Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2668-95
Published on April 5, 1995
Implemented on January 1, 1996
Ministry of Chemical Industry of the People's Republic of China
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2668-95
Replaces GB/T1654-79
This standard specifies the technical requirements, test methods, acceptance rules and requirements for marking, packaging, transportation and storage of Naphthophenol AS-D. This standard applies to Naphthophenol AS-D prepared by the condensation of 2-hydroxy-3-naphthoic acid and o-toluidine. Naphthophenol AS-D is mainly used for the manufacture of pigments, dyeing and printing of cotton fibers.
Structural formula:
Molecular formula: C18H1502N
Relative molecular mass: 277.28 (according to the 1991 international relative atomic mass) Reference standards
GB/T601 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB2374 General conditions for dyeing determination GB/T2381 Determination method for insoluble matter content in dyes GB/T2383 Determination method for sieving fineness of dyes GB/T2384 General method for determination of melting point range of dye intermediates 3 Technical requirements
3.1 Appearance: beige uniform powder.
3.2 The quality of chromophore AS-D shall comply with the requirements of Table 1. Table 1
(1) Dyeing shade produced by coupling with scarlet base G on cotton fiber(2) Dyeing intensity produced by coupling with scarlet base G on cotton fiber(3) Content of phenol AS-D, %
(4) Initial melting point of dry product, °C
(5) Content of insoluble matter in alkali solution, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995>
Similar to the standard product to the nearest micro
100 points of the standard
1996-01-01 implementation
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(6) 2-hydroxy-3-naphthoic acid content, %
HG/T2668-95
Continued Table 1
(7) Fineness (content of residue passing through a standard sieve with an aperture of 250μm), % Note:
① The content and melting point of the chromophore AS-D used for dyeing are not measured. ② The color light and intensity of the chromophore AS-D used for other purposes are not measured. 4 Test method
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water in accordance with GB/T6682. 4.1 Determination of appearance
The appearance is evaluated by visual inspection.
4.2 Identification of the color and intensity of the dyeing generated by coupling with scarlet base G on cotton fibers 4.2.1 Principle of the method
The sample and standard sample of Naphthophenol AS-D are coupled with scarlet base G diammonium salt solution (4-nitro-2-aminotoluene diazonium salt solution) on cotton fibers respectively, and the color and intensity of the dyeing generated on the cotton fibers are visually compared. 4.2.2 Reagents and solutions
95% ethanol (GB/T679);
Sodium hydroxide (GB/T629): 35% solution; Formaldehyde solution (GB/T685);
Scarlet red base G: industrial product;
Anhydrous sodium carbonate (GB/T639);
Hydrochloric acid (GB/T622),
Anhydrous sodium acetate (GB/T694): 20% solution Sodium nitrite (GB/T633): 10% solution; Neutral soap: industrial product, containing 60% fatty acids; Turkish red oil: industrial product, 40%;
Turkish red oil alkaline solution: take 20mL of Turkish red oil, add 10mL of 35% sodium hydroxide solution, dilute to 1000mL with water, soap solution: 5g soap flakes, 3g sodium carbonate are dissolved in 1000mL water. 4.2.3 Determination steps
4.2.3.1 Preparation of primer
Accurately weigh 1g of the standard sample and test sample of Naphthophenol AS-D (accurate to 0.001g), place them in a 600mL beaker, add 1.5mL of 95% ethanol, mix into a homogeneous slurry, then add 0.5mL of 35% sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution, and after it is completely dissolved, add 0.5mL of 30% formaldehyde solution. Let it stand for 10 minutes, transfer it to a 500mL volumetric flask, and dilute to the mark with Turkey red oil alkali solution. In five 300mL dye vats, prepare the primer according to the provisions of Table 2. 2
Wbzsoso，cO Dyeing vat number
1g/500mL standard sample solution, mL
1g/500mL sample solution, mL
Add Turkey red oil alkali solution, mL
Bath ratio: 1:20
4.2.3.2 Primer operation
HG/T2668—95
Adjust the primer solution temperature to 40℃, and immerse five skeins of cotton yarn (or cotton cloth) weighing 10g each into the primer solution in the order of number, stir frequently to ensure uniform absorption, maintain the primer solution temperature at 35-40℃, and prime for 30min. Take out and wring dry evenly, so that the moisture content is 90-100% (if it is cotton cloth, it should be rolled dry evenly on the roller dyeing machine after taking it out, so that the moisture content is 90-100%, but the roller should be scrubbed with chromophore AS-D solution before rolling dyeing), and then quickly develop color. 4.2.3.3 Preparation of color developing solution
Weigh 1g of scarlet base G (accurate to 0.01g), put it in a 1000mL beaker, adjust it into a slurry with a small amount of water, and then add 2mL35% hydrochloric acid and 30mL water to dissolve it. If it does not dissolve, heat it until it dissolves, add ice cubes, adjust the temperature to about 510℃, and add 5mL10% sodium nitrite solution for diazotization under stirring, and the diazotization time is 30min. Adjust the pH to 4-5 with about 10mL of 20% sodium acetate solution, and dilute it to 800mL.
