Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2747—1996
Published on April 8, 1996
Implemented on January 1, 1997
Published by the Ministry of Chemical Industry of the People's Republic of China WHG/T2747—1996
This standard is revised on the basis of the original standard HG/T2—378—80. Since the format and expression rules of the original standard do not meet the requirements of GB/T1.1—1993, it is compiled in accordance with the provisions of the new standard. The original standard about "the color light generated by coupling with scarlet salt R on cotton fiber" was changed to scarlet base RC after experimental verification because scarlet salt R is not stable enough, and the dyeing strength item was added. Through the revision of this standard, it is made more standardized and conducive to implementation and improvement of product quality. From the date of implementation, this standard will replace HG/T2—378—80 at the same time. 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. This standard was jointly drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry and Shanghai Dyeing and Chemical Factory No. 9. The main drafters of this standard are Li Chunmei and Ding Meifang. This standard was first issued in 1966 and revised for the first time in 1980.
W.bzsoso.cOm1Scope
Chemical Industry Standard of the People's Republic of China
HG/T2747-1996
Replaces HG/T2-378-80
This standard specifies the requirements, sampling, test methods, inspection rules, and marking, packaging, transportation and storage requirements for naphthol AS-OL.
This standard applies to naphthol AS-OL prepared by condensation of 2-hydroxy-3-naphthoic acid and o-aminoanisole. It is mainly used for dyeing, printing and pigment production of cotton fibers.
Structural formula:
Molecular formula: C18H15OsN
Relative molecular mass: 293.32 (according to the 1991 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601-88 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB2374-94 General conditions for dye staining determination GB/T2381-94 Determination method for insoluble matter content in dyes GB/T2383-80 Determination method for sieving fineness in dyes GB/T2384-92 General method for determination of melting point range of dye intermediates 3 Requirements
3.1 Appearance: Beige brown uniform powder.
3.2 The quality index of chromophore AS-OL shall meet the requirements of Table 1. Table 1 Quality indicators of Naphthophenol AS-OL
Naphthophenol AS-OL content, %
Initial melting point of dry product, ℃
2-Hydroxy-3-naphthoic acid content, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 8, 1996
Implementation on January 1, 1997
W.bzsoso,comContent of insoluble matter in alkali solution, %
HG/T2747-1996
Continued Table 1 (end)
Dyeing intensity of RC-coupled dyeing with scarlet base on cotton fiber (with standard product)Dyeing intensity of RC-coupled dyeing with scarlet base on cotton fiber (with standard product)Fineness (residue passing through 0.28mm sieve), %Note:
Content and melting point of Naphthophenol AS-OL used for dyeing are not measured. Color and intensity of Naphthophenol AS-OL used for pigment production are not required to be measured. 4 Sampling
Approximately~micro
100±5
Sampling is done from 10% bags (or barrels) of each batch (with homogeneous products as one batch), and the number of small batches shall not be less than 3 bags (or barrels). When sampling, use a probe to take samples including the upper, middle and lower parts, and the sampling volume shall not be less than 500g. The sample is carefully mixed and placed in two clean and dry glass bottles with ground stoppers. Seal with paraffin wax, and label the bottles with: manufacturer name, product name, batch and sampling date. One bottle is used for inspection, and one bottle is kept for future reference.
5 Test method
5.1 Appearance
Visual assessment is adopted.
5.2 Determination of the content of phenol AS-OL
5.2.1 Principle of the method
As phenol AS-OL is a weakly acidic compound. In the presence of ethanol, it is dissolved with an excess of alkali and titrated potentiometrically with a standard hydrochloric acid titration solution. The content of phenol AS-OL can be determined by determining the total alkali and free alkali. 5.2.2 Reagents and instruments
5.2.2.1 Reagents
Absolute ethanol;
Sodium hydroxide: 100g/L solution,
Hydrochloric acid:℃ (HCI) = 0.1mol/L standard titration solution, prepared and calibrated according to the relevant provisions of GB/T601. 5.2.2.2 Instruments
Potentiometric titrator (or acidity meter): measuring range 0~14pH, minimum division of meter 0.1pH, accuracy ±0.1pH/3pH: glass electrode: type 231;
calomel electrode: type 232.
