Methods of chemical analysis for glass raw materials for colour picture tubes-Methods for chemical analysis of dolomite
Some standard content:
Electronic Industry Standard of the People's Republic of China SJ/1 10087. 1~~10087. 8—91
Chemical analysis methods for main raw materials of color picture tube glass
Published on April 8, 1991
Implementation on July 1, 1991
Published by the Ministry of Machinery and Electronics Industry of the People's Republic of China Electronic Industry Standard of the People's Republic of China Chemical analysis methods
Methods tot cheroical aitalysis nl dilomite:1 Main content and scope of application
1.1 SJ/T 10087.2—91
This standard defines the analysis methods for raw materials for color picture tubes. 1.2 Scope of application This standard applies to the materials used in color picture tubes and also applies to the analysis of the corresponding raw materials used in black and white type glass products. 2. Calcium and oxidative analysis using standard (+H9000.1) electron beam cross-chemical method 3. 3.1.1 Calcium and oxidative analysis 3.1.2 Reagents: 1:3 diolamine: 1:1 1:1 calcium indicator: 5.1 and 0.1 activator: 0.1 MgSO4: 1% ... Standard melt flow: J.02 M
You take it = amine tetraacid "fishing, b& water rate solution and release rate! uuml. Calibration: absorb sub 0. system standard drop micro 25ml water 75m tablets 20 years old sodium chlorine oxide drop wave to 16. Add H [ammonia grade impact grid wave 10, with black T anti-cloud agent a few drops. Month EDTA standard clear alcohol is determined to shrink red to Yi Er endpoint meter network A standard rate method
People's Republic of China Figure Machinery and Electronics Industry Ministry 1991.04-08 approved 1910701 implementation
J. Zinc standard drop liquid: 0.0?Mbzxz.net
sJ/r10057.2—91
standard weigh pure evaluation (3. 99 above 6538g. Add 5 drops of 502:1 salt to 75ml of water. Heat for a while: cool and transfer to 505ml of water, sample until the temperature is low. Take nitrogen water to determine the water content.
3.1.3 Samples
Take about 0.3 of the sample and dry it in a constant temperature drying oven at 10°C. Cool to room temperature in a drying oven. 3.1.5 Sample steps
Weigh the sample 1.C and place it in a 100° hot water bath. Wet the surface with water and add 5ml of F:1. After the reaction is completed, wash the cup with water, add 1 ml of hydrochloric acid, put it on the surface and heat it. When smoke appears on the surface of the slice, add 5 ml of hydrochloric acid and 5 ml of water. After decomposition, use an appropriate amount of water, wash once, and put the mixture into a 250 ml bottle. Transfer the mixture to a dry place. Cool and dry 0.5 ml of hydrofluoric acid on a heating plate, cool, add 2 ml of hydrochloric acid, decompose thoroughly with 20 ml of water, and add 250 ml of a container, dilute with water to the specified concentration. Determination of chemical reaction;
25 ml of bottle A is taken out of a 33 ml beaker, add 75 ml of water m, 5m ethanol chamber, add 20% potassium hydroxide (K2O) at a temperature of 12.5-13.0. Add a little DTA indicator: the red color of the solution changes to blue, which is the end point. The amount of the solution is 5m, 5m of ethanol chamber, 5m of water, 95% amine salt and 10% glycol glue, and then add 0m of standard A indicator solution until the liquid changes from alcohol color to pure black, which is the end point: take the set number, calculate the result of 31.5, and calculate the content of calcium oxide in the sample by the formula: CaO) × 253X10
25 X 1000 x
2 1: ×
In the formula, .T.
E1A is the standard liquid for the guest solution. The standard liquid oxygen is the volume of the standard EDTA obtained by the standard oxygen consumption: the volume of the standard calcium oxide consumption DTA light flow, 8
51.6 analysis sent to the standard with small deviation.
3.2 Separation of ferrous metals
3.2.16 Method Summary
Route 1. Reagents and reagents
Chlorine water, 1:
b. Tartaric acid: 10%:
e. Hydrochloric acid:
NaCl, 1:
Amine solution: 10%:
Salt solution: 0.2%
SI/T 1C087.2--91
Weigh 1g of ferrous metal, dissolve it in 50ml of 95% ethanol, and dilute it to 530ml with water. g, Iron standard solution: containing FeS, 0.0lna/ml. Weigh 6.04 g of ammonium ferric sulfate, dissolve in 1 ml water and 10 ml of 1H2O, transfer to 1000 ml of a flask, mark the scale with water, divide 10 ml into 1000 ml bottles, and dilute to the scale with water. 3-2-5 Trial mixing
Same as 3.1.3.