4.2.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 800mL of color development solution at the same time, stir frequently, keep the liquid temperature at 10-15℃, and color for 30 minutes. Take out and wring dry, wash, boil in 800mL of soap solution, take out and wash, wring dry. Dry at 60-70℃, cool to room temperature, and then conduct visual evaluation.
4.2.4 Evaluation of color and intensity of dyeing
Perform in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation is ±5%. 4.3 Determination of the content of chromophore AS-D
4.3.1 Principle of the method
Chromophore AS-D is a weakly acidic compound. In the presence of ethanol, it is dissolved with excess alkali and titrated with a standard hydrochloric acid solution to determine the content of chromophore AS-D. 4.3.2 Reagents and solutions
Sodium hydroxide (GB/T629): 10% solution; anhydrous ethanol (GB/T678);
Hydrochloric acid (GB/T622) standard solution: 0.1mol/L; 4.3.3 Instruments
Potentiometric titrator (or acidometer):
Measuring range 0~14pH:
The minimum grid of the meter is 0.1pH, and the accuracy is ±0.1pH/3pH; glass electrode: type 231;
calomel electrode: type 232.
Installation of the instrument is as shown in Figure 1.
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HG/T2668—95
1—burette; 2—calomel electrode, 3—glass electrode; 4—rubber stopper, 5—glass titration cup; 6—electromagnetic stirring rod 4.3.4 Determination steps
Weigh 0.75g (accurate to 0.0002g) of the naphthol AS-D sample and place it in a glass titration cup. Add 10mL of anhydrous ethanol, put in an electromagnetic stirring rod, cover the stopper, start the magnetic stirrer to fully wet the naphthol AS-D, and add about 1.1mL of 10% sodium hydroxide solution (the amount added can be adjusted according to the actual concentration of the sodium hydroxide solution and the concentration of the hydrochloric acid standard solution, so that the consumption of the hydrochloric acid standard solution is preferably less than 5mL when determining the free alkali). Cover the stopper and continue stirring until the sample is completely dissolved. Install the instrument according to Figure 1, and perform potentiometric titration with 0.1mol/L hydrochloric acid standard titration solution. At one pH value (about pH 13) before the free alkali titration endpoint, gradually add the hydrochloric acid standard titration solution in batches, about 0.1mL each time, and record the corresponding pH value and the amount of hydrochloric acid standard titration solution consumed. When the difference between the two adjacent pH values reaches the maximum, it is the free alkali titration endpoint, and record the milliliters of 0.1mol/L hydrochloric acid standard titration solution consumed V1. Continue titrating until the pH is about 9 (that is, about 1.5 pH values), drip hydrochloric acid standard titration solution in batches, 1 drop each time, and record the corresponding pH value and milliliters of hydrochloric acid standard titration solution. When the difference between two adjacent pH values reaches the maximum, it is the total alkali titration endpoint (about pH7.7), and record the milliliters of 0.1mol/L hydrochloric acid standard titration solution consumed V2.
Blank test: In another glass titration cup, add 10mL of anhydrous ethanol and 1.1mL of 10% sodium hydroxide solution, and install the instrument according to Figure 1. When titrating to pH11, drip 0.1mol/L hydrochloric acid standard titration solution in batches, 1 drop each time, and record the pH value and milliliters of hydrochloric acid standard titration solution consumed. There is a sudden jump near pH8.7 and 5.7, and the difference AV of the hydrochloric acid standard titration solution at the two sudden jumps is the blank value.
