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Chemical Industry Standard of the People's Republic of China
HG2280-92
Published on June 1, 1992wwW.bzxz.Net
Implemented on January 1, 1993
Ministry of Chemical Industry of the People's Republic of China
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG2280-92
This standard specifies the technical requirements, test methods, inspection rules and packaging, marking, storage and transportation requirements for Naphthol AS-G. This standard applies to Naphthol AS-G prepared by condensation of 3,3'-dimethylbenzylamine and diketene. This product is mainly used for dyeing and printing of cotton fibers and in the coating and organic pigment industries. Molecular formula: C2H2/N204
Structural formula:
H:COCH,COCHN
-NHCOCH,COCH:
Relative molecular mass: 380.42 (according to the international relative atomic mass in 1989)2
Cited standards
Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagentsGeneral rules for sampling of chemical products
GB6678
GB6679
General rules for sampling of solid chemical products
GB2374
GB2381
3 Technical requirements
General conditions for dye staining determination
Determination method of insoluble matter content in dyes
Naphthol AS-G shall comply with the provisions of Table 1.
Naphthophenol AS-G content, %
The intensity of the color light generated by coupling with scarlet base G diazonium salt on cotton fiber, alkali-insoluble matter content, %
Test method
4.1 Appearance
Determine by visual method.
Approved by the Ministry of Chemical Industry of the People's Republic of China on 1992-06-01>
First-class product
Qualified product
Beige to light gray uniform powder
Similar to the standard product~slightly
100% of the standard product
Implemented on 1993-01-01
4.2 Determination of the content of phenol AS-G
4.2.1 Principle
HG2280—92
Nanophenol AS-G is hydrolyzed under acidic conditions to generate 3,3'-dimethylbenzidine, which is then quantitatively diazotized with sodium nitrite under acidic conditions. Excess sodium nitrite is detected by iodide ion to determine the end point. 4.2.2 Reagents and solutions
4.2.2.1 95% ethanol (GB679): chemically pure; 4.2.2.2 Hydrochloric acid (GB622) solution: 1+1; 4.2.2.3 Potassium bromide (GB649) solution: 100g/L 4.2.2.4 Sodium hydroxide (GB629) solution: chemically pure, 350g/L; 4.2.2.5
Sodium nitrite (GB633) standard titration solution: c (NaNO?) = 0.1mol/L Prepared according to the requirements of GB601, the end point of calibration is tested with potassium iodide starch test paper.
4.2.2.6 Potassium iodide starch test paper: Prepared according to 4.2.3 of GB603. 4.2.3 Determination steps
Weigh about 0.5g (accurate to 0.0002g) of the naphthol AS-G sample and place it in a 250mL ground-mouth conical flask. Add 4mL of ethanol (4.2.2.1) and 0.3mL of sodium hydroxide solution (4.2.2.4). After heating to dissolve, add 50mL of hydrochloric acid solution (4.2.2.2), connect a condenser, and heat under reflux until the solution is completely clear. Rinse the condenser with 50mL of distilled water, transfer the solution into a 400mL beaker, and wash the conical flask twice with 100mL of distilled water. Combine the washing liquid into a beaker, add 15 mL of potassium bromide solution (4.2.2.3), dilute with ice water to a total volume of 300 mL, maintain 5-10 °C, and titrate with sodium nitrite standard titration solution (4.2.2.5) until the test solution turns light blue on the potassium iodide starch test paper (4.2.2.6). After 5 minutes, use the same method to test. If it still turns light blue, it is the end point. Perform a blank test under the same conditions. The mass percentage content (X) of chromophore AS-G is calculated according to formula (1): _(VV)·c×0.1902×100
Wherein:
V1—the volume of sodium nitrite standard titration solution consumed in titration, mL; V. The volume of sodium nitrite standard titration solution consumed in the blank test, mL; the actual concentration of sodium nitrite standard titration solution, mol/L; m—the mass of the sample of naphthoic acid AS-G, g;
0.1092——the mass of naphthoic acid AS-G expressed in grams equivalent to 1.00mL sodium nitrite standard titration solution Cc(NaNO2)=1.000mol/L).
The calculation result is rounded to two decimal places. The difference between the two parallel determination results is not greater than 0.3%, and the arithmetic mean of the parallel determination results is taken as the determination result.
4.3 Determination of the color light and intensity generated by coupling with scarlet base G diazonium salt on cotton fiber 4.3.1 Reagents and solutions
4.3.1.1 95% ethanol (GB679): chemically pure; 4.3.1.2 Anhydrous sodium carbonate (GB639): chemically pure; 4.3.1.3 Hydrochloric acid (GB622) solution: 1+1; 4.3.1.4 Sodium hydroxide (GB629) solution: chemically pure, 350g/L; 4.3.1.5
Sodium nitrite (GB633) solution: chemically pure, 100g/L; 4.3.1.6
Sodium acetate (GB693) solution: chemically pure, 100g/L; 4. 3. 1.7
Sodium chloride (GB1266) solution: 100g/L; 4.3.1.8
Glacial acetic acid (GB676) solution: 100g/L: Turkey red oil alkali solution: measure 20mL of Turkey red oil (industrial product, 50%) and 3mL of sodium hydroxide solution, dilute to 1000mL with distilled water;
Soap solution: 5g of neutral soap (industrial product, containing 60% fatty acids) and 3g of anhydrous sodium carbonate, dissolve in 1000mL of distilled water. 2
4.3.2 Determination steps
4.3.2.1 Preparation of primer
HG2280—92
Accurately weigh 1.000g of each of the sample and standard of Naphthophenol AS-G, place them in 500mL beakers, add 2mL of ethanol (4.3.1.1), mix into slurry, add 0.6mL of sodium hydroxide solution (4.3.1.4), mix thoroughly to dissolve the sample completely, and then dilute to 500mL with Turkey red oil alkali solution (4.3.1.9).