The instrument shall be installed as shown in Figure 1.
bzsoso，cOHG/T2747—1996
1 burette, 2—calomel electrode; 3—glass electrode, 4—rubber electrode, 5—glass titration cup, 6—electromagnetic stirring rod Figure 1 Potentiometric titration apparatus
5.2.3 Determination steps
Weigh 0.8g (accurate to 0.0002g) of the naphthol AS-0OL sample and place it in a glass titration cup. Add 10mL of anhydrous ethanol, put in an electromagnetic stirring rod, cover with a stopper, start the electromagnetic stirrer, and after the naphthol AS-OL is fully wetted, add 1.1mL of 100g/L 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 1.03.0mL when determining the free alkali). Cover with a 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 solution. At one pH value (about pH13.50) before the free alkali titration endpoint, gradually add hydrochloric acid standard titration solution in batches, drip about 0.1mL each time, and record the corresponding pH value and the number 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. Record the number of milliliters of 0.1mol/L hydrochloric acid standard titration solution consumed V1, continue titration, when titrated to about pH9 (i.e., about 1.5 pH values away from the titration endpoint of total alkalinity), drip hydrochloric acid standard titration solution in batches, one drop each time, and record the corresponding pH value and the number of milliliters of hydrochloric acid standard titration solution at the same time. When the difference between the two pH values reaches the maximum, it is the total alkali titration endpoint (about pH7.7). Record the number of 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 100g/L sodium hydroxide solution. Install the instrument according to Figure 1. When the titration reaches pH 10.50, add 0.1mol/L hydrochloric acid standard titration solution in batches, one drop at a time, and record the pH value and the number of milliliters of hydrochloric acid standard titration solution consumed. Add the solution gradually until the pH value is below 4. There is a sudden jump near pH 8 and pH 5. The difference in the number of milliliters of hydrochloric acid standard titration solution consumed between the two sudden jumps is 4V, which is the blank value. 5.2.4 Expression of analytical results
The mass percentage of the content of phenol AS-OL is represented by X1 and calculated according to formula (1):3
WHG/T2747—1996
Xi= (V2-V1-AV) X0. 293 3
Wherein: c——concentration of hydrochloric acid standard titration solution, mol/L; K100
V1—volume of 0.1mol/L hydrochloric acid standard titration solution consumed in titration of free alkali, mL; V2—volume of 0.1mol/L hydrochloric acid standard titration solution consumed in titration of total alkali, mL; AV—volume of 0.1mol/L hydrochloric acid standard titration solution consumed in blank test, mL; m——mass of sample, g;
0.2933—mass of naphthol AS-0L expressed in grams equivalent to 1.00mL hydrochloric acid standard titration solution [c(HCI)=1.000mol/L].
5.2.5 Allowable difference
The difference between two parallel determination results shall not exceed 0.5%, and the arithmetic mean shall be taken as the determination result. 5.3 Determination of initial melting point of dry product
Carry out in accordance with the relevant provisions of GB/T2384.
5.4 Determination of 2-hydroxy-3-naphthoic acid content 5.4.1 Principle of the method
Use paper chromatography to separate the components by utilizing the difference in relative affinity of each group of molecules in the substance being analyzed to the mobile phase and the stationary phase, and use the reference standard as a control to determine the impurity content. 5.4.2 Instruments and materials
Square chromatography cylinder or round specimen cylinder;
Micro syringe: 1μL,
Chromatographic filter paper: No. 1;
Ultraviolet analyzer: 254nm.
5.4.3 Reagents and solutions
Absolute ethanol;
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: Refined product, the industrial product is recrystallized twice from ethanol, and there should be no other impurities when checked by paper chromatography. Preparation of 2-hydroxy-3-naphthoic acid standard series solutions: Weigh 0.125g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it into a 250mL volumetric flask, dilute it to the mark with anhydrous ethanol, and then 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, dilute them to the mark with anhydrous ethanol, and prepare standard solutions with 2-hydroxy-3-naphthoic acid contents of 0.1%, 0.2%, 0.3%, 0.4%, and 0.5% in Naphthophenol AS-0L. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g of Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing agent: ethanol + water = 1 + 3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm from the bottom, and use a pencil to dot a point every 2cm on the line. At the pencil point, use a micro-syringe to dot 1μL of the chromatin AS-OL 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 front edge of the solution rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard under the ultraviolet analyzer. When they are consistent, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
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HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the phenol AS-0L standard sample and test sample respectively, place them in a 600mL beaker, add 1.5mL of 95% ethanol to make a uniform slurry, then add 0.5mL of 350g/L sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution and dissolve it completely. Then add 0.5mL of 30% formaldehyde solution, let it stand for 10min, transfer it to a 500mL volumetric flask, and dilute to the scale with Turkey red oil alkali solution. In 5 300mL dye vats, prepare the primer solution according to the provisions of Table 2: 5
W. Dye vat number
1g/500mL standard sample solution
1g/500mL test sample solution
Add Turkey red oil alkali solution
Bath ratio: 1:20 (Cotton bath ratio 1:40) 5.6.3.2 Primer operation
HG/T2747—1996
Table 2 Preparation of primer solution
Adjust the temperature of the primer solution To 40℃, immerse five skeins of cotton yarn (or cotton cloth) each weighing 5g in the primer in the order of number, turn it over frequently to ensure uniform absorption, maintain the primer temperature at 35~40℃, primer for 30 minutes, take it out and wring it evenly to make the moisture content 90%~100% (if it is cotton cloth, it should be rolled dry on the roller dyeing machine after taking it out to make the moisture content 90%~100%, but the roller should be wiped with AS-OL alkaline solution before roller dyeing), then quickly develop color (the weight of the cloth sample is 10g during arbitration). 5.6.3.3 Preparation of color developing solution
