Some standard content:
Chemical Industry Standard of the People's Republic of China
Dyeing Salt S
1 Main Contents and Scope of Application
HG/T2591-94
Daiyu HG 2-379-80
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of dye-resistant salt S. This standard applies to sodium m-nitrobenzene sulfonate (called dye-resistant salt S) made from benzene as raw material. Structural formula:
Molecular formula: C, H, O, NSNa
Relative molecular mass: 225.15 (according to the international relative original mass in 1989) 2 Reference standards
GB/T 601
GB/T 602
GB/T 603
GB/T 2386wwW.bzxz.Net
3 Technical requirements
Chemical reagents Preparation of standard solutions for titration analysis (volumetric analysis) Chemical reagents
Preparation of standard solutions for impurity determination
Preparation of preparations and products used in chemical reagent test methods Determination of moisture content in dyes and dye intermediates The quality of anti-dyeing salt S should meet the requirements of the following table. Table 1
Content, %
plI value
Water-soluble matter content, dead
Calcium salt content (calculated as calcium ion), %
Water content, %
Test method
Yellow amorphous particles or powder
The standard solution, impurity standard solution, preparation and product required for the determination shall be prepared in accordance with the provisions of GB/1601, GB/T602 and GB/T603. 4.1 Appearance determination
Audio-visual evaluation
Approved by the Ministry of Chemical Industry of the People's Republic of China on March 9, 1994 348
Implemented on December 1, 1994
4.2 Content determination
4.2.1 Reagents and solutions
HG/T2591-94
4.2.1.1 Hydrochloric acid (GB/T622): analytically pure, 36%~38%; 4.2.1.2 Zinc powder: analytically pure;
4.2.1.3 Hydrochloric acid solution (GB/T622): analytically pure, 1+100; 4.2.1.4 Potassium bromide solution (GB/T649): analytically pure: 100g/l; 4.2.1.5 Sodium nitrite (GB/T 633) Standard titration solution: c(NaNO,) = 0.2 mol/L. Prepared according to GB/T 601, calibrated with potassium iodide starch test paper;
4.2.1.6 Potassium iodide-starch test paper, prepared according to GB/T603. 4.2.2 Determination steps: Weigh 2g (accurate to 0.002g) of anti-dyeing salt S sample into a 500mL beaker, add 250mL of water to dissolve, add 30mL of hydrochloric acid (4.2.1.1), and add 7g of zinc powder (4.2.1.2) in batches while stirring. Continue stirring for 30 minutes after the addition, filter, and wash the residue with 100ml of hydrochloric acid solution (1.2.1.3) in four times. Combine the filtrate with the washing solution, and then add 10ml of hydrochloric acid (4.2.1.1) and 10mL of potassium bromide solution (4.2.1.4). Cool to about 5℃ in an ice bath, and titrate with sodium nitrite standard solution (4.2.1.5). During titration, the tip of the burette should be inserted into the solution about 10min. Titrate slowly under stirring. When approaching the end point, the tip of the burette should leave the liquid surface and be washed with a small amount of water. The washing liquid should be added to the solution and the titration should be continued slowly. Use a glass rod to take a drop of liquid and place it on potassium iodide starch paper. If a slight blue color is found, use the same method to test after 5min. If a slight blue color still appears, it is the end point. At the same time, perform a blank test. The mass percentage content X of the anti-dyeing salt S is calculated by formula (1): X,-(V
V.) X0. 225 2
Wherein:
concentration of industrial sodium nitrate standard titration solution, mol/L; .…-volume of industrial sodium nitrate standard titration solution consumed by the test sample, mL; V,——volume of sodium nitrite standard titration solution consumed by the vacuum test, mL: 97
mass of the sample·g:
0.2252—-mass of the anti-dyeing salt S expressed in grams equivalent to 1.00mL of sodium nitrite standard titration solution le(NaNO,)=1.000mol/LJ.
The difference between parallel determinations shall not exceed 0.4%. The arithmetic mean of the parallel determination results shall be taken as the determination result. 4.3 Determination of pH value
4.3.1 Materials and instruments
4.3.1.1 Acidity meter
4.3.1.2 Distilled water: pH 7
4.3.2 Determination step: Weigh 1g (accurate to 0.001g) of the resist salt S sample in a beaker, add 100mL of distilled water, stir to dissolve it, and determine it with an acidity meter at room temperature.
