Methods of chemical analysis for glass raw materials for colour picture tubes-Methods for chemical analysis of Sodium fluorosilicate
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
Issued on April 8, 1991
Implementation on July 1, 1991
Issued 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 of sodium fluorosilicate
Mh:dhpds for chrmleai anulysis ol sodlum hexutluorsiticale1 Subject content and applicable scope
1.—Subject contentwwW.bzxz.Net
S/T 10987.7—97
This standard specifies the analysis items and analysis methods of sodium fluorosilicate used as raw material of color picture tube glass. 1.2 Scope of application
This standard is applicable to the analysis or secondary analysis of chlorosilicic acid waste raw materials of color picture tubes. It is also applicable to the analysis of other glass raw materials with similar technical requirements. 2 Reference standards
C 9093.1 General principles for chemical analysis of electronic glass 5 Analysis method
3.7 Analysis of sodium silicate
3. .1 Summary
The sample is dissolved in water and heated. The hydrolysis reaction is determined by the presence of NaSiE+ 3H.O-?NaF--SiO+ HF
The standard sodium hydroxide solution is dissolved and the hydrogen fluoride released, thereby calculating the content of sodium silicate. 3. 2 Reagents and solutions: Hydrogen hydride standard solution: 1 M sodium hydride, accurately weigh 0.1% sodium hydride, use solvent that does not contain carbon monoxide, weigh to 1000. Add the newly prepared oxidation saturated flow to precipitate again, change the hook and let it rest for a few days, then transfer the above solution to single material for single calibration: take amino acid (standard reagent>2~2.5B, put it in a 300℃ flask, add 100M water without carbon dioxide, dissolve it with phenol blue as indicator: titrate with the prepared sodium hydroxide standard solution, the color changes from back to blue, which is the end point, calculate the accuracy of sodium hydroxide standard solution according to the formula: the concentration of sodium hydroxide standard solution; approved by the Ministry of Machinery and Electronics Industry of the People's Republic of China No. 1331.34-08 28
implemented on July 1, 1991
SI/T 1D087.791
During titration, the volume of sodium hydroxide standard drop is consumed, mb. Acid indicator: 1%
Weigh 1 ml of sodium hydroxide, add 90% sodium hydroxide (95%) solution, and dilute to 130ml with water. 3.1.3 Test
Use the reduction method to take about 20ml of the sample to be tested, grind it in a mortar and grind it into fine particles. When rubbed lightly with fingers, it should be 100ml. After drying for 1 hour, place it in a gas burner and cool it down
31.4 Steps
Accurately weigh 1.0ml of glass sample in a 500ml triangular beaker, add 20ml of water. Heat to dissolve the sample. After cooling, add 5 drops of phenolic acid indicator. Filter and determine with sodium hydroxide standard drop until the liquid turns red, which is the end point. 3.1.5 Calculation of analytical results
The content of sodium silicate in the test sample is calculated according to the following formula: Na SiFa(1 - M --P 34701 × 100w
Wu Zhong: Group
Oxidation standard solution concentration:
The volume of the standard solution consumed by the titration is .ml, the sample volume is .,
3.1.6 Density
Relative standard period is 0.15%.
3.2 Analysis of ferric oxide
3.2.1 Six abstracts
The sample is treated with perchloric acid, the silicon and chlorine are evaporated, and then the residue is dissolved. Add sulfuric acid to dissolve it, and form a gastric acid complex with iron, and measure it with a grid photometer:
3. 2. 2 Reagents and solutions
B High acid
Nitric acid: 11:
Ammonium thiocyanate solution: 10%
Weigh 5g of sulfuric acid powder in 500ml and calcine, dissolve at 1.1 ℃, and dilute to 5nnml. Store in a reagent bottle. e. Standard solution of ferric oxide: Fe2O3, 3.01mg/ml. Take ferric sulfate (CNHF(S)), 12HO: U.e0.4g. Dissolve in water and put into a 1000ml container, and measure with a water release chamber.
5.2.3 Sample
Same as 3.1. 3.