Weigh 1g of scarlet base RC (accurate to 0.04g), place it in a 1000mL beaker, add a small amount of distilled water to make it into a slurry, then add 2mL of 350g/L hydrochloric acid and 30mL of distilled water to dissolve it. If it does not dissolve, heat it until it dissolves. After cooling to room temperature, add ice cubes to adjust the temperature to about 5~10℃. While stirring, add 5mL of 100g/L sodium nitrite solution to carry out diazotization reaction. The diazotization time is 30min. Use about 10mL of 200g/L sodium acetate to adjust the pH to 4~5, and then dilute to 1000mL. 5.6.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 1000mL of color development solution at the same time, stir frequently, keep the solution temperature at 10-15℃, color development for 30min, take out and wring dry, wash, boil in 1000mL of soap solution, take out and wash, wring dry, dry at 60-70℃, cool to room temperature and then visually evaluate.
The evaluation of color and intensity of dyeing shall be carried out in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation shall be ±5%. 5.7 Determination of fineness
It shall be carried out in accordance with the provisions of GB/T2383.
6 Inspection plan
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
Naphthophenol AS-OL shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-OL cannot be accepted. 6.4 User Acceptance
The user has the right to inspect the received Naphthophenol AS-OL in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
7 Marking, packaging, transportation and storage
7.1 Marking
Wbzsoso.cOnHG/T2747—1996
The outer packaging container of Naphthophenol AS-OL should be painted with a firm mark, indicating: manufacturer name, product name, registered trademark, standard number, product batch number, production date and net weight. Each batch of packaged products should be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, batch number, production date, product net weight, proof that the product quality meets the requirements of this standard and this standard number. 7.2 Packaging
Naphthophenol AS-OL is packaged in iron barrels or cardboard barrels lined with plastic bags, with a net weight of 25kg or 50kg per barrel. 7.3 Transportation
Prevent exposure and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 7
W.1 Principle of the method
Use paper chromatography to separate the components by using the difference in relative affinity of each group of molecules in the analyzed substance to the mobile phase and the stationary phase, and use the reference standard as a control to determine the impurity content. 5.4.2 Instruments and materials
Square chromatography cylinder or round specimen cylinder;
Micro syringe: 1μL,
Chromatography filter paper: No. 1;
Ultraviolet analyzer: 254nm.
5.4.3 Reagents and solutions
Absolute ethanol;
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 solutions: Weigh 0.125g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it into a 250mL volumetric flask, dilute it to the mark with anhydrous ethanol, and then 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, dilute them to the mark with anhydrous ethanol, and prepare standard solutions with 2-hydroxy-3-naphthoic acid contents of 0.1%, 0.2%, 0.3%, 0.4%, and 0.5% in Naphthophenol AS-0L. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g of Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing agent: ethanol + water = 1 + 3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm from the bottom, and use a pencil to dot a point every 2cm on the line. At the pencil point, use a micro-syringe to dot 1μL of the chromatin AS-OL 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 front edge of the solution rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard under the ultraviolet analyzer. When they are consistent, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
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HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the standard sample and test sample of Naphthophenol AS-0L, respectively, and place them in a 600mL beaker. Add 1.5mL of 95% ethanol to make a slurry. Then add 0.5mL of 350g/L sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution. After the solution is completely dissolved, add 0.5mL of 30% formaldehyde solution. Let it stand for 10min, transfer it to a 500mL volumetric flask, and dilute to the scale with Turkey red oil alkali solution. In 5 300mL dye vats, prepare the primer solution according to the provisions of Table 2: 5
W. Dye vat number
1g/500mL standard sample solution
1g/500mL test sample solution
Add Turkey red oil alkali solution
Bath ratio: 1:20 (Cotton bath ratio 1:40) 5.6.3.2 Primer operation
HG/T2747—1996
Table 2 Preparation of primer solution
Adjust the temperature of the primer solution To 40℃, immerse five skeins of cotton yarn (or cotton cloth) each weighing 5g in the primer in the order of number, turn it over frequently to ensure uniform absorption, maintain the primer temperature at 35~40℃, primer for 30 minutes, take it out and wring it evenly to make the moisture content 90%~100% (if it is cotton cloth, it should be rolled dry on the roller dyeing machine after taking it out to make the moisture content 90%~100%, but the roller should be scrubbed with AS-OL alkaline solution before roller dyeing), then quickly develop color (the weight of the cloth sample is 10g during arbitration). 5.6.3.3 Preparation of color developing solution
Weigh 1g of scarlet base RC (accurate to 0.04g), place it in a 1000mL beaker, add a small amount of distilled water to make it into a slurry, then add 2mL of 350g/L hydrochloric acid and 30mL of distilled water to dissolve it. If it does not dissolve, heat it until it dissolves. After cooling to room temperature, add ice cubes to adjust the temperature to about 5~10℃. While stirring, add 5mL of 100g/L sodium nitrite solution to carry out diazotization reaction. The diazotization time is 30min. Use about 10mL of 200g/L sodium acetate to adjust the pH to 4~5, and then dilute to 1000mL. 5.6.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 1000mL of color development solution at the same time, stir frequently, keep the liquid temperature at 10-15℃, color development for 30min, take out and wring dry, wash, boil in 1000mL soap solution, take out and wash, wring dry, dry at 60-70℃, cool to room temperature and then visually evaluate.
