). Cool to 15-20℃. Titrate with sodium nitrite standard titration solution (4.2.1.4) under stirring until the starch potassium iodide test paper (4.2.1.5) turns slightly blue. After 3 minutes, the same method is used to test and the test still turns slightly blue, which is the end point. Perform a blank test under the same conditions. The mass percentage of the total amino value X1 is calculated according to formula (1): o·(V.VX0. 223 2×100
mX25/250X(1-X3)
Wherein: c——concentration of sodium nitrite standard titration solution, mol/L, Vi——volume of sodium nitrite standard titration solution consumed by the sample; mL, V2—volume of sodium nitrite standard titration solution consumed by the blank, mL, m——mass of the sample, g;
X3—mass percentage of water content, %;
0.2232—mass of Tobias acid expressed in grams equivalent to 1.00mL sodium nitrite standard titration solution [c(NaNO2)=1.000mol/L].
The difference between the results of two parallel determinations is not greater than 0.25%, and the arithmetic mean is taken as the determination result. 4. 3.2-Naphthylamine content determination Gas chromatography method 4.3.1 Reagents and solutions Www.bzxZ.net
4.3.1.1 Toluene (GB/T684);
Chloroform (GB/T682);
4.3.1.3 Hydrochloric acid (GB/T622) solution: 1mol/L4.3.1.4 Sodium hydroxide (GB/T629) solution: 100g/L; 4.3.1.5 2-Naphthylamine: refined product;
4.3.1.6 Biphenyl.
4.3.2 Instruments
Gas chromatograph: sensitivity and stability meet the requirements of GB9722; recorder: chromatography data processor;
Injector: L micro-syringe:
Detector: Hydrogen flame ionization detector (FID); Chromatographic column: U-shaped or spiral stainless steel column with a length of 1m and an inner diameter of 3mm. 4.3.3 Preparation of chromatographic column
4.3.3.1 Filler
Carrier: 101 white silanized chromatographic carrier, 0.250~0.180mm (60~80 mesh); Stationary liquid: methyl silicone rubber SE-30, maximum operating temperature 350℃, solvent chloroform (4.3.1.2); Coating degree: 10%.
4.3.3.2 Coating of stationary liquid
Weigh 0.5g SE-30 in a beaker, add 18mL chloroform, and after it is completely dissolved, add 101 white silanized carrier 5 dried in a constant temperature oven at 105℃. 0g is poured into a beaker while hot, placed in a fume hood, and allowed to evaporate slowly under an infrared lamp until the solvent is dry (the beaker should be tapped and rotated frequently to ensure even coating). 2
W.4.3.3.3 Filling of stationary phase
HG2548—93
Wrap the end of the chromatographic column connected to the detector with gauze, connect it to a vacuum pump, and connect a funnel to the other end. Slowly pour in the dried stationary phase under vacuum, tap the chromatographic column gently to ensure even and tight filling, plug the filled chromatographic column with glass wool, and prepare for aging. 4.3.3.4 Aging of chromatographic column
Install the filled chromatographic column into the column box of the chromatograph, do not connect a detector after the column, and age it for 8 hours at a carrier gas flow rate of 5 to 10 mL/min and a column temperature of 240°C.
4.3.4 Chromatographic operating conditions
Select the chromatographic operating conditions according to different instruments and the requirements of this standard. Taking 102G chromatograph as an example, the chromatographic operating conditions are as follows: column temperature: 200±1℃;
Detection chamber temperature: 250℃;
Vaporization chamber temperature: 300℃;
Carrier gas (nitrogen) flow rate: 15~20mL/min (pressure 0.1MPa); combustion gas (hydrogen) flow rate: 50~55mL/min; auxiliary gas (air) flow rate: 600mL/min; injection volume: luL;
Recorder paper speed: 300mm/h,
Amplifier sensitivity: high resistance 10%.
4.3.5 Preparation of calibration mixed solution and determination of correction factor 4.3.5.1 Preparation of 2-naphthylamine standard solution
Weigh 0.5g (accurate to 0.0002g) of 2-naphthylamine (4.3.1.5) into a small beaker, add appropriate amount of water and 10mL of hydrochloric acid (4.3.1.3) to dissolve (if the dissolution is slow, slightly heat it), transfer to a 250mL volumetric flask, and dilute to the scale with water. The concentration of this solution is 2.0g/L. Store it below 15℃ and it is valid for two months.
