Some standard content:
National Standard of the People's Republic of China
Anbydrous aluminium chloride for industrial use1 Subject content and scope of application
GB/T3959-94
Replaces GR3959-83
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of industrial anhydrous aluminium chloride. This standard applies to industrial anhydrous aluminium chloride. The product is mainly used as a catalyst in the organic chemical industry. Formula: AC
Relative molecular weight: 133.34 (according to the relative atomic mass of solid in 1989)2 Reference standards
GH191 Pictorial marking for packaging, storage and transportation
GB/T 602 Preparation of standard solutions for determination of impurities in chemical reagents GB/T 603 Preparation of preparations and products used in test methods for chemical reagents GB1250 Methods for expressing and determining limit values GB/T 3049 General method for determination of iron content in chemical products O-phenanthroline spectrophotometry
GB/T6678 General rules for sampling of chemical products
GB/T6682 Specifications and test methods for water used in analytical laboratories 3 Technical requirements
3.1 Appearance: white, yellow or slightly gray particles or powder, no lumps larger than 1mm, 3.2 Industrial anhydrous aluminum chloride should meet the requirements of the following table: % (m/m)
Aluminum chloride (AICl,) content
Iron (as FcCl Content of impurities (in terms of Pb)
Content of water impurities
Content of heavy metals (in terms of Pb)
Content of ionized aluminum
Test method
Superior qualitybZxz.net
First-class quality
Qualified quality
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and the impurity standard solutions, preparations and products required for the third-level water test specified in GB/T 6682. Unless otherwise specified, they are prepared in accordance with the provisions of GB/T 602 and GB/T 603.
Approved by the State Administration of Technical Supervision on December 22, 1994 and implemented on October 1, 1995
4.1 Determination of aluminum chloride content
4.1.1 Method summary
CB/T 3959--94
In a slightly acidic solution, use diphenylazocarbonyl hydrazide as an indicator and use mercuric nitrate standard titration solution to titrate chloride ions. 4.1.2 Reagents and materials
4.1.2.1 95% Z alcohol (GB/T 679).
4.1.2.2 Nitric acid (GB/T 626): 1+1 solution. 4.1.2.3 Nitric acid (GB/T 626): 1+15 solution. 4.1.2.4 Mercuric nitrate standard titration solution.c[1/2Hg (NO,). About 0.1mal/L. #Preparation
Weigh 17.13g nitric acid [Hg(NO3)：·H2O3], add 7ml nitric acid solution (4-1.2.2) and a small amount of water to dissolve, filter if necessary, dilute to 1000ml with water, shake well.
Alternatively, weigh 10.85g nitric acid (Hg0), add 20mL nitric acid solution (4.1.2.2) and a small amount of water to dissolve, filter if necessary. Dilute to 1 000ml with water, shake well.
Weigh 0.15-0.20g sodium chloride (basic reagent) (GB1253) pre-burned at 500-600C to constant weight, accurate to 0.0002g. Place in a 250mL conical flask, add 100mL water to dissolve. Add 2-3 drops of bromophenol blue indicator solution, add nitric acid solution (4.1.2.3) until it turns yellow and add 2 drops in excess. Add 1mlL diphenylazocarbonyl hydrazide indicator solution, and titrate with the prepared nitric acid multiplied by the standard titration solution until the solution turns light purple red, which is the end point. Perform a blank test at the same time. Collect the mercury-containing waste liquid after titration and treat it according to the provisions of Appendix A. c Calculate the concentration of the standard titration solution of mercuric nitrate c[1/2Hg(NO,), according to formula (1): zi1/2Hg(NO)=(VV)× 0. 058 44 Formula A: m-the mass of sodium chloride weighed, g, V-the volume of the standard titration solution of mercuric nitrate consumed in the titration, mL; V.-the volume of the nitric acid consumed in the blank test multiplied by the standard titration solution, mL (1)
Calculate the mass of sodium chloride in grams equivalent to 1.00mL nitric acid (c[1/2Hg(NO,),]=1.000mol/l.) 0. 058 44——
4.1.2.5 Bromophenol blue (GB/T 12592), 0.1 g/L ethanol solution. 4.1.2-6
Diphenylazocarbonyl: 5B/L ethanol solution. 4.1.3 Analysis steps
4.1.3.1 Preparation of test solution
Use a weighing bottle with an inner diameter of about 15mm to weigh about 1g of sample at a fast speed, accurate to 0.0002g. Carefully place the weighing bottle into a 200ml. measuring cylinder with a grinding stopper (or other equivalent container) filled with 80mL of water, immediately cover it with a ground stopper, and gently shake it to open the weighing bottle cap. After the sample is completely dissolved and the fluorine oxide gas is completely absorbed by the water, transfer all the solution to a 250ml. volumetric flask, dilute it to the scale with water, and shake it.
