Methods of chemical analysis for glass raw materials for colour pictrue tubes-Methods for chemical analysis of feldspar
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 of feldspar
Methods for chomical analysls of feldspar1 Subject content and scope of application
1. 1 Subject content
S/T 10087. 3 --9'
This standard defines the analysis items of feldspar used as the raw material of color picture tube glass. 1-2 Scope of application
This standard applies to the routine analysis of raw materials for color highlight glass tubes; it is also applicable to the analysis of raw materials for black picture tubes and other technical requirements. 2 Reference standards
2.1 G9000.1 General chemical analysis methods for electronic glass: 2.2 SJ! 0D37.2 Chemical analysis of clouds
3 Analytical methods
3.1 Analysis of dihydrogen hydride
5-1.1 Method description
Use dihydrogen hydride to treat the sample. Then, dissolve it in non-acidic solution and combine the solution with EDTA standard solution under appropriate conditions. Then, add sulfuric acid standard solution to saturate the EDTA with a fixed pump. 3.1.2 Reagents and solvents
Blue: 1 1, 1 2, 2:
Hydrogen hydride,www.bzxz.net
Reagent 1.1
Acid: 1:
EDTA standard solution: 0.C2M
Take 7.68 sodium disodium ethylenediaminetetraacetate, dissolve it in water and dilute it to the mark in a 1000ml volumetric plate to obtain calibration.
Calibration: Accurately pipette 25ml of the prepared EDTA standard into a 900ml conical flask, add 10l of pH 5.5 buffer solution and 2-3 drops of orange indicator, and titrate with 0.02M zinc standard solution until the solution changes from yellow to red, which is the end point. Record the readings and calculate the original concentration of the EDTA standard solution. 1. Zinc standard solution: 0.02M zinc (U%>0.6538), 50ml water, 7.5ml 2+1 hydrochloric acid, read 5ml water. Heat to dissolve, cool and transfer into a 500ml bottle, and filter with water. B. Copper acid standard zinc solution: Accurately weigh the dead acid preparation [CuO,·2O>1Gs and transfer to 1000ml of the original through the sieve. Sieve with E, can be accurately absorbed 1>rA standard submersible 20ml with 1:1 nitrogen water and 1:1 hydrochloric acid to 2--3. Use 1 red test paper Test, heat to a temperature of 1 mol, add 5 ml of Cu-PA solution, about 1 ml of 6-base solution, drip the standard solution with sulfuric acid, add 10 ml of ethanol near the end point, and continue dripping until the solution turns purple-red. Calculate the value below:
The ratio of the ELXTA standard solution to the EDTA standard solution;
The volume ratio of the EDTA standard solution to the EDTA standard solution,
3. 1. 3.1.4 Steps
Take 5 samples of the test piece and wet them with a little water until the acid is completely absorbed. Heat them in a bath until the sulfuric acid emits white smoke, cool and continue heating with acid. Cool, heat with 25l of 10ml of salt water and dissolve thoroughly, and transfer the portion to a 253ml volumetric flask with a water wheel: A Test wave.
Absorb 50m of A test solution and add standard water to wash it in the 300m-high frequency. 1: Adjust and 1: Water retreat H is 2~3, with a special red test low control test, put it on the electric protection heating energy boiling plate, so that DTA and along the road platform are fully added. Add hexamethyleneamine: 6 u-PA as the reference agent, and the acid standard sodium sulfate is dripped with excess ETA. The end point is when the grass turns red. 3.1.5 The calculation of the results of the test
The lead trioxide content in the test is calculated as follows: A,.(%)
:tda,a --
)X250130
2×CX H
The molecular weight of the chemical
EDTA standard solution:
The volume of the standard solution, ml:-the ratio of EDTA standard solution to sodium sulfate standard solution: F g