4.3.5.2 Preparation of internal standard extract
Preparation of 0.1g/L internal standard extract:
Weigh 0.025g (accurate to 0.0002g) of internal standard biphenyl, dissolve it with extractant toluene (4.3.1.1), transfer it into a 250mL volumetric flask, and dilute it to the mark with toluene.
Preparation of 0.5g/L internal standard extract:
Weigh 0.125g (accurate to 0.0002g) of internal standard biphenyl, and prepare it in the same way as above. 4.3.5.3 Preparation of calibration mixed solution
In a group of 6 50mL volumetric flasks, add 0.10, 0.20, 0.40, 0.60, 0.80, 1.0mL of 2-naphthylamine standard solution and 2.5mL of 10% sodium hydroxide solution, respectively, and use a pipette to draw 5mL of 0.1g/L internal standard extract into the above volumetric flasks, dilute to the scale with water, shake for 2min, and stand to separate. At this time, the 2-naphthylamine content in the extract layer of each volumetric flask is equivalent to the mass percentage of 2-naphthylamine in the sample (calculated based on 4g sample) of 0.005%, 0.010%, 0.020%, 0.030%, 0.040%, 0.050%, respectively. This group is group A. In another set of 5 50 mL volumetric flasks, add 1.0, 2.0, 3.0, 4.0, and 5.0 mL of 2-naphthylamine standard solution and 2.0 mL of 10% sodium hydroxide solution, respectively.5mL, use a pipette to draw 5mL of 0.5g/L internal standard extract into the above volumetric flasks, dilute to the mark with water, shake for 2min, and let stand to separate. At this time, the 2-naphthylamine content in the extract layer of each volumetric flask is equivalent to the mass percentage of 2-naphthylamine in the test sample (calculated based on 4g sample) of 0.05%, 0.10%, 0.15%, 0.20%, and 0.25%, respectively. This group is Group B. 4.3.5.4 Determination of relative correction factor
After the operating conditions of the instrument are stable, use the injector to draw 1uL of the upper extract of the volumetric flask for injection, and repeat three times in a row. The relative correction factor is calculated according to formula (2):
m,·As
Wherein: ——relative correction factor,
（2）
W.HG2548-93
m; ——mass of 2-naphthylamine in a 50mL volumetric flask, g; ms—mass of the internal standard in a 50mL volumetric flask, g; A.—peak area of the internal standard, mm;
A——peak area of 2-naphthylamine, mm2.
4.3.6 Determination steps
Weigh 4g of Tobias acid sample (accurate to 0.01g) in a 50mL beaker, add 25mL of sodium hydroxide (4.3.1.4), place the beaker on an electric furnace and heat to dissolve until it is almost boiling, transfer it to a 50mL volumetric flask, use a pipette to draw 5.0mL of the internal standard extract into the volumetric flask, dilute to the scale with water, shake vigorously for 2min, and cool to separate layers. After the instrument operating conditions are stable, use the injector to draw 1uL of the upper extract from the volumetric flask. The mass percentage of 2-naphthylamine in Tobias acid X2 is calculated according to formula (3):
wherein A—peak area of 2-naphthylamine, mm;
A. Peak area of internal standard, mm,
A..m..f×100
-mass of internal standard in 50mL volumetric flask, 8;-mass of Tobias acid sample, g;
f——relative correction factor.
Each time the measurement is performed, a calibration mixed solution with a 2-amine content close to that in the sample being tested is used to determine the relative correction factor. ***(3)
The absolute difference between two parallel measurements is no more than 0.003% for superior products and no more than 0.01% for first-class products and qualified products. The arithmetic mean is taken as the measurement result.
4.3.7 Chromatogram
W.4.4 Determination of moisture
4.4.1 Instrument
HG2548-93
Gas chromatogram
1—Solvent toluene; 2—Internal standard biphenyl; 3-naphthylamineElectric constant temperature drying oven: temperature fluctuation range can be controlled within ±2°C; weighing bottle: d5055mm;
Dryer: containing color-changing silica gel or anhydrous calcium chloride. 4.4.2 Operation steps
Weigh about 2g of sample (accurate to 0.0002g) in two weighing bottles with known constant weight, place them in the electric constant temperature drying oven, open the bottle cap, make the distance between the weighing bottle and the mercury ball of the thermometer no more than 100mm, dry at 100°C for 4h, then move the weighing bottle into the dryer, cool to room temperature (about 30min), and then weigh. The moisture mass percentage X3 is calculated according to formula (4): ml-m2×100
Where: m1——sample mass before heating, g; sample mass after heating, g.