The evaluation of color and intensity of dyeing shall be carried out in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation is ±5%. 5.7 Determination of fineness
It shall be carried out in accordance with the provisions of GB/T2383.
6 Inspection plan
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
Naphthophenol AS-OL shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-OL cannot be accepted. 6.4 User Acceptance
The user has the right to inspect the received Naphthophenol AS-OL in accordance with the provisions of this standard to check whether it meets the requirements of this standard. bzxZ.net
7 Marking, packaging, transportation and storage
7.1 Marking
Wbzsoso.cOnHG/T2747—1996
The outer packaging container of Naphthophenol AS-OL should be painted with a firm mark, indicating: manufacturer name, product name, registered trademark, standard number, product batch number, production date and net weight. Each batch of packaged products should be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, batch number, production date, product net weight, proof that the product quality meets the requirements of this standard and this standard number. 7.2 Packaging
Naphthophenol AS-OL is packaged in iron barrels or cardboard barrels lined with plastic bags, with a net weight of 25kg or 50kg per barrel. 7.3 Transportation
Prevent exposure and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 7
W.1 Principle of the method
Use paper chromatography to separate the components by using the difference in relative affinity of each group of molecules in the analyzed substance to the mobile phase and the stationary phase, and use the reference standard as a control to determine the impurity content. 5.4.2 Instruments and materials
Square chromatography cylinder or round specimen cylinder;
Micro syringe: 1μL,
Chromatography filter paper: No. 1;
Ultraviolet analyzer: 254nm.
5.4.3 Reagents and solutions
Absolute ethanol;
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 solutions: Weigh 0.125g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it into a 250mL volumetric flask, dilute it to the mark with anhydrous ethanol, and then 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, dilute them to the mark with anhydrous ethanol, and prepare standard solutions with 2-hydroxy-3-naphthoic acid contents of 0.1%, 0.2%, 0.3%, 0.4%, and 0.5% in Naphthophenol AS-0L. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g of Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing agent: ethanol + water = 1 + 3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm from the bottom, and use a pencil to dot a point every 2cm on the line. At the pencil point, use a micro-syringe to dot 1μL of the chromatin AS-OL 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 front edge of the solution rises to about 80mm from the starting line, take out the filter paper, blow dry, and compare the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard under the ultraviolet analyzer. When they are consistent, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
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HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the phenol AS-0L standard sample and test sample respectively, place them in a 600mL beaker, add 1.5mL of 95% ethanol to make a uniform slurry, then add 0.5mL of 350g/L sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution and dissolve it completely. Then add 0.5mL of 30% formaldehyde solution, let it stand for 10min, transfer it to a 500mL volumetric flask, and dilute to the scale with Turkey red oil alkali solution. In 5 300mL dye vats, prepare the primer solution according to the provisions of Table 2: 5
W. Dye vat number
1g/500mL standard sample solution
1g/500mL test sample solution
Add Turkey red oil alkali solution
Bath ratio: 1:20 (Cotton bath ratio 1:40) 5.6.3.2 Primer operation
HG/T2747—1996
Table 2 Preparation of primer solution
Adjust the temperature of the primer solution To 40℃, immerse five skeins of cotton yarn (or cotton cloth) each weighing 5g in the primer in the order of number, turn it over frequently to ensure uniform absorption, maintain the primer temperature at 35~40℃, primer for 30 minutes, take it out and wring it evenly to make the moisture content 90%~100% (if it is cotton cloth, it should be rolled dry on the roller dyeing machine after taking it out to make the moisture content 90%~100%, but the roller should be wiped with AS-OL alkaline solution before roller dyeing), then quickly develop color (the weight of the cloth sample is 10g during arbitration). 5.6.3.3 Preparation of color developing solution
Weigh 1g of scarlet base RC (accurate to 0.04g), place it in a 1000mL beaker, add a small amount of distilled water to make it into a slurry, then add 2mL of 350g/L hydrochloric acid and 30mL of distilled water to dissolve it. If it does not dissolve, heat it until it dissolves. After cooling to room temperature, add ice cubes to adjust the temperature to about 5~10℃. While stirring, add 5mL of 100g/L sodium nitrite solution to carry out diazotization reaction. The diazotization time is 30min. Use about 10mL of 200g/L sodium acetate to adjust the pH to 4~5, and then dilute to 1000mL. 5.6.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 1000mL of color development solution at the same time, stir frequently, keep the solution temperature at 10-15℃, color development for 30min, take out and wring dry, wash, boil in 1000mL of soap solution, take out and wash, wring dry, dry at 60-70℃, cool to room temperature and then visually evaluate.