3.2.4 Analysis Steps
Weigh 5.0% of the test solution accurately and place it in a sand bath. Add 5 ml of sodium chlorate and stir well. Heat on a sand bath until the smoke disappears. After cooling, add 5 ml of peroxy acid until the smoke disappears. Cool and wash the residue in the solution into a 1Dal beaker with a small amount of water. Add 15 ml of saline and 5 ml of nitric acid, heat and dissolve on water for 30 min. After cooling, pour into a 2S Cml volumetric flask and dilute to 1 degree. This is test solution A.
Put 50 ml of A in a 10 ml equal volume flask, add 5 ml of sodium chlorate, shake and add water to the sample. Follow the steps for sample analysis and prepare the sample blank solution at the same time: use the sample blank as the control and use 1 cm colorimetric blood to determine the absorbance at 1a0nm. 29-
SI/T 10087.7·-91
Preparation of the standard curve of the sample: Pipette 0, 24, 6, 6, 10 ml of the standard ferric oxide into 100 ml of the volume, add cyanide solution for 5 minutes, and separate them into a standard wave series with water. Determine the absorbance of the standard series with the same sample, and prepare the curve of the absorbance of ferric oxide and the absorbance as the standard working curve, 3. 2. 5 Calculation of analysis results
According to the measured absorbance of the sample solution, find the corresponding ferric oxide concentration on the standard curve and calculate the content of ferric oxide in the test sample according to the following formula:
AX250X1DD
Fe (%)=
100X0XW
Where: 4 is the concentration of ferric oxide in the test sample found on the standard curve; W is the concentration of sample.g.
3.2.6 Density
The relative standard deviation is less than 0%
5.5 Analysis of phosphorus pentoxide
5.31 Key points
Phosphorus reacts with vanadate and chromogen in the color developer solution in an acid medium to form a polyhydric solution. The content of vanadate in the sample is calculated by measuring the absorbance.
3.3.2 Reagents and standards
b. 1.
Colorimetric analysis
Weigh 1.2g of metavanadic acid in 10ml of water. Add 250ml of amber acid and dissolve until completely dissolved. Weigh 2g of vanadic acid and dissolve it in 30ml of water (if necessary), mix the two drops evenly, dilute to 1m with water, mix well, and transfer to a color reagent bottle for 4 hours. Store in a dark place.
d. Chemical Group II Standard Solution: Containing P: mg/a1. Dry potassium monohydrogen phosphate at 110°C for 2 hours, then cool in a 1000 mL flask and dissolve in water. Transfer to a 1000 mL flask, add nitric acid, add water to the mark, and shake. 3.3.3 Test sample
Same as 3.1.3.
5.3.4 Dispersion test solution
Put 10 ml of the test solution in 3.2. in a 100 mL flask, add 2 drops of phenol indicator, and spread evenly. Neutralize with 1:1 hydrogen water to yellow, then adjust to colorless and add excess "full", add color developer, shake with a spoon to dilute until dilute, set to 30, and compare at 1m, using the reagent manufacturer's own as a reference. When drawing the standard, take 0, 2.4.6, B, and 1D of the phosphorus oxide standard and place them in 100 ml mother bottles respectively, dilute to about 1 ml, first add 2 drops of 1% nitrophenol indicator and adjust to shade, then add 1% aldehyde to make it colorless and pass through a plate 1. Add 20ml of colorimetric reagent, shake and dilute to the mark with water. After 30 minutes, measure the absorbance of the standard series wave with the test solution, and finally prepare the correlation between the phosphorus pentoxide and the absorbance as the standard curve. 3.3.5 Calculation of analytical results
According to the measured absorbance of the test sample, find the corresponding phosphorus pentoxide from the standard curve. Calculate the phosphorus pentoxide content in the sample according to the following ratio:
T000WX10X100
SI/T 10087.7-91
Where is the maximum amount of phosphorus pentoxide in the test solution on the standard curve: F sample amount·B
3.3.6 Precision
Frame deviation from approval is less than 10%
Additional remarks:
This standard was drafted by the Electronic Standardization Research Institute of the Ministry of Machinery and Electronics Industry. This standard was drafted by 40 factories and the North China Standardization Research Institute of the Ministry of Machinery and Electronics Industry. The main drafters of this standard are: Ben Guanghui, Liu Mingjun.
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