4.1.3.2 Determination
Use a pipette to transfer 25mL of the test bath solution (4.1.3.1) into a 250ml conical flask, add about 75mL of water and 2-3 drops of bromophenol indicator solution. Add nitric acid solution (4.1.2.3) until it turns yellow and add 2 drops in excess. Add 1mL of diphenylazocarbonylhydrazide indicator solution. Titrate with standard mercuric nitrate titration solution until the solution turns light purple-red, which is the end point. Perform a blank test at the same time.
Collect the waste liquid after titration and dispose of it according to the provisions of Appendix A. 4.1.4 Expression of analysis results
GB/T 3959-94
The aluminum chloride (AICl.) content (X,) expressed as mass percentage is calculated according to formula (2): X,=cV-V) X0 04 45 × 100 - 0 22 × xx
44. 45 × c(V - V,)
2-0.822×X
wherein c-
0. 044 45-
actual concentration of mercuric nitrate standard titration solution, ol/L volume of mercuric acid standard titration filtrate consumed in titration, L volume of mercuric nitrate standard titration solution consumed in blank test, mL: mass of sample t
and 1. 00mL nitric acid to obtain standard titration solution te[1/2Hg(NO,),]=1.000 mol/I.) equivalent to the mass of aluminum chloride expressed in grams:
X24.2 Iron content (in FcCl) measured, %: 0.822-
Coefficient for converting ferric chloride into aluminum chloride.
4.1.5 Allowable error
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.3%. 4.2 Determination of iron content
4.2.1 Summary of the method
Same as Chapter 2 of GB/T 3049.
4.2.2 Reagents and materials
Same as Chapter 3 of GB/T 3049.
4.2.3 Apparatus and equipment
Same as Chapter 4 of GB/T 3049.
4.2.4 Analysis steps
4.2.4.1 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 the working curve. 4.2.4.2 Determination
Use a pipette to transfer 50 mL (superior products, inferior products) or 20 mL (qualified products) of the test solution (4.1.3.1) and place it in a 100 mL beaker. Then transfer the same volume of water and place it in another 100 mL beaker. The following operations are carried out according to Article 5.4.1 of GB/T3049\If necessary, add water to 60 ml...\.
4.2.5 Expression of analysis results
The iron content (in terms of FeCl2) expressed as mass percentage (X) is calculated according to formula (3): X ~ (m -m) × 18 × 2.90 × 100 = Z72.5 (m - mg)
m×250
武中.mi-
The amount of iron found from the curve based on the measured absorbance of the test solution, mg; m?The amount of iron found from the curve based on the measured absorbance of the reagent blank solution, mg:V——The volume of the test solution (4.1.3.1) taken,mL; m—mass of the sample weighed when preparing the test solution (4.1.3.1), g; coefficient for converting iron into ferric chloride.
4.2.6 Allowable error
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results, the superior product, the inferior product shall not exceed 0.01%, and the qualified product shall not exceed 0.02. 4.3 Determination of water-insoluble matter content
4.3.1 Reagents and materials
GB/T 3959-94
4.3.1.1 Silver nitrate (GB/T670): 10g/L solution. 4.3.2 Instruments and equipment
4.3.2.1 Filter: pore size of filter plate 5~15 μm 4.3.3 Analysis steps
Weigh about 10g of the sample, accurate to 0.01g, place in a dry 400mL beaker, and cover with blood. Slowly add 100ml of water to dissolve (operate in a fume hood). Filter through a filter that has been dried to constant weight at 105-110℃, and wash with water until there is no oxygen ion (check with silver nitrate solution). Dry at 105-110℃ to constant weight. 4.3.4 Expression of analysis results
The water-insoluble content (X,) expressed as mass percentage is calculated according to formula (4): X, = \ = m × 100
Where: m1-\ mass of the filter, g-water-insoluble matter and mass of the filter + m + —·mass of the sample, g.