3.1.6 The concentration of the standard solution is less than 5%.
3.2 Analysis of trioxide
3.2.1 For the purpose of summary
, 3.1, 1 test section is used to monitor the reduction of iron hydroxyl groups, the adjacent non-color development, the separation is optical change determination. 3.2.2 Reagents and Reagents: Hydrochloric acid: 1:1; Hydrochloric acid is chromium-ammonium chloride, 10+ alcohol solution: 62% distilled water: 0: alcoholic acid: 0: 0.2% S/T 1CO87.3-91 Take 1 ferrocyanide solution, dissolve it in 50ml of 95% alcohol, and dilute it to 550ml with water. Accurately dissolve 6.0:6 ammonium ferric acid in 1:6 sulfuric acid. 1. Transfer to a 100 ml volumetric flask, and dispense 10 ml into a 10 ml volumetric flask, dilute to the mark with water - this solution contains 1.31 mg/ml of ferric oxide. 3.2.3 Optional 3.1.3, 3.2.4 Analysis Step 8, take 3.10 ml of test solution, add 1 drop of 13% acid 5 ml of water to adjust the color, then pass 1-2 drops of water through the color plate, shake well, add 0.2 ml of non-penetrating water, and place it along the plate. Fully color, on the spectrophotometer, measure the absorbance at 51nm with the standard solution: b. Standard curve
Pipette three-carboxylic acid two-soft standard (1.1 yuan g/ml) 5.10.15, 23.25ml respectively 122m) into the bottle, add 1~2 cups of base age indicator, 0% tartaric acid, add hydrogen peroxide to yellow and then add hydrochloric acid to colorless and add 1~2 drops of water to about 80m After adding 10% hydroxylamine 2m, 0.2% o-hydroxylamine 5rl, measure the absorbance of the sample and finally make a correlation curve between the absorbance of ferric oxide and the absorbance as the standard. 3.2.5 Calculation of analysis results Based on the measured test solution and the concentration of ferric oxide, find out the corresponding content of ferric oxide from the standard working line and calculate the total amount of ferric oxide in the sample according to the following formula: AX 250 X 100 The amount of ferric oxide in the sample was measured... 3-2.6 The auxiliary density was 5% smaller than the standard. 3.3 Analysis of sodium hydroxide and sodium oxide 3.3.1 The test sample was treated with hydronitric acid and mineral acid, and then dissolved. Potassium hydroxide and sodium hydroxide were respectively used for absorption spectrophotometry. 3.3.2 Reagents and reagents were added. Sulfuric acid: 10%; potassium hydroxide and sodium oxide were mixed and dissolved to make sure that the potassium hydroxide content was 0.1 g/l each.-(33) Potassium chloride and sodium oxide were respectively dissolved in 500-60 °C for 5 min, and cooled in a dryer to catalyze the absorption of N3/r 10087.3.9: 5.1583, 13338 sodium chloride water: 10303. 3.3 Instrument and its working record
The absorption spectrum is assumed.
Hollow core light lamp,
Recommended working conditions are shown in Table 1.
Energy elements
3.3.4 Test ladder
3.1.3,
3.5.5 Analysis steps
The Shimadzu A·G1 spectrophotometer is set to 1 operating system and wavelength
Combustion height
Heat volume, L/m
Accurately collect 0.10g sample in the center of the pin, moisten with water, and measure the hydrogen atmosphere potential 2Um.Comb 5-10 drops: Heat on high heat to emulsify hair, wash with water for nearly a thousand seconds, add 5ml of oxygen, continue adding, continue to add as much as possible for 3-5 minutes, cool to the minimum. Water 30-10ml: Heat in a water container to dissolve, put in a 500ml container, dilute.
Absorb 50 ml of the filtered solution into 100 ml volume, dilute with water, and simultaneously determine the atomic absorption sensitivities of potassium oxide and sodium oxide with the obtained standard solution. Prepare the absorption line-concentration curve as the standard working line: absorb the filtered standard solution into 5, 15, 20, 25 ml bottles, dilute with water until the solution becomes neutral. 3.3.6 Calculation of analysis results
Obtain the measured atomic absorption sensitivities of potassium oxide and sodium oxide in the test sample, and substitute the corresponding chemical values from their respective working lines. Calculate the content of sodium oxide in the sample using the following formula: 600 × :00 × 4
UU? X b0 XW
b00 × 100 X t
Na0%)=10e×50×W
A. The potential of potassium permanganate in the station is obtained by the typical line. 1. I checked the sodium permanence in the station. 3.3.7 The precision width of the machine and the standard band interval difference are less than 2: 3.4 Analysis of chromium trioxide 5.4.1 Summary of the method: Same as S.1/): JCC87. 2 Article 3.3.1: 3.4.2 Test solution: SJ/T10087.2 Article 3.3.2: 3.4.3 Test sample: Same as 3.1.3.
5.44 Analysis Steps
S1/T10087.391
Wet the feldspar with water, heat evaporate the sulfuric acid on a sand bath, and wash with water, then add domestic acid to continue heating until the sulfur smokes. Cool and drain with water. When the smoke has stopped, cool, add water, heat on a water bath, fill with paper, and add hot water. Collect the washing liquid in a 260ml beaker, and control the volume to about 70ml. Add 1 ml of p-nitro indicator, adjust to yellow with hydrogenated water, then adjust to colorless with distilled water for 3 min, and then add 5% potassium phosphate solution for 4 min. Heat slightly while stirring. Bring the volume to below 8 ml, remove and cool. Add 20 ml of 205% urine, stir, add 10 drops of sodium ion solution until the color of potassium permanganate disappears, stir vigorously, transfer to a whole bottle after all bubbles are exhausted, add 2 drops of the solution and spread evenly, simmer with water until 2 min, and measure the absorbance at the same time on a spectrophotometer at a wavelength of 5UUnm.
The standard working curve is prepared by absorbing chromium standard solution of 0, 0.5, 0.1.5, 2.0:2.5. respectively in a 200 μm beaker, and the following operation is performed to prepare the standard solution: the relationship between the concentration and the absorbance is plotted as the standard working curve. 3.4.5 Calculation of analysis results
The absorbance of the tested sample is measured by the standard line to find out the content of chromium trioxide. The maximum content of chromium trioxide in the sample is calculated according to the following formula:
1 × 16G
The content of chromium trioxide in the test solution is checked by the standard line, S: or
--8
5-4.6
The difference with the standard is within 10%.
Additional Date:
This standard is prepared by the Electronic Standardization Research Institute of the Ministry of Machinery and Electronics Industry. The Electronic Standardization Research Institute of the Ministry of Machinery and Electronics Industry is responsible for this standard. The main drafters of this standard are Li Guanghui and Li Guanghui.
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