The evaluation of color and intensity of dyeing shall be carried out in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation is ±5%. 5.7 Determination of fineness
It shall be carried out in accordance with the provisions of GB/T2383.
6 Inspection plan
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
Naphthophenol AS-OL shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-OL cannot be accepted. 6.4 User Acceptance
The user has the right to inspect the received Naphthophenol AS-OL in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
7 Marking, packaging, transportation and storage
7.1 Marking
Wbzsoso.cOnHG/T2747—1996
The outer packaging container of Naphthophenol AS-OL should be painted with a firm mark, indicating: manufacturer name, product name, registered trademark, standard number, product batch number, production date and net weight. Each batch of packaged products should be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, batch number, production date, product net weight, proof that the product quality meets the requirements of this standard and this standard number. 7.2 Packaging
Naphthophenol AS-OL is packaged in iron barrels or cardboard barrels lined with plastic bags, with a net weight of 25kg or 50kg per barrel. 7.3 Transportation
Prevent exposure and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 7
W.3 Reagents and solutions
Absolute ethanol;
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: Refined product, the industrial product is recrystallized from ethanol twice, and there should be no other impurities by paper chromatography. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.125g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it to a 250mL volumetric flask, dilute it to the mark with anhydrous ethanol, and then use a 1mL graduated pipette to draw 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 standard solutions with 2-hydroxy-3-naphthoic acid content of 0.1%, 0.2%, 0.3%, 0.4%, and 0.5% in Naphthophenol AS-0L. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing solvent: ethanol + water = 1+3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm away from the lower end, and use a pencil to dot a point every 2cm on the line. At the pencil points, use a microsyringe to apply 1μL of the chromophore AS-OL sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2. Blow dry, put it into the chromatography cylinder, and develop it using the ascending method. When the front edge of the solution rises to about 80mm from the starting line, take out the filter paper and blow dry. When the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard are consistent under the ultraviolet analyzer, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
W.0
HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the phenol AS-0L standard sample and test sample respectively, place them in a 600mL beaker, add 1.5mL of 95% ethanol to make a uniform slurry, then add 0.5mL of 350g/L sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution and dissolve it completely. Then add 0.5mL of 30% formaldehyde solution, let it stand for 10min, transfer it to a 500mL volumetric flask, and dilute to the scale with Turkey red oil alkali solution. In 5 300mL dye vats, prepare the primer solution according to the provisions of Table 2: 5
W. Dye vat number
1g/500mL standard sample solution
1g/500mL test sample solution
Add Turkey red oil alkali solution
Bath ratio: 1:20 (Cotton bath ratio 1:40) 5.6.3.2 Primer operation
HG/T2747—1996
Table 2 Preparation of primer solution
Adjust the temperature of the primer solution To 40℃, immerse five skeins of cotton yarn (or cotton cloth) each weighing 5g in the primer in the order of number, turn it over frequently to ensure uniform absorption, maintain the primer temperature at 35~40℃, primer for 30 minutes, take it out and wring it evenly to make the moisture content 90%~100% (if it is cotton cloth, it should be rolled dry on the roller dyeing machine after taking it out to make the moisture content 90%~100%, but the roller should be wiped with AS-OL alkaline solution before roller dyeing), then quickly develop color (the weight of the cloth sample is 10g during arbitration). 5.6.3.3 Preparation of color developing solution
Weigh 1g of scarlet base RC (accurate to 0.04g), place it in a 1000mL beaker, add a small amount of distilled water to make it into a slurry, then add 2mL of 350g/L hydrochloric acid and 30mL of distilled water to dissolve it. If it does not dissolve, heat it until it dissolves. After cooling to room temperature, add ice cubes to adjust the temperature to about 5~10℃. While stirring, add 5mL of 100g/L sodium nitrite solution to carry out diazotization reaction. The diazotization time is 30min. Use about 10mL of 200g/L sodium acetate to adjust the pH to 4~5, and then dilute to 1000mL. 5.6.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 1000mL of color development solution at the same time, stir frequently, keep the solution temperature at 10-15℃, color development for 30min, take out and wring dry, wash, boil in 1000mL of soap solution, take out and wash, wring dry, dry at 60-70℃, cool to room temperature and then visually evaluate.