4.3.5 Calculation
The mass percentage content of phenol AS-D (X,) is calculated according to formula (1): Xi = °C. (Vi-Vz-AV)X0. 273 3.m
In the formula: c-concentration of standard hydrochloric acid solution, mol/L, 100
V,—volume of 0.1mol/L standard hydrochloric acid solution consumed in titration of free alkali, mL; V2——volume of 0.1mol/L standard hydrochloric acid solution consumed in titration of total alkali, mL, AV——volume of 0.1mol/L standard hydrochloric acid solution consumed in blank test, mL, 4
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mass of chromophore AS-D sample, g;
HG/T2668-95
0.2773——mass of chromophore AS-D expressed in grams equivalent to 1.00mL standard hydrochloric acid solution [c(HCI)=1.000mol/L].
4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.5%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of initial melting point of dry product
Carry out in accordance with the relevant provisions of GB/T2384.
4.5 Determination of insoluble matter in alkali solution
Carry out in accordance with the determination method of alkali-insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
The components are separated by using the difference in relative affinity of the molecules of each component in the analyzed substance to the mobile phase and the stationary phase, and the impurity content is determined by comparing with the reference standard.
4.6.2 Apparatus and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography that there should be no other impurities. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, to prepare 1, 2, 3, 4, 5mg/100mL solutions.
Preparation of 10g/100mL Naphthol AS-D sample solution: Weigh 1.0g of Naphthol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and dot a point every 2cm on the line with a pencil. At the pencil point, use a micro syringe to apply 1mL of the chromophore AS-D sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2, blow dry, put into the chromatography cylinder, and develop by the ascending method. When the solvent front rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and fluorescence intensity of the 2-hydroxy-3-naphthoic acid spots in the standard and sample under the UV analyzer to determine the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Wherein: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthoic acid sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthoic acid AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-naphthoic acid standard solution is added at each point 1, 2, 3, 4, and 5, and its concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of naphthoic acid sample solution is added at each point A, B, C, D, and E.
Note: When UV analyzer is not used, the colorimetric method of GB/T1652 can be used for verification. 4.7 Determination of fineness
Perform according to the relevant provisions of GB/T2383. A standard sieve with an aperture of 250μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items, among which, except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Factory inspection
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meets the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples from the upper, middle and lower parts. The sampling volume shall not be less than 500g. Mix the sample carefully and put it in two clean and dry glass bottles with ground stoppers and seal them with paraffin. Stick labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for future reference. 5.5 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for inspection. If the re-inspection results do not meet the requirements of this standard even if only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-D shall be unqualified. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis shall be conducted in accordance with the test methods specified in this standard.
Wbzsoso，cOn6 Marking, packaging, transportation and storage
6.1 Marking
HG/T2668—95
The outer packaging of Naphthophenol AS-D shall be painted with a firm mark indicating: manufacturer name, product name, registered trademark, product grade, batch number, production date and net weight.
Each batch of packaged products shall be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that the product quality meets the requirements of this standard and the number of this standard. 6.2 Packaging
Naphthophenol AS-D is packaged in sacks, woven bags or iron barrels lined with plastic bags, with a net weight of 25kg or 50kg per bag (barrel). 6.3 Transportation
Do not place near fire during transportation. Be careful and gentle when handling, avoid heavy pressure, so as not to damage the packaging. 6.4 Storage
Naphthophenol AS-D should be stored in a clean, dry and ventilated warehouse, away from fire, and prevent from heat and moisture. Additional remarks:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and this standard is drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dye Chemical Factory No. 9. The main drafters of this standard are Wang Qiongxuan, Ding Meifang and Ding Lingying. From the date of implementation of this standard, the original national standard GB/T1654-79 "Naphthophenol AS-D" will be invalid. 7
W.1mol/L hydrochloric acid standard titration solution milliliters V2.
Blank test: In another glass titration cup, add 10mL of anhydrous ethanol and 1.1mL of 10% sodium hydroxide solution, and install the instrument according to Figure 1. When titrating to pH11, add 0.1mol/L hydrochloric acid standard titration solution in batches, 1 drop each time, and record the pH value and the milliliters of hydrochloric acid standard titration solution consumed. There is a sudden jump near pH8.7 and 5.7. The difference AV of the hydrochloric acid standard titration solution at the two sudden jumps is the blank value.
4.3.5 Calculation
The mass percentage content of phenol AS-D (X,) is calculated according to formula (1): Xi=℃. (Vi-Vz-AV)X0. 273 3.m
In the formula: c-concentration of standard hydrochloric acid solution, mol/L, 100
V,—volume of 0.1mol/L standard hydrochloric acid solution consumed in titration of free alkali, mL; V2——volume of 0.1mol/L standard hydrochloric acid solution consumed in titration of total alkali, mL, AV——volume of 0.1mol/L standard hydrochloric acid solution consumed in blank test, mL, 4
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mass of chromophore AS-D sample, g;
HG/T2668-95
0.2773——mass of chromophore AS-D expressed in grams equivalent to 1.00mL standard hydrochloric acid solution [c(HCI)=1.000mol/L].
