Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2897—1997
1-Naphthol-4-sulfonic acid
l-Naphthol-4-sulfonicacid
(Neville and Winter'sacid)
Published on April 22, 1997
Ministry of Chemical Industry of the People's Republic of China
Implemented on October 1, 1997
WHG/T2897—1997
This standard is revised on the basis of HG/T2-811-75 "1-Naphthol-4-sulfonic acid". With reference to relevant foreign standards and combined with the actual situation of domestic production and users of this product, in this revision, the analysis of 1-naphthol-4-sulfonic acid content is changed from nitrosation method to coupling method, and the index of dry product is added. According to the requirements of GB/T1.1-1993, the writing format of the standard is modified. Appendix A of this standard is the appendix of the standard.
This standard shall replace HG/T2-811-75 from the date of entry into force. 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 Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was jointly drafted by Tianjin Yazhong Chemical Factory and Shenyang Institute of Chemical Industry. The main drafters of this standard are Chen Yaqing, Geng Guomin and Liu Jinlan. This standard was first issued in 1975.
WW.bzsoso.cOmFree download of American standard industry dataICS71.100.01
Registration No. 433—1997
Chemical Industry Standard of the People's Republic of China
1-Naphthol-4-sulfonic acid
1-Naphthol-4-sulfonic acid
(Neville and Winter's acid)
1Scope
HG/T2897—1997
Replaces ZB/T2-811—75
This standard specifies the requirements, sampling, test methods, inspection rules and marking, packaging, transportation and storage requirements for 1-naphthol-4-sulfonic acid.
This standard applies to 1-naphthol-4-sulfonic acid prepared by addition and hydrolysis of 1-naphthylamine-4-sulfonic acid. This product is mainly used in the dye industry.
Structural formula:
Molecular formula: C1oHO,S
Relative molecular mass: 224.17 (according to the 1991 International Relative Atomic Mass) 2 Referenced 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 GB/T603-88 Preparation of preparations and products used in chemical reagent test methods GB/T6682-92 Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987) 3 Requirements
The quality of 1-naphthol-4-sulfonic acid shall comply with the provisions of Table 1. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 22, 1997 and implemented on October 1, 1997
W.bzsoso.cOmAppearance
1-Naphthol-4-sulfonic acid content, %
HG/T2897-1997
Table 11 Technical requirements for 1-naphthol-4-sulfonic acid
Light yellow powder
1-naphthylamine-4-sulfonic acid content (based on 100% 1-naphthol-4-sulfonic acid), %Sulfur oxide content, %
4Sampling
Paste
White to light yellow paste
Select 10% of the barrels (bags) from each batch of products for sampling. For small batches, not less than 3 barrels (bags) shall be taken (the number of paste samples is 100%). When sampling, insert a stainless steel sampler vertically into the bottom of the barrel (bag), take the sample from top to bottom, put it in a sugar porcelain plate, mix the sample carefully, select no less than 500g of sample, and divide it into two clean and dry wide-mouth bottles with ground mouths. Paste labels, indicate the manufacturer's name, product name, batch number and sampling date, one bottle for inspection, and one bottle for future reference. 5 Test method
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and the third-grade water specifications in GB/T6682. The standard solutions, preparations and products required in this standard, unless otherwise specified, are prepared in accordance with the provisions of GB/T601 and GB/T603.
5.1 AppearanceWww.bzxZ.net
Visual determination is adopted.
5.2 Determination of 1-naphthol-4-sulfonic acid content
5.2.1 Principle of the method:
1-naphthol-4-sulfonic acid and aromatic primary amine diazonium salt undergo quantitative coupling reaction to generate azo compounds. The end point of the reaction is tested by the color displayed at the intersection of the moist circles on the filter paper. 5.2.2 Reagents and solutions
Sodium nitrite: c(NaNO2)=0.2mol/L standard titration solution, prepared and calibrated according to the provisions of GB/T601, but starch-potassium iodide test paper is used for endpoint judgment,
Hydrochloric acid solution: 1+1, 1+4;
Anhydrous sodium carbonate solution: 100g/L;
Congo red test paper, starch potassium iodide test paper; Industrial p-nitroaniline: content 99%;
H acid indicator solution: weigh 0.5g of powdered H acid industrial product and dissolve it in 100mL50g/L sodium carbonate solution: Filter paper: medium-speed qualitative filter paper.