4.3.5 Allowable error
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference between the parallel determination results of two drinks shall not exceed 0.01%. 4.4 Determination of heavy metal content
4.4.1 Method summary
In a micro-medium, heavy metal ions react with hydrogen sulfide to generate sulfide precipitation and form a dark suspension. Compare with the standard colorimetric solution.
4.4.2 Reagents and materials
4.4.2.1 Ascorbic acid.
4.4.2.2 Acetic acid-sodium acetate buffer solution; pH is about 34.4.2.3 Saturated hydrogen sulfide water, prepared before use. 4.4.2.4 Lead standard solution: 1mL contains 0.1 mgh. 4.4-3 Instruments and equipment
4.4.3.1 Colorimetric tube: 50mL.
4.4.4 Analysis steps
4.4.4.1 Preparation of test solution
Weigh 2.50+0.01g (superior product) or 1.25±0.01g (first-class product) sample, carefully dissolve, filter if necessary, transfer all to a 50 mL volumetric flask, dilute with water to scale, and shake. 4.4.4.2 Determination
Pipette 30 mL of test solution (4-4.4.1) into a 50 mL colorimetric tube, add 0.1 g ascorbic acid, 5 mL buffer solution, and 10 mL saturated hydrogen sulfide water, dilute with water to scale, and shake. Let it evaporate in a dark place for 10 minutes. The color should not be darker than the standard colorimetric solution. Preparation of standard colorimetric solution:
Put 10mL of the test solution (4.4.4.1) into another 50tml colorimetric tube, transfer 0.6mL (for superior products) or 2mL (for inferior products) of lead standard solution, and treat it in the same way as the sample. 4.5 Determination of free aluminum content
4.5.1 Summary of the method
In the presence of ferric chloride, in a sulfuric acid and phosphoric acid mixed medium, use sodium monophenylamine sulfonate as an indicator and titrate with potassium dichromate standard titration solution. 4.5.2 Reagents and materials
4.5.2-1 Phosphoric acid (GB/T 1282).
4.5.2.2 Sulfuric acid (GB/T625): 1+3 solution. GB/T 3959—94
4.5.2.3 Ferric chloride (HG/3-1085): 100g/L solution. 4.5.2.4 Potassium dichromate (working standard reagent) (GB1259): c(1/6K,Cr0,)=0.0100mol/1. Standard titration solution. Weigh 0.4903g of potassium dichromate that has been dried to constant weight at 150-200℃, and dissolve it in water. Transfer all of it to a 1000ml volumetric flask, dilute to the mark with water, and check.
4.5.2.5 Sodium diphenylamine sulfonate: 2.5&/L solution.4.5.3 Instruments and equipment
4.5.3.1 Ice bath.
4.5.3.2 Electromagnetic stirrer: equipped with a stirrer.4.5.4 Analysis steps
Place the ice bath on the electromagnetic stirrer. Measure 50mL of ferric oxide solution and place it in a 400mL beaker containing 100mL of water, add a stirrer, and insert a thermometer. Place the beaker in the ice bath. Start stirring and cool the solution to below 20°C. Weigh about 10g of sample, accurate to 0.01g, and slowly (a small amount at a time) add it to the cold ferric chloride solution, keeping the temperature below 25°C. After the sample is completely dissolved, remove the beaker from the ice bath. Add 4.5mL of sulfuric acid solution, mix, then add 4.5-5.0mL of phosphoric acid and mix. Add 6-7 drops of sodium diphenylamine sulfonate indicator solution and titrate with potassium dichromate standard titration solution until the solution turns purple, which is the end point. Follow the above steps, but do not add sample and perform a blank test. 4.5.5 Expression of separation results
The free aluminum content (X,) expressed as mass percentage is calculated according to formula (5): X, VV)X0.08994 ×100
0. 899 4 × e(V Ve)
The actual concentration of potassium dichromate standard titration solution, mlal/L1:
The volume of potassium dichromate standard titration solution consumed in the titration, ml.; V. —The volume of potassium dichromate standard titration solution consumed in the blank test, ml.m-mass of the sample·g;
0.008994——The mass of cobalt expressed in grams equivalent to 1.00mL of potassium dichromate standard titration solution [c (1/6K,Cr,0,) = 1.000mol/L].