The evaluation of color and intensity of dyeing shall be carried out in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation is ±5%. 5.7 Determination of fineness
It shall be carried out in accordance with the provisions of GB/T2383.
6 Inspection plan
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
Naphthophenol AS-OL shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-OL cannot be accepted. 6.4 User Acceptance
The user has the right to inspect the received Naphthophenol AS-OL in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
7 Marking, packaging, transportation and storage
7.1 Marking
Wbzsoso.cOnHG/T2747—1996
The outer packaging container of Naphthophenol AS-OL should be painted with a firm mark, indicating: manufacturer name, product name, registered trademark, standard number, product batch number, production date and net weight. Each batch of packaged products should be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, batch number, production date, product net weight, proof that the product quality meets the requirements of this standard and this standard number. 7.2 Packaging
Naphthophenol AS-OL is packaged in iron barrels or cardboard barrels lined with plastic bags, with a net weight of 25kg or 50kg per barrel. 7.3 Transportation
Prevent exposure and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 7
W.3 Reagents and solutions
Absolute ethanol;
N,N-dimethylformamide;
2-Hydroxy-3-naphthoic acid: Refined product, the industrial product is recrystallized from ethanol twice, and there should be no other impurities by paper chromatography. Preparation of 2-hydroxy-3-naphthoic acid standard series solution: Weigh 0.125g (accurate to 0.002g) of 2-hydroxy-3-naphthoic acid, dissolve it in anhydrous ethanol, transfer it into a 250mL volumetric flask, dilute it to the mark with anhydrous ethanol, and then use a 1mL graduated pipette to draw 0.2, 0.4, 0.6, 0.8, and 1.0mL of the above solution into five 10mL volumetric flasks, and dilute each of them to the mark with anhydrous ethanol, that is, to prepare standard solutions with 0.1%, 0.2%, 0.3%, 0.4%, and 0.5% of 2-hydroxy-3-naphthoic acid content in Naphthol AS-0L. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing solvent: ethanol + water = 1+3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm away from the lower end, and use a pencil to dot a point every 2cm on the line. At the pencil points, use a microsyringe to apply 1μL of chromophore AS-OL sample solution and 2-hydroxy-3-naphthoic acid standard solution respectively as shown in Figure 2. Blow dry, put into the chromatography cylinder, and develop using the ascending method. When the front edge of the solution rises to about 80mm from the starting line, take out the filter paper and blow dry. When the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard are consistent under the ultraviolet analyzer, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
W.0
HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the phenol AS-0L standard sample and test sample respectively, place them in a 600mL beaker, add 1.5mL of 95% ethanol to make a uniform slurry, then add 0.5mL of 350g/L sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution and dissolve it completely. Then add 0.5mL of 30% formaldehyde solution, let it stand for 10min, transfer it to a 500mL volumetric flask, and dilute to the scale with Turkey red oil alkali solution. In 5 300mL dye vats, prepare the primer solution according to the provisions of Table 2: 5
W. Dye vat number
1g/500mL standard sample solution
1g/500mL test sample solution
Add Turkey red oil alkali solution
Bath ratio: 1:20 (Cotton bath ratio 1:40) 5.6.3.2 Primer operation
HG/T2747—1996
Table 2 Preparation of primer solution
Adjust the temperature of the primer solution To 40℃, immerse five skeins of cotton yarn (or cotton cloth) each weighing 5g in the primer in the order of number, turn it over frequently to ensure uniform absorption, maintain the primer temperature at 35~40℃, primer for 30 minutes, take it out and wring it evenly to make the moisture content 90%~100% (if it is cotton cloth, it should be rolled dry on the roller dyeing machine after taking it out to make the moisture content 90%~100%, but the roller should be wiped with AS-OL alkaline solution before roller dyeing), then quickly develop color (the weight of the cloth sample is 10g during arbitration). 5.6.3.3 Preparation of color developing solution
Weigh 1g of scarlet base RC (accurate to 0.04g), place it in a 1000mL beaker, add a small amount of distilled water to make it into a slurry, then add 2mL of 350g/L hydrochloric acid and 30mL of distilled water to dissolve it. If it does not dissolve, heat it until it dissolves. After cooling to room temperature, add ice cubes to adjust the temperature to about 5~10℃. While stirring, add 5mL of 100g/L sodium nitrite solution to carry out diazotization reaction. The diazotization time is 30min. Use about 10mL of 200g/L sodium acetate to adjust the pH to 4~5, and then dilute to 1000mL. 5.6.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 1000mL of color development solution at the same time, stir frequently, keep the solution temperature at 10-15℃, color development for 30min, take out and wring dry, wash, boil in 1000mL of soap solution, take out and wash, wring dry, dry at 60-70℃, cool to room temperature and then visually evaluate.