5.2.3 Preparation and calibration of p-nitroaniline diazonium salt [c(CcH4NO2Cl)=0.04mol/L] standard titration solution 5.2.3.1 Preparation of p-nitroaniline hydrochloride [c(CHN202Cl)=0.2mol/L] solution: Weigh 27.7g of p-nitroaniline that has been ground in advance into a 500mL beaker, add 100mL of water while stirring, adjust to a paste, then add 180mL of 1+1 hydrochloric acid, heat and stir to dissolve, let stand for 8-12h until all p-nitroaniline hydrochloride is converted, filter with a G2 filter, then transfer the filtrate into a 1000mL volumetric flask and dilute to the mark with water. 2
W.bzsoso，cOnHG/T2897—1997
5.2.3.2 Standardization of p-nitroaniline hydrochloride [c(CHzN202C1)=0.2mol/L] solution Take 25mL of the above prepared solution, transfer it into a 400mL beaker, add 100mL of 1+4 hydrochloric acid solution, and cool to 0~5℃. Titrate with 0.2mol/L sodium nitrite standard solution at 0~5℃, and check the end point with starch potassium iodide test paper. After a drop of titration solution is added, take a drop of the titrated solution, which will show a slight blue color on the starch potassium iodide test paper. After 5 minutes, use the same method to check, and it will still show a slight blue color, which is the end point. Perform a blank test at the same time. The concentration c2 of p-nitroaniline hydrochloride solution is calculated according to formula (1): _ci (Vi-V2)
Where: c1——concentration of sodium nitrite standard solution, mol/LVi——volume of sodium nitrite standard solution consumed, mLV2——volume of sodium nitrite standard solution consumed in blank titration, mL. 5.2.3.3 Preparation of p-nitroaniline diazonium salt [c(CH,N3O2C1)=0.04mol/L] standard titration solution (1)
Pull 50mL of 0.2mol/L p-nitroaniline hydrochloride solution into a 250mL brown volumetric flask, add 30mL of 1+1 hydrochloric acid, 20g of ice chips prepared with distilled water, and use a burette to add the calculated amount of 0.2mol/L sodium nitrite standard solution at a time. The solution is slightly blue when tested with starch potassium iodide paper. After 5 minutes, it is still slightly blue when tested with the same method. Then add 0.1mL of sodium nitrite standard solution. Then dilute to the mark with ice water and place in an ice bath in a dark place for later use. The standard solution is prepared freshly when used. The concentration of the p-nitroaniline diazonium salt standard solution is calculated according to formula (2): C2×25
Wherein: cs——the concentration of the p-nitroaniline diazonium salt solution, mol/L; the concentration of the p-nitroaniline hydrochloride standard solution, mol/L. C2
5.2.4 Determination steps
(2)
Use a weighing bottle to weigh 5g of the powdered sample or 10g of the granulated sample (accurate to 0.0002g), put it in a 500mL beaker, add 200mL distilled water, and then add 1+1 hydrochloric acid solution until the Congo red test paper turns blue, heat and boil to drive out sulfur dioxide, cool to room temperature, neutralize with 100g/L sodium carbonate solution to pH=7, transfer to a 500mL volumetric flask, dilute to the scale with distilled water, shake and set aside. Take 50mL of the above prepared solution, put it in a 500mL beaker, add 50mL water and 10g sodium carbonate, cool to below 10℃, use a burette with an ice water jacket, and titrate with 0.04mol/L p-nitroaniline diazonium salt standard titration solution. When the titration is close to the end point, take a drop of coupling solution on the filter paper and the run circle that meets the p-nitroaniline diazonium salt solution does not show color, but when it meets the H acid-base solution, it will show obvious purple within 5-10s, and continue to stir for 2min. Check that the run circle purple does not disappear, which is the end point, and perform a blank test at the same time. 5.2.5 Expression of analytical results
The content X of 1-naphthol-4-sulfonic acid expressed as mass fraction is calculated according to formula (3): .2242x.x1.