4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.5%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of initial melting point of dry product
Carry out in accordance with the relevant provisions of GB/T2384.
4.5 Determination of insoluble matter in alkali solution
Carry out in accordance with the determination method of alkali-insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
The components are separated by using the difference in relative affinity of the molecules of each component in the analyzed substance to the mobile phase and the stationary phase, and the impurity content is determined by comparing with the reference standard.
4.6.2 Apparatus and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography that there should be no other impurities. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, to prepare 1, 2, 3, 4, 5mg/100mL solutions.
Preparation of 10g/100mL Naphthophenol AS-D sample solution: Weigh 1.0g of Naphthophenol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and dot a point every 2cm on the line with a pencil. At the pencil point, use a micro syringe to apply 1mL of the chromophore AS-D sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2, blow dry, put into the chromatography cylinder, and develop by the ascending method. When the solvent front rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and fluorescence intensity of the 2-hydroxy-3-naphthoic acid spots in the standard and sample under the UV analyzer to determine the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Wherein: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthoic acid sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthoic acid AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-naphthoic acid standard solution is added at each point 1, 2, 3, 4, and 5, and its concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of naphthoic acid sample solution is added at each point A, B, C, D, and E.
Note: When UV analyzer is not used, the colorimetric method of GB/T1652 can be used for verification. 4.7 Determination of fineness
Perform according to the relevant provisions of GB/T2383. A standard sieve with an aperture of 250μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items, among which, except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Factory inspection
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meets the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples from the upper, middle and lower parts. The sampling volume shall not be less than 500g. Mix the sample carefully and put it in two clean and dry glass bottles with ground stoppers and seal them with paraffin. Stick labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for future reference. 5.5 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for inspection. If the re-inspection results do not meet the requirements of this standard even if only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-D shall be unqualified. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis shall be conducted in accordance with the test methods specified in this standard.
Wbzsoso，cOn6 Marking, packaging, transportation and storage
6.1 Marking
HG/T2668—95
The outer packaging of Naphthophenol AS-D shall be painted with a firm mark indicating: manufacturer name, product name, registered trademark, product grade, batch number, production date and net weight.
Each batch of packaged products shall be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that the product quality meets the requirements of this standard and the number of this standard. 6.2 Packaging
Naphthophenol AS-D is packaged in sacks, woven bags or iron barrels lined with plastic bags, with a net weight of 25kg or 50kg per bag (barrel). 6.3 Transportation
Do not place near fire during transportation. Be careful and gentle when handling, avoid heavy pressure, so as not to damage the packaging. 6.4 Storage
Naphthophenol AS-D should be stored in a clean, dry and ventilated warehouse, away from fire, and prevent from heat and moisture. Additional remarks:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and this standard is drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dye Chemical Factory No. 9. The main drafters of this standard are Wang Qiongxuan, Ding Meifang and Ding Lingying. From the date of implementation of this standard, the original national standard GB/T1654-79 "Naphthophenol AS-D" will be invalid. 7
W.1mol/L hydrochloric acid standard titration solution milliliters V2.
Blank test: In another glass titration cup, add 10mL of anhydrous ethanol and 1.1mL of 10% sodium hydroxide solution, and install the instrument according to Figure 1. When titrating to pH11, add 0.1mol/L hydrochloric acid standard titration solution in batches, 1 drop each time, and record the pH value and the milliliters of hydrochloric acid standard titration solution consumed. There is a sudden jump near pH8.7 and 5.7. The difference AV of the hydrochloric acid standard titration solution at the two sudden jumps is the blank value.
4.3.5 Calculation
The mass percentage content of phenol AS-D (X,) is calculated according to formula (1): Xi=℃. (Vi-Vz-AV)X0. 273 3.m
In the formula: c-concentration of standard hydrochloric acid solution, mol/L, 100
V,—volume of 0.1mol/L standard hydrochloric acid solution consumed in titration of free alkali, mL; V2——volume of 0.1mol/L standard hydrochloric acid solution consumed in titration of total alkali, mL, AV——volume of 0.1mol/L standard hydrochloric acid solution consumed in blank test, mL, 4
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mass of chromophore AS-D sample, g;
HG/T2668-95
0.2773——mass of chromophore AS-D expressed in grams equivalent to 1.00mL standard hydrochloric acid solution [c(HCI)=1.000mol/L].