The evaluation of color and intensity of dyeing shall be carried out in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation is ±5%. 5.7 Determination of fineness
It shall be carried out in accordance with the provisions of GB/T2383.
6 Inspection plan
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
Naphthophenol AS-OL shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-OL cannot be accepted. 6.4 User Acceptance
The user has the right to inspect the received Naphthophenol AS-OL in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
7 Marking, packaging, transportation and storage
7.1 Marking
Wbzsoso.cOnHG/T2747—1996
The outer packaging container of Naphthophenol AS-OL should be painted with a firm mark, indicating: manufacturer name, product name, registered trademark, standard number, product batch number, production date and net weight. Each batch of packaged products should be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, batch number, production date, product net weight, proof that the product quality meets the requirements of this standard and this standard number. 7.2 Packaging
Naphthophenol AS-OL is packaged in iron barrels or cardboard barrels lined with plastic bags, with a net weight of 25kg or 50kg per barrel. 7.3 Transportation
Prevent exposure and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 7
W.4% and 0.5% standard solutions. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing solvent: ethanol + water = 1+3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm away from the lower end, and use a pencil to dot a point every 2cm on the line. At the pencil points, use a microsyringe to apply 1μL of the chromophore AS-OL sample solution and the 2-hydroxy-3-naphthoic acid standard solution, respectively, as shown in Figure 2. Blow dry, put it into the chromatography cylinder, and develop it using the ascending method. When the front edge of the solution rises to about 80mm from the starting line, take out the filter paper and blow dry. When the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard are consistent under the ultraviolet analyzer, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
W.0
HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the standard sample and test sample of Naphthophenol AS-0L, respectively, and place them in a 600mL beaker. Add 1.5mL of 95% ethanol to make a slurry. Then add 0.5mL of 350g/L sodium hydroxide solution and 1.5mL of water. After the solution is clarified, add 200mL of Turkey red oil alkali solution. After the solution is completely dissolved, add 0.5mL of 30% formaldehyde solution. Let it stand for 10min, transfer it to a 500mL volumetric flask, and dilute to the scale with Turkey red oil alkali solution. In 5 300mL dye vats, prepare the primer solution according to the provisions of Table 2: 5
W. Dye vat number
1g/500mL standard sample solution
1g/500mL test sample solution
Add Turkey red oil alkali solution
Bath ratio: 1:20 (Cotton bath ratio 1:40) 5.6.3.2 Primer operation
HG/T2747—1996
Table 2 Preparation of primer solution
Adjust the temperature of the primer solution To 40℃, immerse five skeins of cotton yarn (or cotton cloth) each weighing 5g in the primer in the order of number, turn it over frequently to ensure uniform absorption, maintain the primer temperature at 35~40℃, primer for 30 minutes, take it out and wring it evenly to make the moisture content 90%~100% (if it is cotton cloth, it should be rolled dry on the roller dyeing machine after taking it out to make the moisture content 90%~100%, but the roller should be scrubbed with AS-OL alkaline solution before roller dyeing), then quickly develop color (the weight of the cloth sample is 10g during arbitration). 5.6.3.3 Preparation of color developing solution
Weigh 1g of scarlet base RC (accurate to 0.04g), place it in a 1000mL beaker, add a small amount of distilled water to make it into a slurry, then add 2mL of 350g/L hydrochloric acid and 30mL of distilled water to dissolve it. If it does not dissolve, heat it until it dissolves. After cooling to room temperature, add ice cubes to adjust the temperature to about 5~10℃. While stirring, add 5mL of 100g/L sodium nitrite solution to carry out diazotization reaction. The diazotization time is 30min. Use about 10mL of 200g/L sodium acetate to adjust the pH to 4~5, and then dilute to 1000mL. 5.6.3.4 Color development operation
Immerse five skeins of cotton yarn (or cotton cloth) that have been primed in 1000mL of color development solution at the same time, stir frequently, keep the liquid temperature at 10-15℃, color development for 30min, take out and wring dry, wash, boil in 1000mL soap solution, take out and wash, wring dry, dry at 60-70℃, cool to room temperature and then visually evaluate.
