HG/T 2279-2000 4,4\'-Diaminostilbene-2,2\'-disulfonic acid (DSD acid)
Some standard content:
JCS 71. 100. 01; 87. 060. 10G 57
Chemical Industry Standard of the People's Republic of China
Dye Intermediates
(2000)
Published on 2000-06-05
Implemented on 20010301
State Administration of Petroleum and Chemical Industry
Reservation No.: 74932000
IIG/T 2279-2000
This standard is equivalent to the previous industry standard TSK4158-1995 4,4-dihydrotetrafluoroethylene-2,2-diiodopropene and the other industry standard EIG/T279-1332,4-dihydrotetrafluoroethylene-2,2-diiodopropene (1\S1) acid. The control items have been determined based on the technical indicators and the needs of domestic and foreign users and the actual domestic production situation. The main differences between the standard and 14158-1 are as follows:
The Japanese Industrial Standard has only one product specification. This standard is divided into two specifications: 1000-grade product and 1000-grade product. This standard has only one grade of marking. This standard divides products into two grades: first-class products and second-class products. The tested products are divided into first-class products and second-class products. This standard adopts liquid chromatography with band method to analyze the content of benzene. This standard adopts the analysis of benzene content. This standard adds chromaticity, non-leafable substances and technical indicators. The main difference between this standard and G279-1 is that
adds 1 grade of products: superior products: second-class products have two grades, total ammonia value, total amino acid content, water content, non-leafable substances, chromaticity, secondary animal content and other seven technical indicators of the tested products, total hydrogen value, total amino acid value, etc., and the technical indicators of the tested products have been revised to reduce the maximum technical indicators of the base content. Added chromaticity indicators:
This standard is the appendix of the environmental standard.
This standard is implemented from the month, weekly replace T227-192. This standard is proposed by the National Petroleum and Chemical Industry Bureau, and the standard is used by the Technical Committee of Standardization of Materials. The units of this standard are Xiyang Chemical Research Institute, Shiju Chemical Industry Co., Ltd., Huayu Chemical Co., Ltd., Jiang Xiaowei Chemical Co., Ltd., Henan Anyang Feidi Chemical Co., Ltd.: This standard is required to be signed by the staff of the National Dye Certification Committee. The first publication of the standard was in 1982. It was first subscribed in 1SS2. This standard is issued by the Secretariat of the National Dye Certification Committee and is responsible for interpretation.-
Chemical Industry Standard of the People's Republic of China
4,4-Dichlorostilbene-2,2-disulfonic acid (DSI) 4,4'-1iaminostibene-2,2'-digulronic acid (1S1) Acid 1 Scope
JIGT22792000
Generation Lane/22791992
This standard specifies the requirements for sampling, testing, inspection, packaging and production of 4,4-diphenyldisulfonic acid 1)SL acid>
This standard is applicable to industrial SI acids obtained by catalysis, air oxidation and reduction. This product is mainly used in dyes and inflammation In the production of additives industry, the structure or:
formula: .HS.ON
relative end: 37C.1: (Interstate Relative Pressure 187) 2 Reference standards
The following referenced texts are also combined and constitute the reference text through use in this standard. When this standard is published, the versions shown are valid: All standards are subject to revision. Parties using this standard should explore the possibility of using the following standard versions: GB C.
[955 Chemical reagent titration analysis (6C3-1933
Preparation of standard electrodes for container analysis-25J-1389
G3/T 2355-138)
GB,T GGH2
GB/TSS78
GH/T 7531
3 Requirements
Limiting number of methods for determination of moisture content in dyes and dye intermediates Specification and test method for water content in test results [S) 6S:987) General rules for chemical product samples
The amount of DSD acid in the determination of the content of organic chemical products shall comply with Table F.
