Some standard content:
Chemical Industry Standard of the People's Republic of China
Industrial Barium Hydroxide
Subject Content and Scope of Application
HG 2566-94
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of industrial barium hydroxide. This standard applies to industrial barium hydroxide. This product is mainly used in petroleum processing, refining of vegetable oil, fine chemicals, daily chemicals and production of barium salts, etc.
Molecular formula: Ba(OH)2·8H20
Relative molecular mass: 315.47 (according to the international relative atomic mass in 1989) 2 Reference standards
GB 190
Marking of dangerous goods packaging
GB/T 601
GB/T602
GB/T 603
GB1250
Chemical reagents
Preparation of standard solutions for titration analysis (volume analysis) Chemical reagents
Preparation of standard solutions for impurity determination
Preparation of preparations and products used in chemical reagent test methods Methods for expressing and determining limit values GB/T3049
GB/T 3051
GB/T 6678
GB/T 6682
GB 8946
GB 8947
3 Technical requirements
General method for determination of iron content in chemical products O-phenanthroline spectrophotometric method General method for determination of chloride content in inorganic chemical products Mercury titration method General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories Plastic woven bags
Composite plastic woven bags
3.1 Appearance: This product is white crystals or crystalline powder. 2 Industrial barium hydroxide should meet the requirements of the following table. 3.2
%(m/m)
Barium hydroxide C is calculated as Ba(OH),·8HOContent of JContent of Carbonate (BaCO)
Content of Chloride (calculated as CI)Content of Iron (Fe)
Content of Hydrochloric Acid Insoluble Matter
Content of Sulfuric Acid Non-precipitateBase
Content of Iodine Reducing Product (calculated as S)
Approved as Superior Product by the Ministry of Chemical Industry of the People's Republic of China on February 9, 1994
Qualified Product
Implemented from July 1, 1994
4 Test Methods
HG 2566—94
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and Grade 3 water specified in GB/T6682. The standard titration solution, impurity standard solution, preparation and products required in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified.
4.1 Determination of Hydroxide Content
4.1.1 Method Summary
Dissolve the sample in appropriate amount of water, and titrate with hydrochloric acid standard titration solution using phenolic acid as indicator. 4.1.2 Reagents and Materials
4.1.2.1 Hydrochloric acid (GB/T 622) standard titration solution: c(HCI) about 1 mol/L. 4.1.2.2 Phenolphthalein (GB/T10729) indicator solution: 10 g/L; 4.1.2.3 Carbon dioxide-free water.
4.1.3 Analysis Steps
Weigh about 3 g of the sample (accurate to 0.0002 g) and place it in a 250 ml conical flask. Dissolve it in 50mL of water without carbon dioxide, add 2 drops of phenolphthalein indicator solution, and immediately titrate with hydrochloric acid standard titration solution until the red color disappears. Keep this solution (solution A) for the determination of barium carbonate content.
4.1.4 Expression of analysis results
The content of strontium hydroxide [Ba(OH)2·8H,O] expressed as mass percentage is calculated according to formula (1): _Xc×0. 1577×100=
-the volume of hydrochloric acid standard titration solution consumed in titration, mL; formula tV
the actual concentration of hydrochloric acid standard titration solution, mol/L; m the mass of the sample·g;
the mass of strontium hydroxide [Ba(OH)2 *8H,O] expressed in grams equivalent to 1.00mL of hydrochloric acid standard titration solution (c (HCl) = 1.000mol/L).
4.1.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.3%. 4.2 Determination of barium carbonate content
4.2.1 Method summary
Add bromophenol blue indicator solution to the solution A retained in 4.1.3, and continue to titrate with hydrochloric acid standard titration solution until the solution color changes from blue-purple to yellow and the barium carbonate is completely neutralized.
4.2.2 Reagents and materials
4.2.2.1 Hydrochloric acid (GB/T622) standard titration solution: c (HCI) is about 1 mol/L, 4.2.2.2 Bromophenol blue (HG/T3-1224) indicator solution: 0.4 g/L. 4.2.3 Instruments and equipment
Microburette: graduation value 0.02 mL.