4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.5%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of initial melting point of dry product
Carry out in accordance with the relevant provisions of GB/T2384.
4.5 Determination of insoluble matter in alkali solution
Carry out in accordance with the determination method of alkali-insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
The components are separated by using the difference in relative affinity of the molecules of each component in the analyzed substance to the mobile phase and the stationary phase, and the impurity content is determined by comparing with the reference standard.
4.6.2 Apparatus and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography that there should be no other impurities. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, to prepare 1, 2, 3, 4, 5mg/100mL solutions.
Preparation of 10g/100mL Naphthol AS-D sample solution: Weigh 1.0g of Naphthol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and dot a point every 2cm on the line with a pencil. At the pencil point, use a micro syringe to apply 1mL of the chromophore AS-D sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2, blow dry, put into the chromatography cylinder, and develop by the ascending method. When the solvent front rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and fluorescence intensity of the 2-hydroxy-3-naphthoic acid spots in the standard and sample under the UV analyzer to determine the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Wherein: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthoic acid sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthoic acid AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-naphthoic acid standard solution is added at each point 1, 2, 3, 4, and 5, and its concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of naphthoic acid sample solution is added at each point A, B, C, D, and E.
Note: When UV analyzer is not used, the colorimetric method of GB/T1652 can be used for verification. 4.7 Determination of fineness
Perform according to the relevant provisions of GB/T2383. A standard sieve with an aperture of 250μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items, among which, except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Factory inspection
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meets the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples from the upper, middle and lower parts. The sampling volume shall not be less than 500g. Mix the sample carefully and put it in two clean and dry glass bottles with ground stoppers and seal them with paraffin. Stick labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for future reference. 5.5 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for inspection. If the re-inspection results do not meet the requirements of this standard even if only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-D shall be unqualified. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis shall be conducted in accordance with the test methods specified in this standard.
Wbzsoso，cOn6 Marking, packaging, transportation and storage
6.1 Marking
HG/T2668—95
The outer packaging of Naphthophenol AS-D shall be painted with a firm mark indicating: manufacturer name, product name, registered trademark, product grade, batch number, production date and net weight.
Each batch of packaged products shall be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that the product quality meets the requirements of this standard and the number of this standard. 6.2 Packaging
Naphthophenol AS-D is packaged in sacks, woven bags or iron barrels lined with plastic bags, with a net weight of 25kg or 50kg per bag (barrel). 6.3 Transportation
Do not place near fire during transportation. Be careful and gentle when handling, avoid heavy pressure, so as not to damage the packaging. 6.4 Storage
Naphthophenol AS-D should be stored in a clean, dry and ventilated warehouse, away from fire, and prevent from heat and moisture. Additional remarks:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and this standard is drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dye Chemical Factory No. 9. The main drafters of this standard are Wang Qiongxuan, Ding Meifang and Ding Lingying. From the date of implementation of this standard, the original national standard GB/T1654-79 "Naphthophenol AS-D" will be invalid. 7
W.(Vi-Vz-AV)X0. 273 3.m
Wherein: c-concentration of standard hydrochloric acid titration solution, mol/L, 100
V,—volume of 0.1mol/L standard hydrochloric acid titration solution consumed in titration of free alkali, mL; V2——volume of 0.1mol/L standard hydrochloric acid titration solution consumed in titration of total alkali, mL, AV——volume of 0.1mol/L standard hydrochloric acid titration solution consumed in blank test, mL, 4
Wbzsoso,cOm-
mass of chromophore AS-D sample, g;
HG/T2668—95
0.2773——mass of chromophore AS-D expressed in grams equivalent to 1.00mL standard hydrochloric acid titration solution [c(HCI)=1.000mol/L].
4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.5%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of initial melting point of dry product
Carry out in accordance with the relevant provisions of GB/T2384.
4.5 Determination of insoluble matter in alkali solution
Carry out in accordance with the determination method of alkali-insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
The components are separated by using the difference in relative affinity of the molecules of each component in the analyzed substance to the mobile phase and the stationary phase, and the impurity content is determined by comparing with the reference standard.
4.6.2 Apparatus and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography that there should be no other impurities. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, to prepare 1, 2, 3, 4, 5mg/100mL solutions.