5 Inspection rules
5.1 Inspection classification
All items in Table 1 are factory inspection items. W.bzsoso, cOn(4)
5.2 Manufacturer inspection
HG254893
Tobias acid should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all Tobias acid shipped out of the factory meets the requirements of this standard. Each batch of Tobias acid shipped out of the factory should be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, trademark, grade, net weight, batch number, production date and proof of compliance with this standard. 5.3 User acceptance
The user has the right to inspect the Tobias acid received in accordance with the provisions of this standard. 5.4 Sampling method
Take the uniform products inspected each time as a batch, and randomly select 10% of the bags from each batch of products. However, for small batches, the sampling shall not be less than 5 bags. Use a stainless steel sampler to take samples from the upper, middle and lower layers of the container, mix them thoroughly, and use the quartering method to reduce them to about 500g. Pack them in two clean and dry glass bottles or plastic bags with ground mouths, and affix labels to indicate: manufacturer name, product name, batch number, production date and sampling date. One bottle (bag) is inspected by the inspection department, and one bottle (bag) is kept away from light for three months for future reference. 5.5 Re-inspection
If one of the inspection results does not meet the requirements of this standard, samples should be taken from the double amount of containers for re-inspection. Even if only one of the inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 Arbitration
When the supply and demand parties have objections to the product quality, they can be resolved through negotiation. When arbitration is required, the arbitration institution shall be agreed upon by both parties. 6 Marking, packaging, transportation and storage
6.1 Marking
The packaging of Tobias acid should have obvious fixed markings, indicating: manufacturer name, product name, batch number, production date, net weight, trademark, quality grade and this standard number, and indicate the word "moisture-proof". 6.2 Packaging
Tobias acid is packaged in polypropylene woven bags lined with plastic bags, with a net weight of 25kg per bag. When it is packaged in iron drums (lined with plastic bags), the net weight of each drum is 50kg, and the drum cover is sealed.
6.3 Transportation
Tobias acid should be protected from rain during transportation. During shipment, it must be handled with care to prevent the bags from being damaged. 6.4 Storage
Tobias acid products should be stored in a cool and dry place. Additional remarks:
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 technically managed by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Qian Yingchun.
This standard adopts Japanese Industrial Standard SK4152-89 "Tobias Acid". The original professional standard ZBG56001-86 "Tobias Acid" of the People's Republic of China will be invalid from the date of implementation of this standard.2 Operation steps
In two weighing bottles with known constant weight, weigh about 2g of sample (accurate to 0.0002g), place them in an electric constant temperature drying oven, open the bottle cap, make sure the distance between the weighing bottle and the mercury ball of the thermometer is no more than 100mm, dry at 100℃ for 4h, then move the weighing bottle into a dryer, cool to room temperature (about 30min), and then weigh. The moisture mass percentage X3 is calculated according to formula (4): ml-m2×100
Where: m1——sample mass before heating, g; sample mass after heating, g.
5 Inspection rules
5.1 Inspection classification
All items in Table 1 are factory inspection items. W.bzsoso，cOn(4)
5.2 Inspection by the manufacturer
HG254893
Tobias acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all Tobias acid shipped out of the factory meets the requirements of this standard. Each batch of Tobias acid shipped out of the factory shall be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, trademark, grade, net weight, batch number, production date and proof of compliance with this standard. 5.3 User acceptance
The user has the right to inspect the Tobias acid received in accordance with the provisions of this standard. 5.4 Sampling method
Take the uniform products inspected each time as a batch, and randomly select 10% of the bags from each batch of products. However, for small batches, the sampling shall not be less than 5 bags. Use a stainless steel sampler to take samples from the upper, middle and lower layers of the container, mix them thoroughly, and use the quartering method to reduce them to about 500g. Pack them in two clean and dry glass bottles or plastic bags with ground mouths, and affix labels to indicate: manufacturer name, product name, batch number, production date and sampling date. One bottle (bag) is inspected by the inspection department, and one bottle (bag) is kept away from light for three months for future reference. 5.5 Re-inspection
If one of the inspection results does not meet the requirements of this standard, samples should be taken from the double amount of containers for re-inspection. Even if only one of the inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 Arbitration
When the supply and demand parties have objections to the product quality, they can be resolved through negotiation. When arbitration is required, the arbitration institution shall be agreed upon by both parties. 6 Marking, packaging, transportation and storage
6.1 Marking
The packaging of Tobias acid should have obvious fixed markings, indicating: manufacturer name, product name, batch number, production date, net weight, trademark, quality grade and this standard number, and indicate the word "moisture-proof". 6.2 Packaging
Tobias acid is packaged in polypropylene woven bags lined with plastic bags, with a net weight of 25kg per bag. When it is packaged in iron drums (lined with plastic bags), the net weight of each drum is 50kg, and the drum cover is sealed.