4.2.4 Analysis steps
Add 10-12 drops of bromophenol blue indicator solution to the solution A retained in 4.1.3. Use a microburette to continue titrating with hydrochloric acid standard titration solution until the color of the solution changes from blue-purple to yellow and remains unchanged for 30 seconds, which is the end point. 4.2.5 Expression of analysis results
The content of barium carbonate (BaCO3) X expressed as a mass percentage is calculated according to formula (2): X,
VXcX 0. 098 7
（2）
HG 2566—94bzxz.net
Wherein: V is the volume of standard hydrochloric acid solution consumed in titration, mL; the actual concentration of standard hydrochloric acid solution, mol/L; m is the mass of the sample, g;
0.0987 is the mass of barium carbonate (BaCO3) expressed in grams equivalent to 1.00 ml of standard hydrochloric acid solution (c(HCl)-1.000 mol/L).
4.2.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 4.3 Determination of chloride content
4.3.1 Quantitative method (arbitration method)
4.3.1.1 Reagents and materials
Same as Article 4 of GB/T3051.
4.3.1.2 Instruments and equipment
Same as (Article 3 of GB/T3051.
4.3.1.3 Analysis steps
Weigh about 5g of sample (accurate to 0.01g), place it in a conical flask, add 100mL of water, and heat to dissolve. After cooling, add 4.5ml. 1+1 nitric acid solution to neutralize. Add 2-3 drops of bromophenol blue indicator solution; if the solution is yellowish yellow, add sodium hydroxide solution until it turns blue, and then add 1+16 nitric acid solution until it turns yellow, and add 2-6 drops in excess; if the solution is blue, add 1+16 nitric acid solution until it turns yellow, and then add 2-6 drops in excess; add 1ml. benzyl azocarbonyl indicator solution, and titrate with standard mercuric nitrate titration solution (c[1/2Hg(NO)2) is about 0.05mol/1.) until the solution turns from yellowish yellow to purple-red as the end point. Perform a blank test at the same time. Mercury-containing wastewater shall be treated in accordance with Appendix D of GB/T3051. 4.3.1.4 Expression of analysis results
The chloride (as Cl) content X3 expressed as mass percentage shall be calculated according to formula (3): X = V-Vo)Xex0. 035 45×100
3. 545(V--V.)c
The volume of standard mercuric nitrate titration solution consumed in titration, mL; V: V---
The volume of standard mercuric nitrate titration solution consumed in blank test, mL; V.
The actual concentration of standard mercuric nitrate titration solution, mol/l; m——mass of sample, g;
0.03545—The mass of 1.00mL standard mercuric nitrate titration solution lc(C1).
（3）
Hg（NO)211.000mol/L) equivalent to chlorine expressed in party 4.3.1.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.01%. 4.3.2 Turbidimetric method
4.3.2.1 Reagents and materials
4.3.2.1.1 Nitric acid (GB/T626) solution: 1+2; 4.3.2.1.2 Silver nitrate (GB/T670) solution: 17g/L; 4.3.2.1.3 Dextrin solution: 20g/;
4.3.2.1.4 Chloride standard solution: 1mL contains 0.01mg chlorine. Use a pipette to transfer 10mL of the chloride standard solution prepared according to GB/T602 and place it in 100ml.Put it in a volumetric flask, dilute it to the mark with water, and shake it well. This solution can only be used on the same day. 4.3.2.2 Analysis steps
Weigh 1.000.01g of the sample, put it in a 100mL beaker, add 25mL of water and 3mL of nitric acid solution, heat to dissolve; after cooling, transfer all of it to a 250ml. volumetric flask, dilute it to the mark with water, shake it, and dry filter; use a pipette to transfer 10mL of this test solution, put it in a 50ml381
HG 2566--94
colorimetric tube, add 5mL of nitric acid solution, 0.2mL of dextrin solution, and 1ml of silver nitrate solution, add water to the mark, and shake it well; place it in a dark place for 15min, and the turbidity should not be greater than that of the standard turbidimetric solution. Preparation of standard turbidity solution: Use a pipette to transfer an appropriate amount of chloride standard solution (2 mL for superior products, 8 mL for first-class products: 12 mL for qualified products), place it in a 50 mL colorimetric tube, and treat it in the same way as the test solution. 4.4 Determination of iron content
4.4.1 Summary of method
Same as Article 2 of GB/T3049.