3.2.4 Analysis steps
Pipette 25 ml of A solution into a 100 ml flask, add 5 ml of 10% reagent, 1-2 drops of 1% solution, neutralize with nitrogen solution until colorless, and then adjust to colorless with acetic acid. Add 10% hydroxylamine hydrochloride 2ml, add 0.2% o-hydroxylamine 5ml, dilute to scale with water, and place in water for 5-10 minutes, and measure the absorbance at a wavelength of 5-10nm with the standard series solution. Standard series:
Absorbance standard solution 0.5, 10.15, 20, 25ml are put into 100ml bottles respectively, add 10% tartaric acid solution 5ml, use p-nitroketone as indicator, neutralize with 11 ammonia water to yellow, then add 1:1 hydrochloric acid to colorless, add 0.2% hydroxylamine hydrochloride solution 2ml, shake well. Add 0.2% o-hydroxylamine solution 5ml, and mix well to form a standard series. Draw the relationship between concentration and absorbance from the measured light and then draw a curve as a standard. 3.2.5 Calculation of analysis results Based on the measured absorbance of the sample, find the corresponding amount of iron nitrate on the standard curve and calculate the content of dichromate in the sample according to the following formula:
FeO,(%) =
Wherein: A
350×100×4
The amount of dichromate in the sample solution + K
3.2.8 Density
The relative standard deviation is less than 5%.
3.3 Analysis of disulfide
3.3.1 Flake method
After the sample is dissolved, the insoluble sulfur is separated. The solution is oxidized with permanganate. At an appropriate H value, the color of III-disulfide is developed and the determination is made by spectrophotometry. 3.3.2 Reagent solution A. Sulfur, I 1.
National solution:
Acid solution: 1D%
Phenol solution: 0.2%
Water: 1
Urea solution: 20%
Potassium sulfate solution: C.5%
Diphenyl phthalate solution: 0.2%;
Iron solution: 1mg/ml
SJ/T 10087.2--91
Weigh the iron content of 0.048 and add 10ml of acid and 50ml of water in a ratio of 1:1. Heat on sand and evaporate to dryness. Add water to about 23ml. Place in hot water to dissolve thoroughly, and then dissolve in the sample until it reaches the mark. The standard solution of Cr2O3 is accurately weighed (0.19368) and then transferred to a 1000ml volumetric bottle. Draw 26 from it in a 600ml container and dilute it to the mark with water (containing Cr: 10mg/mr). This is the standard solution of Cr2O3 (containing 5mg/mr).
5-3.3 Sample
Same as 3.1.3,
3.35 Analysis steps
Weigh 23 ml of sample on a sintered rod, add about 1 ml of water to make a slurry, cover the surface with 20 ml of hydrochloric acid, and then wash it with warm water. Fill 800 ml of the mixture with a paper towel and transfer it to a dry ashing paper. After cooling, add 1 drop of acid and 1 drop of sulfuric acid. When the white smoke of sulfuric acid evaporates completely, remove it and heat it with 10 ml of water until it is completely dissolved. Combine it with the solution in the beaker, add 10 ml of sulfuric acid, stir, precipitate the sulfate, and quickly precipitate it in a 300 ml beaker. After thorough washing, discard the residue. Heat the washing liquid and judge whether there is white smoke. Continue for 1 minute. Take 1 cooled, add 70ml of water and 2ml of nitrophenol. Adjust with water until yellow, then adjust with 1ml of bromine to colorless. Add 1ml of iron solution. Heat until slightly full, stir, add 3.5ml of high-pressure acid solution, cool to below 50ml, and dissolve in 20% original solution in a flask. Stir, dissolve with sodium vanadate until the purple color just disappears, stir vigorously to remove all bubbles, weigh into a 100ml dissolving bottle. Dissolve 8ml of distilled water, dilute to scale with rice. After 2min, measure the absorbance at a wavelength of 540nm on a spectrophotometer and at the same time measure the absorbance of the standard sieve series according to the regulations. Draw the standard working line:
Absorbance = C. 0.5, 1.0, 1.5.2.0, 2.5rl are respectively placed in 200ml flasks, and the following operations are carried out with the test tube. Question: Prepare a series of chromium trioxide solutions. According to the measured absorbance of the standard series solutions, the relationship between the concentration and the aurora density is used as the standard working line.
3.3.6 Calculation of separation results
According to the absorbance of the test sample, find out the corresponding amount of chromium trioxide from the curve, and calculate the content of chromium trioxide in the test sample according to the following formula:
Cr:O:()
In the formula, 1 is the amount of chromium trioxide in the test sample found from the standard curve. W is the sample weight g.
3.3.6 The relative deviation of the standard is 10%.
Additional Notes
1/r:0087.291
This standard was drafted by the Electronic Standardization Research Institute of the Ministry of Machinery and Electronics Industry and the Electronic Standardization Research Institute of the Ministry of Machinery and Electronics Industry. The main drafters of this standard are: Yun Guanghui and Liu Chengjun.
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