m×50X500
Wherein: c3—concentration of p-nitroaniline diazonium salt standard titration solution, mol/L; volume of p-nitroaniline diazonium salt standard titration solution consumed in one titration, mL, V3
mass of sample, g;
0.2242——mass of 1-naphthol-4-sulfonic acid expressed in grams equivalent to 1.00mL of p-nitroaniline diazonium salt standard titration solution [c(C6H^Ns02CI)=1.000mol/L]. 3
W.HG/T2897—1997
The difference between the results of the two parallel determinations shall not exceed 0.3%, and the arithmetic mean shall be taken as the determination result. 5.3 Determination of 1-naphthylamine-4-sulfonic acid content
5.3.1 Method summary
The paper chromatography method is used to separate the components by utilizing the difference in relative affinity of the components of the analyzed substance to the mobile phase and the stationary phase, and their content is determined by comparing with the standard. 5.3.2 Reagents, solutions and materials
n-Butanol;
n-Propanol;
Hydrochloric acid solution: 0.1mol/L, 1+1;
Anhydrous sodium carbonate solution: 50g/L;
Industrial p-nitroaniline: content ≥99%; Sodium nitrite solution: 0.1mol/L;
Anhydrous sodium acetate solution: 300g/L;
Sodium 1-naphthylamine-4-sulfonate, refined product: prepared according to the provisions of Appendix A; 95% ethanol;
Chromatography filter paper;
Developing agent: n-butanol-n-propanol-hydrochloric acid (0.1mol/L) Micro syringe: 10μL;
Chromatography cylinder: square or round.
=1+2+1
5.3.3 Preparation of 0.02mol/L p-nitroaniline diazonium salt solution for color development: Weigh 2.76g p-nitroaniline, add 50mL of 1+1 hydrochloric acid solution, heat to dissolve, and cool to room temperature. Transfer to a 1000mL volumetric flask and dilute to scale with water. Pipette 10mL of the above solution into a 100mL beaker, add 2.5mL of 0.1mol/L sodium nitrite solution in an ice bath for diazotization. The solution should be blue when tested with starch potassium iodide paper, and then add 15mL of 300g/L sodium acetate. Transfer to a glass sprayer, place in an ice bath and place in a dark place for use on the same day. 5.3.4 Determination steps
5.3.4.1 Preparation of 1-naphthylamine-4-sulfonic acid standard series solutions Weigh 0.1g (accurate to 0.0002g) of refined 1-naphthylamine-4-sulfonic acid (100%), dissolve it in 50g/L sodium carbonate solution, adjust the pH to 7, transfer it to a 100mL volumetric flask, and dilute it to the mark with distilled water. Then take 1mL, 2mL, 3mL, 4mL, 6mL, and 8mL respectively and place them in 100mL volumetric flasks, and dilute them to the mark with distilled water. The concentrations of the above standard series solutions are 0.01, 0.02, 0.03, 0.04, 0.06, and 0.08g/L, respectively. 5.3.4.2 Development
Take a filter paper of size 15cm×15cm, draw a straight line with a pencil at 2.5cm below it, use a microsyringe to draw 5μL of the sample solution and 1-naphthylamine-4-sulfonic acid standard solution prepared in 5.2 of this standard, and drip them on the filter paper, with the spot interval of 2cm. After drying with a hair dryer, put it into a glass chromatography cylinder filled with a developing agent and develop it by the ascending method. When the solvent front rises to 68cm, the filter paper can be taken out (time is about 2h) and blown dry.
5.3.4.3 Color development
Spray the p-nitroaniline diazonium salt solution on the filter paper, blow dry and develop the color, compare the spot size and color depth of 1-naphthylamine-4-sulfonic acid in the sample with the spots developed by the 1-naphthylamine-4-sulfonic acid standard series solution to determine the content of 1-naphthylamine-4-sulfonic acid in the sample. 5.3.4.4 Expression of analysis results
The 1-naphthylamine-4-sulfonic acid content X2 expressed as mass percentage is calculated according to formula (4): X2
Cg·X1
(4)
WHG/T2897—1997
WHG/T2897—1997
Wherein: c—concentration of 1-naphthylamine-4-sulfonic acid standard solution equivalent to the sample, 8/L; Cs—concentration of 1-naphthol-4-sulfonic acid sample solution, g/L; X1——content of 1-naphthylamine-4-sulfonic acid, %. The difference between the results of two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 5.4 Determination of sulfur dioxide content
5.4.1 Summary of method
Sulfur dioxide undergoes a quantitative redox reaction with iodine in an acidic medium. The sulfur dioxide content is titrated and analyzed using a standard iodine titration solution and starch as an indicator.