4.4.2 Reagents and materials
Same as Article 3 of GB/T3049.
4.4.3 Instruments and equipment
Same as Article 4 of GB/T3049.
4.4.4 Analysis steps
4.4.4.1 Drawing of working curve
According to Article 5.3 of GB/T3049, use a 3 cm absorption cell and the corresponding amount of iron standard solution to draw a working curve. 4.4.4.2 Preparation of test solution
Weigh about 3g of sample (accurate to 0.01g), place in a 100mL beaker, add 15mL of water, 20mL of 1+1 hydrochloric acid solution, 5 drops of nitric acid, heat and boil for 5min; after cooling, filter into a 100mL volumetric flask, dilute with water to the mark, and shake to hook. 4.4.4.3 Preparation of blank test solution
Except for not adding sample, other operations are the same as in 4.4.4.2. 4.4.4.4.4 Determination
Use a pipette to transfer 25 mL of the test solution and the same volume of the blank test solution into 100 mL volumetric flasks respectively. According to the provisions of Article 5.4 of GB/T3049, add water to about 60 mL when necessary and proceed with the operation. 4.4.4.5 Expression of analysis results
The iron (Fe) content X expressed as mass percentage is calculated according to formula (4): X.
(ml-mo)X10-×100
0. 4(mm.)
The amount of iron found from the working curve based on the measured absorbance of the test solution, mg; Where: m,
The amount of iron found from the working curve based on the measured absorbance of the reagent blank solution, mg; Sample mass, g.
4.4.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.002%. 4.5 Determination of hydrochloric acid insoluble matter content
4.5.1 Reagents and materials
4.5.1.1 Hydrochloric acid (GB/T622).
4.5.1.2 Nitric acid Silver (GB/T670) solution: 17g/L. 4.5.2. Instruments and equipment
Crock filter: filter plate pore size 5~15um. (4)
4.5.3 Analysis steps
Weigh about 5g of sample (accurate to 0.01g) and place it in a 100mL beaker, add 20mL of water and 7mL of hydrochloric acid to dissolve; filter with a crucible filter that has been dried to constant weight at 105~110°C, wash with hot water until there is no chloride ion (check with silver nitrate solution); dry at 105~110°C 382
to constant weight.
4.5.4 Expression of analysis results
HG 2566—94
The hydrochloric acid insoluble matter content X expressed as a mass percentage is calculated according to formula (5): X,
wherein: m2---the mass of the residue and the crucible filter, g; - the mass of the crucible filter, g;
m—the mass of the sample, g.
4.5.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.01%. 4.6 Determination of sulfuric acid insoluble matter content
4.6.1 Reagents and materials
4.6.1.1 Hydrochloric acid (GB/T 622);
4.6.1.2 Sulfuric acid (GB/T625) solution: 1+15. 4.6.2 Analysis steps
(5)
Weigh about 2g of sample (accurate to 0.01g), place in a 250mL beaker, add 100mL water and 2mL hydrochloric acid to dissolve, and boil; add 8mL of pre-warmed sulfuric acid solution under constant stirring, heat on a water bath for 30min, transfer all into a 250mL volumetric flask after cooling, add water to the scale, shake well, filter, and discard the first 20mL of filtrate. Use a pipette to transfer 50mL of filtrate, place in 100mL evaporator III that has been burned to constant weight at 800C, and heat and evaporate to dryness. Burn at 800℃ to constant weight. 4.6.3 Expression of analysis results
Content X of sulfuric acid non-precipitate expressed as mass percentage. Calculate according to formula (6): X2 = m = -m × 100 =
500(m2 - m2)
m × 250
Mass of residue and evaporated blood, g,
Where: m2 — -
m —Mass of evaporated blood, g;
m —Mass of sample, g.
4.6.4 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.1%. 4.7 Determination of iodine-reducing substance content
4.7.1 Reagents and materials
4.7.1.1 Hydrochloric acid (GB/T622) solution: 2+1; 4.7.1.2 Iodine (GB/T 675) solution: c(No.-I,) about 0.1 mol/L
4.7.1.3 Sodium thiosulfate (GB/T637) standard titration solution: c(NazSO3) about 0.1 mol/L; 4.7.1.4 Starch indicator solution: 10 g/L.