National Petroleum and Chemical Industry High 200-06-05 approved 2091-03-01 implementation
HG/T2279-2C0D
Table 1 Quality requirements of DST acid
Total modified base estimate (total US value of controlled natural product dosage form): total or prohibited product (according to the total supply and total balance), 4,4-digram to absorb this-2,2-lan garbage magnetic aromatic compound) content (limited to 11G% 1 deer
Agricultural exchange contains members·%
Lu Ge contains 1M
Fenxian Road
1 deep sample
Each list product
Growth status
Compared with two colors of minced ||t t||Sampling is done in batches. The products are collected from 10 bags (or) of each batch of products. The sampling units specified in 668--1986.5 are used for sampling. The packaging of the sampled products must be intact: When sampling, the external impurities are closed to prevent them from falling into the product. The sampler is used to take samples from the upper, middle and lower parts, including the upper, middle and lower parts. The total amount of the sample taken shall not be less than 50%, and the sample shall not be less than 50%. The sampled products shall be separated by light and packaged into sterile and dry bottles. Labels shall be placed on the bottles, indicating: manufacturer name, product name, batch number, quality assurance, and location: one bottle is sealed with wax and kept for future reference. 5 Test method
Unless otherwise specified, each bottle shall be sealed with wax and kept for future reference. The reagents used shall be analytically pure reagents; the test reagents shall comply with the three-grade requirements of GB662. The preparation of the standard shall be in accordance with the relevant provisions of GB601 and GB1693. The test results shall be determined by comparing the modified mean values in GB250189. 5. Appearance
The appearance shall be determined by the standard.
5.2 Determination of total nitrogen
5.2.1 Summary
The total nitrogen at room temperature shall be determined by the chemical method. In the presence of inorganic acid, sodium nitrite is reacted with sodium nitrite to form a heavy reaction:
5.2.2 Reagents and solutions
5.2.2.1 Basic nitrogen: Chemistry.
5.2.2.2 Sodium carbonate solution: chemically pure, 1g/1.5.2.2.3 Potassium hydroxide solution: chemically pure, 100μ/T. 5.2-2.47. Determine the solution of sodium nitrate: c(VaN0). 1g/1.5.2.2.5 Determine the solution of sodium nitrate.
5.2.3 Determine the solution weight
Weigh the sample 8 and the sample 4 to 200g accurately. Place 3ml sodium carbonate solution in a 31. beaker and beat into charcoal with a small amount of distilled water. Dissolve in distilled water, then transfer to a 100ml container, transfer gently with hot water and set aside.
HG/T 2279—2000
Take the whole sample and add 430 ml of hot water and 100/30 molten liquid into a 600ml cup. At 15-31℃, estimate the concentration of the sample once, add more sodium nitrate into the standard titration box under rapid stirring, add acid once, stir well, test it with the powder-activated test paper, it should not turn blue early, continue to titrate with the acid-activated standard solution until the test solution turns slightly blue on the test paper. Ensure that the titration changes to the endpoint within 5mr. (If it exceeds 1, it is not enough to perform the calculation.) Carry out a blank test under the same conditions. 3.2.4 Expression of analytical results The total concentration of the standard sodium nitrate solution expressed as a percentage of volume is calculated according to Formula 1: X-+X(VV)/185 2X100. Determine the volume of sodium nitrate standard solution consumed in titration, and the volume of sodium nitrate standard solution consumed in the blank test is the volume of sodium nitrate standard solution consumed in titration. .m process:)
equivalent to 1.0mL sodium iodide standard solution c(NaVO:=1.(00mol/L). The maximum mass of the DSD test expressed in grams. The difference between the results of the two parallel determinations shall not exceed U.2%. Take the arithmetic half mean of the total number of determinations as the total number of determinations. 5.3 Total number of samples of benzene
5.3.1 Determination of the total number of samples
Use a flat plate to weigh about 100 ml of the sample (accurate to 0.cc:g) and place it in an oven and dry it at 1cc-95. The new sample is used for the determination of the basic quantity, 5-3.2115I acid content calculation
Expressed in mass percentage! Solid content ×, calculated according to formula (2): X
Wherein, - full sample energy mass:
mass of the sample before construction
5.3.3 Full value of the total basis value of the product
Total basis value of the DST acid product expressed as a percentage of the plate: calculated according to formula (5): X.=
Formula: - S acid content expressed as a mass number X
Total amino value of the DSD whole product expressed as a mass percentage [natural commercial dosage form], fire, 5.4 Determination of water content in the lower grade DSE acid
5.4.1 Implementation
Weigh the whole product in a bottle (precision to taste in a box at 1 ~.105 °C) and weigh it according to the machine weight,
5.4.2 Analytical results are expressed as a percentage of the total amount The water content of the product S represented by formula (4) is Xm×100. Better than the quality of the previous sample: The quality of the sample after drying is R. 5.5 Determination of the content of base material 5.5.1 Principle of the method HG/T2279-2000 Paper chromatography: The relative affinity of each component molecule to the mobile phase is different, so that each component is separated: Under the reference standard, the isomer content is determined. 5.5.2 False Deng Village material 5.5.2.1 Square chromatography red (or end of the original certificate!. b. 5.2.2 Micro-sampler, 10kl.. 5.5.2.3 Folding filter paper: No. 1 medium speed filter paper, 5. 5. 2. 4
Triangular glass spray.