Put them in 4 300mL dye vats and prepare primer according to the requirements of Table 2. Table 2
Composition of primer
1g/500mL sample solution
1g/500mL standard solution
Turkish red oil alkali solution
Bath ratio: 1:20
4.3.2.2 Primer operation
Dyeing vat number
Sequentially immerse four skeins of dry cotton yarn (or cotton cloth) weighing 10g each into the primer solution, stir frequently, keep the primer temperature at 25-30℃, and prime for 30 minutes. Take out the cotton yarn and wring it evenly to make the moisture content 90%-100% (if it is cotton cloth, it should be rolled evenly on the pad dyeing machine after taking it out, and the moisture content should be 90%-100%, but the roller should be rinsed with phenol AS-G alkali solution before pad dyeing), and then quickly develop color.
4.3.2.3 Preparation of color developing solution
Weigh about 1g (accurate to 0.0002g) of scarlet base G and place it in a 1000mL beaker. Add 4mL of hydrochloric acid solution (4.3.1.3) to make a slurry. Add a small amount of boiling distilled water and stir thoroughly to dissolve it completely (heat it in a water bath if necessary). Add 40mL of distilled water and cool it in an ice water bath to maintain 5-10℃. Add sodium nitrite solution while stirring. (4.3.1.5) 6mL, diazotize for 20min (the solution after diazotization should be slightly blue when tested with potassium iodide starch paper, and blue when tested with Congo red paper) and neutralize with 10mL sodium acetate solution (4.3.1.6), then add 80mL sodium chloride solution (4.3.1.7), 40mL sodium acetate solution (4.3.1.6) and 20mL glacial acetic acid solution (4.3.1.8), and finally dilute to 800mL with distilled water.
4.3.2.4 Color development operation
Immerse four skeins of cotton yarn (or cotton cloth) that have been primed in the color development solution at the same time, stir frequently, maintain the temperature at 25-30℃, color for 30min, take out and wring dry, wash, and soak in soap solution (4.3.1.10) (bath ratio 1:20) and boil for 10 minutes, take out and wash with clean water, wring dry, place in 60-70℃ oven to dry or air dry, and then visually identify. 4.4 Determination of alkali-insoluble content
The determination of alkali-insoluble content shall be carried out in accordance with the provisions of Chapter 3 of GB2381. 5 Inspection rules
5.1 Inspection classification
All items specified in Table 1 are factory inspection items. 5.2 Factory inspection
Naphthophenol AS-G shall be inspected by the technical inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all Naphthophenol AS-G shipped out of the factory meet the requirements of this standard, and each batch of Naphthophenol AS-G 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-G in accordance with the requirements of this standard to check whether it meets the requirements of this standard. 5.4 Sampling method
Determine the number of sampling units according to the provisions of GB6678. When sampling, use a probe to take equal amounts of samples from the top, middle and bottom of the opened barrel. The total amount of 3 samples shall not be less than 500g. Mix the samples carefully and divide them into two clean, dry, wide-mouth bottles with ground stoppers and seal them with paraffin. Paste 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 reference. 5.5 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, a sample of Naphthophenol AS-G should be selected from twice the amount of packaging for re-inspection. If the results of the re-inspection show that even if only one indicator does not meet the requirements of this standard, the entire batch of Naphthophenol AS-G cannot be accepted. 5.6 Arbitration
When the supply and demand parties have disputes over product quality and cannot be resolved through negotiation, arbitration verification shall be conducted by an arbitration institution agreed upon by both parties. During arbitration, arbitration analysis shall be conducted in accordance with the test methods specified in this standard. 6 Packaging, marking, purchase, storage and transportation
6.1 Naphthophenol AS-G is packaged in iron barrels lined with plastic bags, with a net weight of 20kg or 25kg per barrel. 6.2 The outer packaging should be painted with a firm mark indicating the manufacturer's name, product name, trademark, standard number, quality grade, production date, batch number and net weight.
6.3 Each batch of packaged finished products shall be accompanied by a quality certificate in a certain format and the words that the product quality meets the requirements of this standard. 6.4 Naphthophenol AS-G should be stored in a dry and ventilated place to avoid sunlight. During transportation, handle with care to prevent heat and moisture. Additional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry and Nantong Acetic Acid Chemical Plant. The main drafters of this standard are Yang Jiemin, Xuan Weicheng and Tan Jianong.
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