6.3 Transportation
Tobias acid should be protected from rain during transportation. During shipment, it must be handled with care to prevent the bags from being damaged. 6.4 Storage
Tobias acid products should be stored in a cool and dry place. Additional remarks:
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 technically managed by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Qian Yingchun.
This standard adopts Japanese Industrial Standard SK4152-89 "Tobias Acid". The original professional standard ZBG56001-86 "Tobias Acid" of the People's Republic of China will be invalid from the date of implementation of this standard.2 Operation steps
In two weighing bottles with known constant weight, weigh about 2g of sample (accurate to 0.0002g), place them in an electric constant temperature drying oven, open the bottle cap, make sure the distance between the weighing bottle and the mercury ball of the thermometer is no more than 100mm, dry at 100℃ for 4h, then move the weighing bottle into a dryer, cool to room temperature (about 30min), and then weigh. The moisture mass percentage X3 is calculated according to formula (4): ml-m2×100
Where: m1——sample mass before heating, g; sample mass after heating, g.
5 Inspection rules
5.1 Inspection classification
All items in Table 1 are factory inspection items. W.bzsoso，cOn(4)
5.2 Inspection by the manufacturer
HG254893
Tobias acid shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all Tobias acid shipped out of the factory meets the requirements of this standard. Each batch of Tobias acid shipped out of the factory shall be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, trademark, grade, net weight, batch number, production date and proof of compliance with this standard. 5.3 User acceptance
The user has the right to inspect the Tobias acid received in accordance with the provisions of this standard. 5.4 Sampling method
Take the uniform products inspected each time as a batch, and randomly select 10% of the bags from each batch of products. However, for small batches, the sampling shall not be less than 5 bags. Use a stainless steel sampler to take samples from the upper, middle and lower layers of the container, mix them thoroughly, and use the quartering method to reduce them to about 500g. Pack them in two clean and dry glass bottles or plastic bags with ground mouths, and affix labels to indicate: manufacturer name, product name, batch number, production date and sampling date. One bottle (bag) is inspected by the inspection department, and one bottle (bag) is kept away from light for three months for future reference. 5.5 Re-inspection
If one of the inspection results does not meet the requirements of this standard, samples should be taken from the double amount of containers for re-inspection. Even if only one of the inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 Arbitration
When the supply and demand parties have objections to the product quality, they can be resolved through negotiation. When arbitration is required, the arbitration institution shall be agreed upon by both parties. 6 Marking, packaging, transportation and storage
6.1 Marking
The packaging of Tobias acid should have obvious fixed markings, indicating: manufacturer name, product name, batch number, production date, net weight, trademark, quality grade and this standard number, and indicate the word "moisture-proof". 6.2 Packaging
Tobias acid is packaged in polypropylene woven bags lined with plastic bags, with a net weight of 25kg per bag. When it is packaged in iron drums (lined with plastic bags), the net weight of each drum is 50kg, and the drum cover is sealed.
6.3 Transportation
Tobias acid should be protected from rain during transportation. During shipment, it must be handled with care to prevent the bags from being damaged. 6.4 Storage
Tobias acid products should be stored in a cool and dry place. Additional remarks:
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 technically managed by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Qian Yingchun.
This standard adopts Japanese Industrial Standard SK4152-89 "Tobias Acid". The original professional standard ZBG56001-86 "Tobias Acid" of the People's Republic of China will be invalid from the date of implementation of this standard.
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