The evaluation of color and intensity of dyeing shall be carried out in accordance with the provisions of GB2374, and the allowable error of dyeing intensity evaluation is ±5%. 5.7 Determination of fineness
It shall be carried out in accordance with the provisions of GB/T2383.
6 Inspection plan
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
Naphthophenol AS-OL shall be inspected by the quality inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 Re-inspection
If one indicator in the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even only one item does not meet the requirements of this standard, the entire batch of Naphthophenol AS-OL cannot be accepted. 6.4 User Acceptance
The user has the right to inspect the received Naphthophenol AS-OL in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
7 Marking, packaging, transportation and storage
7.1 Marking
Wbzsoso.cOnHG/T2747—1996
The outer packaging container of Naphthophenol AS-OL should be painted with a firm mark, indicating: manufacturer name, product name, registered trademark, standard number, product batch number, production date and net weight. Each batch of packaged products should be accompanied by a quality certificate. The certificate includes: manufacturer name, product name, batch number, production date, product net weight, proof that the product quality meets the requirements of this standard and this standard number. 7.2 Packaging
Naphthophenol AS-OL is packaged in iron barrels or cardboard barrels lined with plastic bags, with a net weight of 25kg or 50kg per barrel. 7.3 Transportation
Prevent exposure and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 7
W.4% and 0.5% standard solutions. 5.4.4 Preparation of 1g/100mL Naphthophenol AS-0L sample solution: Weigh 1g Naphthophenol AS-0L sample and dissolve it in 100mL N,N-dimethylformamide.
5.4.5 Developing solvent: ethanol + water = 1+3 (V/V) 5.4.6 Determination steps
Take a chromatographic filter paper with a length of 160mm and a width of 220mm. Use a pencil to lightly draw a line 25mm away from the lower end, and use a pencil to dot a point every 2cm on the line. At the pencil points, use a microsyringe to apply 1μL of chromophore AS-OL sample solution and 2-hydroxy-3-naphthoic acid standard solution respectively as shown in Figure 2. Blow dry, put into the chromatography cylinder, and develop using the ascending method. When the front edge of the solution rises to about 80mm from the starting line, take out the filter paper and blow dry. When the size and depth of the 2-hydroxy-3-naphthoic acid spots in the sample and the standard are consistent under the ultraviolet analyzer, the content of 2-hydroxy-3-naphthoic acid can be determined. The schematic diagram of the paper chromatography of 2-hydroxy-3-naphthoic acid in Naphthoic Acid AS-OL is shown in Figure 2. 4
W.0
HG/T2747—1996
At 1, 2, 3, 4, and 5 in the figure, 1 μL of 2-hydroxy-3-naphthoic acid standard solution is added, and its content 1 represents 0.1%, 2 represents 0.2%, and so on. At A, B, C, D, and E, 1 μL of Naphthoic Acid AS-OL sample solution is added.
Figure 2 Schematic diagram of paper chromatography of 2-hydroxy-3-naphthoic acid 5.5 Determination of the content of insoluble matter in alkali solution
The determination method of alkali-insoluble matter in Naphthoic Acid in GB/T2381—94 is used. 5.6 Determination of color shade and intensity of dyeing on cotton fiber with scarlet RC 5.6.1 Principle of the method
The AS-OL sample and standard sample are coupled with scarlet RC diazonium salt solution on cotton fiber respectively, and the color shade and intensity of the color generated on the cotton fiber are visually compared. 5.6.2 Reagents and solutions
95% ethanol, chemically pure;
Sodium hydroxide, chemically pure, 350g/L solution; Hydrochloric acid, chemically pure, 350g/L solution
Formaldehyde solution, chemically pure, 30% solution
Red base RC industrial product,
Anhydrous sodium carbonate, chemically pure;
Anhydrous sodium acetate, chemically pure, 200g/L solution; Sodium nitrite, chemically pure, 100g/L solution; Neutral soap industrial product, containing 60% fatty acids;
Turkish red oil industrial product, 40%,
Turkish red oil alkali solution: Take 20mL of 40% Turkish red oil, add 10mL of 350g/L sodium hydroxide solution, and dilute to 1000mL with distilled water.
Soap solution: 5g soap flakes and 3g sodium carbonate are dissolved in 1000mL water. 5.6.3 Determination steps
5.6.3.1 Preparation of primer
Accurately weigh 1g (accurate to 0.001g) of the phenol AS-0L standard sample and
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