4.5.6 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.002%. 5 Inspection rules
5.1 All index items specified in this standard Month is the date for type inspection. Among them, aluminum fluoride, iron, water insoluble matter, heavy metals and other four items are factory inspection items, which should be inspected batch by batch. Under normal production conditions, type inspection shall be carried out at least once every three months. 5.2 Industrial anhydrous aluminum fluoride 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 products leaving the factory meet the requirements of the standard. Each batch of products leaving the factory shall have a quality certificate, which includes: manufacturer name, factory address, product name, grade, net weight, batch number or production date, product quality certificate that meets this standard and this standard number. 5.3 The user unit has the right to accept the industrial aluminum chloride received in accordance with the provisions of this standard. The acceptance shall be carried out within one month from the date of arrival of the goods.
5.4 Each batch of products shall not exceed 501.
5.5 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB/T6678. When sampling, insert the sampler along the vertical center line of the package to two-thirds of the depth of the material layer for sampling. Each sample should be no less than 50g. Mix the samples thoroughly and immediately put them into two clean, dry wide-mouth bottles and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other bottle is kept for one month for future reference. 5.6 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sample from twice the amount of packaging for verification. Even if only one indicator in the verification results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.7 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the Product Quality Law of the People's Republic of China. 5.8 The rounded value comparison method specified in GB1250 shall be used to determine whether the inspection results meet the standards. 6 Marking, packaging, transportation and storage
6.1 The packaging of industrial anhydrous aluminum fluoride should be firmly and clearly marked, including: manufacturer name, address, product name, trademark, grade, net weight, batch number or production date, this standard number and the mark specified in GB1917\怕显\. 6.2 Industrial anhydrous aluminum fluoride is double-packed. The inner packaging is made of polyvinyl chloride plastic film bags with a thickness of not less than 0.07mm. The packaging volume should be larger than the outer packaging. The outer packaging is made of iron barrels, galvanized iron barrels or plastic barrels. The net weight of each barrel is 50kg or 100kg. 6.3 The inner bag of the packaging is tied twice with vinyl rope or other ropes of equivalent quality, and the outer packaging is sealed by pressing, hoop or twisting. 6.4 Industrial anhydrous lead fluoride should be protected from rain and moisture during transportation. 6.5 Industrial anhydrous aluminum chloride should be stored in a ventilated and dry warehouse. The shelf life of this product is six months from the date of production. A1 Principle
GB/T3959-94
Appendix A
Method for treating mercury-containing waste liquid
(Supplement)
In an alkaline medium, use an excess of sodium sulfide to precipitate mercury. Use hydrogen peroxide to oxidize the excess sodium sulfide to prevent mercury from dissolving in the form of polysulfides.
A2 Operation steps
Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml.40% sodium oxychloride solution and 100g sodium sulfide (NazS·9H,0) in turn and mix well. After 10min, slowly add 400mL30% hydrogen peroxide solution and mix thoroughly. After standing for 24 hours, the upper clear liquid is discharged into the wastewater, and the sediment is transferred to another container for mercury recovery by a dedicated person. The reagents used in the above operations are all industrial grade. Additional notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard was drafted by the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Jindong Chemical Plant and Tianjin Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Huang Jiashu, Wang Qiwen, Liu Youruo, and Ma Guiping. This standard was first issued on November 30, 1983. This standard refers to the US military standard MIL-A-63471-1987≤Aluminum Chloride Hydrochloride",
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