Preparation of 10g/100mL Naphthol AS-D sample solution: Weigh 1.0g of Naphthol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and dot a point every 2cm on the line with a pencil. At the pencil point, use a micro syringe to apply 1mL of the chromophore AS-D sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2, blow dry, put into the chromatography cylinder, and develop by the ascending method. When the solvent front rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and fluorescence intensity of the 2-hydroxy-3-naphthoic acid spots in the standard and sample under the UV analyzer to determine the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Wherein: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthoic acid sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthoic acid AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-naphthoic acid standard solution is added at each point 1, 2, 3, 4, and 5, and its concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of naphthoic acid sample solution is added at each point A, B, C, D, and E.
Note: When UV analyzer is not used, the colorimetric method of GB/T1652 can be used for verification. 4.7 Determination of fineness
Perform according to the relevant provisions of GB/T2383. A standard sieve with an aperture of 250μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items, among which, except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Factory inspection
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meets the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples from the upper, middle and lower parts. The sampling volume shall not be less than 500g. Mix the sample carefully and put it in two clean and dry glass bottles with ground stoppers and seal them with paraffin. Stick labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for future reference. 5.5 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for inspection. If the re-inspection results do not meet the requirements of this standard even if only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-D shall be unqualified. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis shall be conducted in accordance with the test methods specified in this standard.
Wbzsoso，cOn6 Marking, packaging, transportation and storage
6.1 Marking
HG/T2668—95
The outer packaging of Naphthophenol AS-D shall be painted with a firm mark indicating: manufacturer name, product name, registered trademark, product grade, batch number, production date and net weight.
Each batch of packaged products shall be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that the product quality meets the requirements of this standard and the number of this standard. 6.2 Packaging
Naphthophenol AS-D is packaged in sacks, woven bags or iron barrels lined with plastic bags, with a net weight of 25kg or 50kg per bag (barrel). 6.3 Transportation
Do not approach fire during transportation. Be careful when handling and avoid heavy pressure to avoid damage to the packaging. 6.4 Storage
Naphthophenol AS-D should be stored in a clean, dry and ventilated warehouse. Do not approach fire to prevent heat and moisture. Additional instructions:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dye Chemical Factory No. 9. The main drafters of this standard are Wang Qiongxuan, Ding Meifang and Ding Lingying. From the date of implementation of this standard, the original national standard GB/T1654-79 "Naphthophenol AS-D" will be invalid. 7
W.(Vi-Vz-AV)X0. 273 3.m
Wherein: c-concentration of standard hydrochloric acid titration solution, mol/L, 100
V,—volume of 0.1mol/L standard hydrochloric acid titration solution consumed in titration of free alkali, mL; V2——volume of 0.1mol/L standard hydrochloric acid titration solution consumed in titration of total alkali, mL, AV——volume of 0.1mol/L standard hydrochloric acid titration solution consumed in blank test, mL, 4
Wbzsoso,cOm-
mass of chromophore AS-D sample, g;
HG/T2668—95
0.2773——mass of chromophore AS-D expressed in grams equivalent to 1.00mL standard hydrochloric acid titration solution [c(HCI)=1.000mol/L].
4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.5%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of initial melting point of dry product
Carry out in accordance with the relevant provisions of GB/T2384.
4.5 Determination of insoluble matter in alkali solution
Carry out in accordance with the determination method of alkali-insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
The components are separated by using the difference in relative affinity of the molecules of each component in the analyzed substance to the mobile phase and the stationary phase, and the impurity content is determined by comparing with the reference standard.
4.6.2 Apparatus and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography that there should be no other impurities. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, to prepare 1, 2, 3, 4, 5mg/100mL solutions.
Preparation of 10g/100mL Naphthophenol AS-D sample solution: Weigh 1.0g of Naphthophenol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and dot a point every 2cm on the line with a pencil. At the pencil point, use a micro syringe to apply 1mL of the chromophore AS-D sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2, blow dry, put into the chromatography cylinder, and develop by the ascending method. When the solvent front rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and fluorescence intensity of the 2-hydroxy-3-naphthoic acid spots in the standard and sample under the UV analyzer to determine the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Wherein: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthoic acid sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthoic acid AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-naphthoic acid standard solution is added at each point 1, 2, 3, 4, and 5, and its concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of naphthoic acid sample solution is added at each point A, B, C, D, and E.