5.5.3 Agent and liquid
Anhydrous alcohol.
5. 5. 3.
5. 5. 3. 3
Chlorine North auxiliary water squeeze Bay: 26.
Nitrogen aqueous solution, 1+9.
5. 5. 3.4
5.5.3.519 [wall expansion to product preparation 5 guarantee record A
5.5.3.6 Card H hook standard system - provide
5.5.4 Section Bodhi standard series and sample drop hoop book matching to 5.5.4.1 Card base standard series concentrated roll preparation Weigh the extract standard. 25 (accurate single 0.001g). Ten 50mL shock through the bottle, with a small drop Dehydrate and add to the scale with a pipette, respectively aspirate these five 1.50L (5.50L, 1.m, 1.5m) samples, add 0.FC (accurate to 1%) hydrogen peroxide and then incubate the samples to the scale, that is, prepare the standard solution with the card base content of 1.25%, 0.5%, 0.75%, 1.00% and 1.50% in the corresponding DSD acid product. This standard is valid for 20 years. 5.5.4.2 Preparation of S acid reduction Weigh 1% reduced sample viscosity (accurate to 10). Dissolve in brown electrolyte with water until dissolved. Dissolve until the solution is dissolved. Take a piece of chromatography paper with a length of 233 mm and a width of 233 mm. Use a pencil to lightly draw a line every 2 mm on the line 25 mm from one end. Use a micrometer to mark the spot with a pencil. Use a microscope to spot the standard matrix solution and the sample solution respectively. Place the spots in the marked positions slightly to make them consistent. After the spots are cooked, change to the blue R layer (be careful to avoid light). Use the upper limit to start from 2 hours.
5. 5.6 Weigh the aldehyde in Table 2 in a colorimetric bottle, add 2.5% hydrochloric acid, and sieve to the scale with anhydrous alcohol. Place it in a bottle next to the triangle plate for later use. After the layer is exposed, the color development period is 53-5 hours. The above results can be used to read the color of the aldehyde: 5-5-7. Under the natural light of the teacher, the color development of the sample is positive. The color depth of the sample is the size of the color of the sample series, and the color of the sample is the depth of the sample. Method: 1. This industry standard adopts the table method to analyze the content of alkali substances in products. 6. HG/T 2779-7000. A. Item 1 Schematic diagram of paper chromatography of alkali substances in DSD acid 5.6 Determination of alkali-insoluble substance content 5.6-1 Reagents and materials: Sodium carbonate; Chemical formula: 1008 J, filtration.
5. 6.2 Determination steps
Weigh the sample of the standard product or the sample with approximately 100 ml of distilled water in a 40-mL beaker, add 10 g/mL of sodium carbonate concentrate, shake until the sample is completely dissolved, then dry it in a 100-105°C oven, filter it, and then wash it with steamed paper until the alkali solution is not rotten. Bake it in a 101C5 oven until constant weight.
5.6.3 Expression of the analysis
The content of alkali-free matter expressed as mass percentage (calculated according to formula (5) 1.=
after drying C, the total mass of filter and free residue, and the formula:
-the mass of the G filter dried to constant temperature·B
m-the mass of the S sample,
-the total nitrogen value of the acid (whole commercial dosage form) expressed as percentage by mass, %. 5.7 The measurement of the immunity is
5.7,1 The original
method hates the Lambert-Jerr rule. When the test light path is fixed, the conditions remain unchanged, then the measured light intensity in a certain range of irradiance is proportional to the sensitivity of the measured substance. 5.7.2 Apparatus and equipment 5-7.2.1 Photometric spectrophotometer: domestic 72-pair spectrophotometer or other spectrophotometer of equivalent performance. 5.7.2.2 Colorimetric stone: 10 ml 5.7.2.3 Volumetric flask: brown, 100 ml, 1 ml 5-7.3 5.7.3.1 Anhydrous carbonic acid: 5.7.3.2 Preparation of slow dilution: 5.7.4 Weigh 1% sodium carbonate and 1% sodium carbonate (accurate to 3.1x), put into a 100ml beaker, evaporate for a while, dissolve in 1CC of water, then dilute with distilled water to the mark: 5.7.5 Weigh the total amount of sample to make 100% (accurate to 3.5%), dissolve the sample with the above dilution, then add into a 3mL brown container, and bring to the mark.