4.7.2 Analysis steps
In a 250mL iodine volumetric flask, add 20mL hydrochloric acid solution, add 10mL iodine solution with a pipette, and mix well; weigh about 4g of sample (accurate to 0.01g), add 100mL water to dissolve, and transfer all to the above mixed solution, cover the bottle cap, and shake; quickly titrate with sodium thiosulfate standard titration solution, add 1-2mL starch indicator solution when the solution turns light yellow, and continue to titrate the solution until the blue disappears as the end point, and perform a blank test at the same time.
4.7.3 Expression of analysis results
The iodine reduction product (in terms of S) content X expressed as mass percentage is calculated according to formula (7): 383
HG 2566-- 94
X, (VV)X0. 016 03 ×100
- 1, 603(V.-V)c..
Wherein: C--actual concentration of sodium thiosulfate standard titration solution, mol/L; V,--volume of sodium thiosulfate standard titration solution consumed in blank test, ml; V--volume of sodium thiosulfate standard titration solution consumed in titration, mL; m---mass of sample.g;
(7)
0.016(3---mass of sulfur (S) in grams equivalent to 1.00mL sodium thiosulfate standard titration solution Cc(Na2S,O3)=1.000mol/1.J.
4.7.4 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.02%. 5 Inspection rules
5.1 Industrial barium hydroxide products shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all industrial barium hydroxide shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate. The content includes the manufacturer's name, address, product name, net weight, grade, batch number or production date, proof that the product quality complies with this standard and the standard number. 5.2 The user has the right to inspect and accept the industrial barium hydroxide products received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 5t.
5.4 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB/T6678. When sampling, insert the sampler vertically from the center of the package to 3/4 of the material depth for sampling. After mixing the sample, it is reduced to about 500g by quartering method and divided into two clean, dry wide-mouth bottles with ground stoppers and sealed. Labels are affixed to the bottles, indicating the manufacturer's name, product name, grade, batch number, sampling date and the name of the sampler. One bottle is used for inspection, and the other bottle is kept for three months for reference. 5.5 If any of the indicators in the inspection results do not meet the requirements of this standard, sampling should be conducted from twice the amount of packaging for verification. Even if only one of the indicators in the inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the quality of the product, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.7 The rounded value comparison method specified in GB1250 shall be used to determine whether the inspection results meet the standards. 6 Marking, packaging, transportation, storage
6.1 The industrial barium hydroxide packaging bag should have firm and clear markings, including the manufacturer's name, address, product name, trademark, net weight, grade, batch number or production date, as well as the "toxic substance" mark specified in GB190 and the number of this standard. 6.2 Industrial barium hydroxide products are packaged in plastic woven bags or composite plastic woven bags. The outer bag is a plastic woven bag (type B or C), with a warp and weft density of 64 × 64/10cm, and the inner bag is a two-layer polyethylene film bag with a bag thickness of not less than 0.1mm; the outer bag is a composite plastic woven bag (type B or C), with a warp and weft density of 64 × 64/10cm, a coating thickness of not less than 0.05mm, and the inner bag is a layer of polyethylene film bag with a bag thickness of not less than 0.1mm. The packaging volume of the inner bag should be larger than that of the outer bag. Each batch of packaging materials should be sampled and inspected, and its performance and inspection methods should comply with the provisions of (GB8946, GB8947, and the net weight of each bag is 25kg or 50kg. 6.3 The inner bag of the package is double-layer tied or sealed to ensure tight sealing, and the outer bag is sewn by a sewing machine with a stitch length of no more than 10mm, neat stitches, even stitch lengths, and no seams or skipped stitches. 6.4. Industrial barium hydroxide products should be covered during transportation, and care should be taken to avoid mixed transportation of items that may cause product deterioration or damage to the packaging. 6.5 Industrial barium hydroxide products should be stored in ventilated and dry warehouses. In the warehouse. Prevent rain and avoid mixing materials and crystals that may deteriorate the product or damage the packaging.
Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Zili Chemical Plant of Qingdao Red Star Chemical Group, and Houma Xinxing Chemical Plant. The main drafters of this standard are Huang Jiaxie, Fan Guoqiang, Liu Yu, and Chai Hongxia. This standard adopts Japanese Industrial Standard JIS K1417-61 (88) "Barium Hydroxide".
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