Note: When UV analyzer is not used, the colorimetric method of GB/T1652 can be used for verification. 4.7 Determination of fineness
Perform according to the relevant provisions of GB/T2383. A standard sieve with an aperture of 250μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items, among which, except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Factory inspection
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meets the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples from the upper, middle and lower parts. The sampling volume shall not be less than 500g. Mix the sample carefully and put it in two clean and dry glass bottles with ground stoppers and seal them with paraffin. Stick labels on the bottles, indicating: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for future reference. 5.5 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for inspection. If the re-inspection results do not meet the requirements of this standard even if only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-D shall be unqualified. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis shall be conducted in accordance with the test methods specified in this standard.
Wbzsoso，cOn6 Marking, packaging, transportation and storage
6.1 Marking
HG/T2668—95
The outer packaging of Naphthophenol AS-D shall be painted with a firm mark indicating: manufacturer name, product name, registered trademark, product grade, batch number, production date and net weight.
Each batch of packaged products shall be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that the product quality meets the requirements of this standard and the number of this standard. 6.2 Packaging
Naphthophenol AS-D is packaged in sacks, woven bags or iron barrels lined with plastic bags, with a net weight of 25kg or 50kg per bag (barrel). 6.3 Transportation
Do not place near fire during transportation. Be careful and gentle when handling, avoid heavy pressure, so as not to damage the packaging. 6.4 Storage
Naphthophenol AS-D should be stored in a clean, dry and ventilated warehouse, away from fire, and prevent from heat and moisture. Additional remarks:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and this standard is drafted by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dye Chemical Factory No. 9. The main drafters of this standard are Wang Qiongxuan, Ding Meifang and Ding Lingying. From the date of implementation of this standard, the original national standard GB/T1654-79 "Naphthophenol AS-D" will be invalid. 7
W.5 Determination of insoluble matter in alkali solution
According to the method for determination of alkali insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
Use the difference in relative affinity of each component molecule in the analyzed substance to the mobile phase and the stationary phase to separate the components, and use the reference standard as a reference to determine the impurity content.
4.6.2 Instruments and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography to see if there are other impurities. Preparation of the standard series of 2-hydroxy-3-naphthoic acid solutions: weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute it to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, and 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, that is, prepare 1, 2, 3, 4, and 5mg/100mL solutions.
Preparation of 10g/100mL Naphthophenol AS-D sample solution: Weigh 1.0g Naphthophenol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and dot a point every 2cm on the line with a pencil. At the pencil point, use a micro syringe to apply 1mL each of the Naphthophenol AS-D sample solution and 2-hydroxy-3-naphthoic acid standard solution, as shown in Figure 2, blow dry, put it into the chromatography cylinder, and develop it by the ascending method. When the solvent front rises to about 80 mm from the starting line, take out the filter paper, blow dry, and compare the spot size and fluorescence intensity of 2-hydroxy-3-naphthoic acid in the standard and sample under the UV analyzer to calculate the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage content of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Where: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthophenol AS-D sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthophenol AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-theocarboxylic acid standard solution is added at each of 1, 2, 3, 4, and 5. The concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of phenol AS-D sample solution is added at each of A, B, C, D, and E.
Note: When UV analyzer is not used, the colorimetric method of GB/T1652 can be used for verification. 4.7 Determination of fineness
It is carried out in accordance with the relevant provisions of GB/T2383. A standard sieve with an aperture of 250 μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items. Except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Inspection by the manufacturer
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meet the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User Acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples including the upper, middle and lower parts. The sampling volume shall not be less than 500g. The sample shall be carefully mixed and placed in two clean and dry glass bottles with ground stoppers and sealed with paraffin. A label is attached to the bottle, indicating: the manufacturer's name, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference. 5.5 Re-inspection
If one of the indicators in the inspection result does not meet the requirements of this standard, a sample should be taken from the twice amount of packaging for re-inspection. If only one of the indicators in the re-inspection does not meet the requirements of this standard, the whole batch of Naphthophenol AS-D is unqualified. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be determined by negotiation between the two parties. During arbitration, arbitration analysis should be conducted in accordance with the test methods specified in this standard.
Wbzsoso，cOn6 Marking, packaging, transportation and storagebZxz.net
6.1 Marking
HG/T2668-95
The outer packaging of Naphthophenol AS-D should be painted with a firm mark indicating: the manufacturer's name, product name, registered trademark, product grade, batch number, production date and net weight.