Take some water as the seasonal substance, use 1)n stone to change the colorimetric blood, and use a spectrophotometer to determine the color of the test solution at 0nm, 462m00m within 3min respectively.
5.7.5 Expression of analytical auxiliary
Color theory (≥01)> According to formula (6), calculate the firstWww.bzxZ.net
om44(r>+o1(46m)-(non)
044Gnm>-
Deotm)
UD(EOO tM)
5.8 Determination of the content of the organic chemical
Absorbance at -447mm,
Absorbance at 1m:
Absorbance at 52m.
According to the determination of organic chemical components in GB/7531, weigh the test sample 28 to C.91g> and heat it to constant temperature in a -7000 degree oven, then slowly heat it in an electric furnace for carbonization, add 0.m acid at room temperature, heat it again in a furnace to volatilize sulfuric acid, then transfer it to a high temperature cabinet: 633.7 carbonization and burn it to constant temperature: then move it to a desiccant (with a desiccant as a glue avoider) and cool it to 0m:n.6 Inspection rules
E.1 Inspection classification
All the stubborn days specified in Table 1 are taken as the output! Dress up items 6.? Production! JIS [) should be inspected by the inspection department of the production plant according to the requirements of this standard: the production department should ensure that all products leaving the factory meet the requirements of this standard. 5.3 The unit shall conduct a quality inspection according to the established L>SD age of this standard, and report that the quality meets the requirements of this standard. 6.4 Inspection If the quality inspection result does not meet the requirements of this standard, the sample shall be re-inspected: even if only one indicator does not meet the requirements of this standard, the quality batch of products cannot be inspected. 7 Marking, labeling, packaging, and storage. 1 Marking, labeling, DS> The acid packaging barrel (bag) should have a clear weekly disinfection mark. Note the production date! Name and factory certificate.Product name, registered trademark, standard number, production number, production date, product quality certification and standard number: 7.2 Packaging
DST> Use plastic plywood or woven packaging, tightly closed, net weight of each piece 50g. Other packaging can be arranged with customers:
7.3 Transportation and storage
HG/T2279
According to the specified accessories and transportation vehicles, it can also be transported through the intermediate protection to prevent the packaging from being damaged and avoid product contact in the air to prevent deterioration. The product should be stored in a cool, dry and ventilated room. A1.1 Reagents and reagents A.1.1 Sodium hydroxide: chemically pure A1.1.2 DSD acid: T grade A1.1.3 Activated carbon: industrial grade. HG/2279—200 Appendix A (material-free attachment) TSD acid refining and inspection method A1.1.4 Sodium hydrogen bath: chemically pure, 4 M*/L. A1.1.5 Chlorination liquid: Chemical 1005/LA1.1.6 with chlorination, chemically pure: 1-1.
A1.2 Preparation steps
Weigh 300g of TASD acid solution and add 500ml of water, add sodium hydroxide solution to make H=8, decompose it completely, add 15g of activated carbon and filter it at room temperature. Add 1g% of micro-solvent, and after decomposing it completely, reduce the content to 2%~3. The filter cake is washed with 1C/0.1% sodium hydroxide solution for four times, and the filter cake is dissolved in 1200l steamed water, filtered with 1+1 acid adjusted to pH=2, and the filter cake is washed with 11m1 steamed water for the second time, and then dried at F100--1G5 for ten times and the cake is broken into pieces. A2 inspection method and quality requirements
stable method; 5.3, 5= and 5.7 are carried out. Quality requirements: the base value is greater than %, and the color point inspection DSD point should be free of other impurities, and the color OD is less than 5.10.
1 said that there are few new and low-purification products until the batch is confirmed. 2) Our products do not require A2 quality, and the color can be reduced by about 2 times. The salt solution is heated with 420ml of water for the first time, and the solution is decomposed by the reaction mixture. The precipitation rate is temporarily increased by 1. Add people to the reaction mixture, and the precipitation rate is temporarily increased by 1.
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