5.4.2 Reagents and solutions
Iodine standard titration solution: c (1/2I2) = 0.1mol/L, prepared and calibrated according to the provisions of GB/T601, sulfuric acid solution: 1mol/L
Soluble starch solution: 1%.
5.4.3 Determination steps
Weigh 10g of sample (accurate to 0.1g), dissolve it with distilled water and place it in a 500mL stoppered conical flask, add 20mL of 1mol/L sulfuric acid solution, quickly cover the bottle stopper, and shake for 2~3min. Rinse the bottle mouth with distilled water. Add 2~3mL of 1% soluble starch, and then titrate with 1mol/L iodine standard titration solution until blue appears, which is the end point. 5.4.4 Expression of analysis results
The sulfur dioxide content X3 expressed as a percentage by mass is calculated according to formula (5): Xs
0.032XcgXV
Wherein: C6——concentration of iodine standard titration solution, mol/L; V4——volume of iodine standard titration solution consumed in titration, mLm1——mass of sample, g;
(5)
2——mass of 0.032
of sulfur dioxide equivalent to 1.00mL of iodine standard titration solution c (1/2I2) = 1.000mol/L) expressed in grams.
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 6 Inspection rules
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Factory Inspection
1-Naphthol-4-sulfonic acid shall be inspected by the quality inspection department of the factory. The factory shall ensure that all 1-naphthol-4-sulfonic acid shipped out of the factory meets the requirements of this standard. Each batch of 1-naphthol-4-sulfonic acid shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 User Acceptance
The user unit has the right to inspect the received 1-naphthol-4-sulfonic acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
6.4 Re-inspection
If one of the indicators in the inspection results does not meet the requirements of this standard, 1-phenol-4-sulfonic acid shall be re-examined from 100% of the packaging. If even one indicator in the re-inspection result does not meet the requirements of this standard, the entire batch of 1-naphthol-4-sulfonic acid cannot be accepted. 5
Wbzsoso.cOn7Marking, packaging, purchase, storage and transportation
7.1Marking
HG/T2897—1997
The outer packaging of 1-naphthol-4-sulfonic acid should be painted with a firm mark, indicating: manufacturer name, product name, batch number, production date, standard number, net weight and gross weight. Each bag (barrel) of packaged finished products should be accompanied by a product quality certificate, including: product net weight, proof that product quality meets the requirements of this standard and the number of this standard. 7.2 Packaging
1-Naphthol-4-sulfonic acid is packaged in iron barrels or wooden barrels lined with plastic bags, with a net weight of 50kg per barrel. 7.3 Transportation
1-Naphthol-4-sulfonic acid should be protected from exposure to sunlight, heavy pressure and moisture during transportation. The means of transportation should be clean and dry. 7.4 Storage
1-Naphthol-4-sulfonic acid should be stored in a cool and dry place, away from sunlight, rain and heat. 6
W.bzsosocomAppendix A (Standard Appendix)
Refining of 1-naphthylamine-4-sulfonic acid
Weigh 100g of industrial sodium 1-naphthylamine-4-sulfonate into a 400mL beaker, add 250mL of distilled water, and heat to dissolve. Add 10g of activated carbon at 7080℃ for 30min to decolorize, and filter while hot. Discard the filter cake, cool the filtrate to room temperature, and acidify it with 1+1 hydrochloric acid solution until the Congo red test paper turns blue, so that the 1-naphthylamine-4-sulfonic acid product precipitates. Filter, wash the filter cake with distilled water until it is neutral, take it out and place it in a 400mL beaker and add 5% sodium carbonate to dissolve it, then recrystallize it again according to the above method, wash the obtained filter cake with 0.5% ethanol solution several times, dry it at 90℃, and analyze its content (molecular weight in acid) according to the method specified in HG/T2-203-80 "1-naphthylamine-4-sulfonic acid sodium". The purified 1-naphthol-4-sulfonic acid is stored in a brown bottle.
W.bzsoso.cOm
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.