Each batch of packaged products shall be accompanied by a quality certificate. The certificate shall include: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that product quality meets the requirements of this standard and the standard number. 6.2 Packaging
Naphthophenol AS-D is packaged in sacks, woven bags or iron barrels lined with plastic bags, with a net weight of 25kg or 50kg per bag (barrel). 6.3 Transportation
Do not approach fire during transportation. Be careful when handling and avoid heavy pressure to avoid damage to the packaging. 6.4 Storage
Naphthophenol AS-D should be stored in a clean, dry and ventilated warehouse, away from fire sources, and prevent from heat and moisture. Additional remarks:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of Shenyang Chemical Research Institute of the Ministry of Chemical Industry, and this standard is drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dyestuff Chemical Factory No. 9. The main drafters of this standard are Wang Qiongxuan, Ding Meifang and Ding Lingying. From the date of implementation of this standard, the original national standard GB/T1654-79 "Naphthophenol AS-D" will be invalid. 7
W.5 Determination of insoluble matter in alkali solution
According to the method for determination of alkali insoluble matter in phenol in Article 3 of GB/T2381. 4.6 Determination of 2-hydroxy-3-naphthoic acid content 4.6.1 Principle of the method
Use the difference in relative affinity of each component molecule in the analyzed substance to the mobile phase and the stationary phase to separate the components, and use the reference standard as a reference to determine the impurity content.
4.6.2 Instruments and materials
Square chromatography cylinder: height 175mm, length 300mm, width 175mm; micro syringe: 1μL;
Xinhua chromatography filter paper: No. 1,
UV analyzer: 254nm.
4.6.3 Reagents and solutions
Absolute ethanol (GB/T678);
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: refined product. Recrystallize the industrial product from ethanol twice, and check with paper chromatography to see if there are other impurities. Preparation of the standard series of 2-hydroxy-3-naphthoic acid solutions: weigh 0.25g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 50mL volumetric flask, and dilute it to the mark with anhydrous ethanol. Use a 1mL graduated pipette to pipette 0.2, 0.4, 0.6, 0.8, and 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each with anhydrous ethanol to the mark, that is, prepare 1, 2, 3, 4, and 5mg/100mL solutions.
Preparation of 10g/100mL Naphthophenol AS-D sample solution: Weigh 1.0g Naphthophenol AS-D and dissolve it in 10mL N,N-dimethylformamide.
Developing agent: ethanol + water = 1 + 3 (V/v)
4.6.4 Determination steps
Take a 160mm, 220mm wide chromatography filter paper, lightly draw a line with a pencil 25mm from the bottom, and make a dot every 2cm on the line with a pencil. At the pencil dot, use a micro syringe to apply 1mL of Naphthophenol AS-D sample solution and 2-hydroxy-3-naphthoic acid standard solution respectively, as shown in Figure 2, blow dry, put it into the chromatography cylinder, and develop it by the ascending method. When the solvent front rises to about 80 mm from the starting line, take out the filter paper, blow dry, and compare the spot size and fluorescence intensity of 2-hydroxy-3-naphthoic acid in the standard and sample under the UV analyzer to calculate the content of 2-hydroxy-3-naphthoic acid.
4.6.5 Calculation
The mass percentage content of 2-hydroxy-3-naphthoic acid (X2) is calculated according to formula (2): 1×100
Where: c1——concentration of 2-hydroxy-3-naphthoic acid standard solution, mg/100mL C2——concentration of naphthophenol AS-D sample solution, mg/100mL. The schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid in naphthophenol AS-D is shown in Figure 2. (2)
Wbzsoso，cOHG/T2668—95
In Figure 2, 1 mL of 2-hydroxy-3-theocarboxylic acid standard solution is added at each of 1, 2, 3, 4, and 5. The concentration 1 represents 1 mg/100 mL, 2 represents 2 mg/100 mL, and so on. 1 mL of phenol AS-D sample solution is added at each of A, B, C, D, and E.
Note: When UV analyzer is not used, the color development method of GB/T1652 can be used for verification. 4.7 Determination of fineness
It is carried out in accordance with the relevant provisions of GB/T2383. A standard sieve with an aperture of 250 μm is used for determination. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are type inspection items. Except for item (6) which is inspected once a month, the remaining items are factory inspection items.
5.2 Inspection by the manufacturer
Naphthophenol AS-D shall be inspected by the inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all Naphthophenol AS-D shipped out of the factory meet the requirements of this standard. Each batch of Naphthophenol AS-D shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.3 User Acceptance
The user unit has the right to inspect the received Naphthophenol AS-D in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method
Take samples from 10% bags (or barrels) of each batch (a batch of uniform products). For small batches, the number shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples including the upper, middle and lower parts. The sampling volume shall not be less than 500g. The sample sh
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