4.4 Determination of water-insoluble matter content
4.4.1 Instruments and reagents
4.4.1.1 Crucible filter, No. 3
4.4.1.2 Distilled water, pH 7
4.4.2 Determination steps:
Weigh 2g (accurate to 0.001g) of anti-dyeing salt S sample in a beaker, add 600ml of water to dissolve it at room temperature, and filter it under reduced pressure in a No. 3 crucible filter at constant weight. Wash the filter residue with distilled water until the washing liquid becomes colorless, and dry it in an oven at 100~-105℃ to constant weight. The mass percentage X of water-insoluble matter is calculated according to formula (2): X.-
mass of the crucible filter together with the water-insoluble matter·name: X100
mass of the crucible filter-name
m——mass of the sample·g:
HG/T 2591-94
The difference between parallel determinations shall not exceed 0.05%. The arithmetic mean of the results of two parallel determinations shall be taken as the determination result. 4.5 Determination of calcium salt content
4.5.1 Reagents and solutions
4.5.1.1 Distilled water: pH 7;
4.5.1.2 Hydrochloric acid solution (GB/T622): analytical grade, 1+4;4.5.1.3 Ammonia solution (GB/T631): analytical grade, 1+10;4.5.1.4 Ammonia-ammonium chloride buffer solution: pH 10;4.5.1.5 Sodium ethylenediaminetetraacetate (EDTA) (GB/I1401) standard titration solution: c(EDTA)-0.1mol/4.5.1.6 Chromium T indicator.
4.5.2 Determination steps: Weigh 2g (accurate to 0.0002g) of the resist salt S sample into a 100mL beaker, add water to dissolve, transfer to a 100ml volumetric flask, dilute to the scale, use a pipette to draw 10mL of the solution into a 250mL conical flask, add 1ml of hydrochloric acid solution (4.5.1.2) and 100mL of distilled water (4..1.1), shake well for later use, neutralize with ammonia solution (4.5.1.3) to pH 7-8, add 1Uml of ammonia-ammonium chloride buffer (4.5.1.4), 3-~4 drops of chrome black T finger agent (4.5.1.G), and titrate with EDTA standard titration solution (1.5.1.5) until the color changes from purple to blue, which is the end point.
Mass percentage of calcium ion X: calculated according to formula (3): Xs-c: VX0.040 08.
Where:?
-Concentration of ELTA standard titration solution, mol/L; V——Volume of ELTA standard titration solution consumed, ml. "Mass of sample g;
Mass of calcium ion expressed in grams equivalent to 1.00mL of ethylenediaminetetraacetic acid sodium (EDTA) standard solution (FDTA) 1.000mol/L).
If the difference between parallel determinations is less than 0.05, the arithmetic mean of the results of two parallel determinations shall be taken as the determination result. 4.6 Determination of moisture content:
According to GB/T The mass percentage of moisture X specified in item 2386 of the method is calculated according to formula (4): X4
wherein: ms—the mass of the weighing bottle and the sample before drying, g: mi—the mass of the weighing bottle and the sample after drying + g; m
the mass of the sample·g.
The difference between parallel determinations shall not exceed 0.2%, and the arithmetic mean of the results of two parallel determinations shall be taken as the determination result. 5 Inspection rules
All items specified in the technical requirements table of this standard are factory inspection items. 5.1 Sampling method
5.1.1 Take samples according to 10% of the number of bags in each batch. When the batch is less than 10 bags, take samples of no less than 3 bags. 4)
5.1.2 When sampling, avoid mixing impurities into the sample. Use a sampler to take samples from the upper, middle and lower parts of the bag respectively. Mix the samples evenly and take out about 100g from them and put them into two clean, dry plastic bottles respectively. Cover and seal them tightly. Stick labels on the bottles, indicating: manufacturer name, sample name, batch number, production date, sampling date, etc. One bottle is for inspection and the other is for reference. 5.2 Factory Inspection
HG/T 2591—94
Products should be inspected by the factory quality inspection department before leaving the factory. The factory should ensure that all products leaving the factory meet the requirements of this standard and be accompanied by a quality certificate and standard code in a certain format. 5.3 User Inspection
Users can verify the quality indicators of the received anti-dyeing salt S products according to this standard to check whether they meet the requirements of this standard.
5.4 Re-inspection
If the inspection results show that one of the indicators does not meet the requirements of this standard, a re-inspection should be conducted at twice the original sampling volume. If the re-inspection results still show that one of the indicators does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.5 Arbitration
When the supply and demand parties have objections to the product quality, the arbitration institution can be decided by negotiation between the two parties. During arbitration, the inspection should be carried out according to the provisions of this standard. 6 Marking, packaging, transportation and storage
6.1 The packaging must be firmly marked: indicate the manufacturer's name, product name, trademark, address, batch number, standard number, net weight and production period, and have obvious safety precautions such as "keep away from fire", "avoid shock", "handle with care", etc. 6.2 The product is packed in a woven bag lined with a layer of plastic bag, and the net weight of each bag is 25kg. 6.3 Each bag should be attached with a product certificate, including the manufacturer's name, product name, batch number, specifications, inspection conclusion and inspector code stamp.
6.4 This product should be moisture-proof during transportation, and should be handled with care to avoid collision during loading and unloading. Do not throw it. 6.5 This product should be stored in a cool, dry and ventilated place, and avoid sunlight: away from heat, fire, acid, etc. The storage period is one year. Additional instructions:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is issued by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. The wood standard was drafted by Shanghai Zhongli Chemical Co., Ltd. in Shanhai, and the main drafters of this standard were Yang Mingda and Cai Yumei.
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