Methods for chemical analysis for glass raw materials for colour picture tubes-Methods for chemical analysis of sodium pyroautimonate
Some standard content:
Electronic Industry Standard of the People's Republic of China SJ/1 10087. 1~~10087. 8—91
Chemical analysis methods for the main raw materials of color picture tube glass
Published on April 8, 1991
Implemented 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 sodium antimonate
Methods lor chrmlcal analysly of sodlum 1 Subject and scope of application
1.1 Subject
51/T10087.8—91
This standard specifies the analysis items and analysis methods of the raw materials of color picture tubes. 1.2 Scope of application
This standard is applicable to the thermal analysis of the raw materials of color picture tubes, and is also applicable to the analysis of raw materials with similar technical requirements using sodium phosphate. 2 Reference standards
GD 9UO.1 General principles of electron microscopy and analysis methods
3.1 Trivalent sodium phosphate: pre-analysis (high potassium volumetric method) This method is used as a standard for the analysis of divalent phosphate. 3.7.1 Summary
The sample is dissolved in sulfuric acid, the pentavalent rust is reduced to trivalent potassium with sodium sulfite, and then titrated with a peroxide standard solution. 3..2 Reagents and fluids
sulfuric acid;
ammonium sulfate:
sodium chloride;
sodium manganate standard solution: 0.12
weigh 3.3g high pressure 1000ml water, heat to boiling for about 1h. Place overnight. Use microporous glass to filter out the reducing substances that can be completely dissolved, and store the white precipitate in a clean place.
Calibration: weigh and absorb the car broken at 150--20%℃ (standard reagent 2.0~2.5g at 250m: customer test version, absorb to the scale 25ml3uUml Sanyao foreign brand Ul, heat to about 75~80 layers, use ionized potassium standard material to instantly determine the liquid red barrier 3, does not disappear to the full point. In addition, use the same body of water, add sulfur to conduct a vacuum test. The concentration of the standard solution of permanganate is calculated according to the formula, approved by the Ministry of Machinery and Electronics Industry of the People's Republic of China on April 8, 1991 32
1991-07.01 implementation
in A:
S1/T EC087.8-81
0×250
2×1000X(V-1a)wwW.bzxz.Net
The mass of potassium permanganate standard solution; The mass of potassium oxalate
The molecular weight of oxalic acid!
During calibration, the volume of potassium permanganate standard solution is 100 ml; air test, the volume of potassium permanganate standard solution is 100 ml; 3.1.3 Sample
Use a scaler to send about 21g of sample to be tested, and place it in a dry place at 110℃ for 2h and cool it down. 3.1.4 Weigh the sample 0.3g and burn it to 300m, and the magnetic field is 5 Heat, dissolve the acid in 151°C. Cover the surface, heat, stop heating and cool to a certain temperature, add water until it is 3. Add hydrochloric acid to 0.0 mL, shake well. Add anhydrous sodium thiosulfate, place for several minutes: put into the capillary tube, heat and boil for 20 minutes. Take out the capillary tube, cool the conical tube in cold water to 102°C, and use potassium permanganate standard solution to determine the red color while stirring. The end point is that the blank test is reversed with the sample at the same time. When calculating the results, deduct: 3.1.5 Calculation of analytical results
The amount of disulfide in the sample is calculated as follows: Sb:0, (%) = L× 0.cC7303 × < - Pe × 1002
wherein - the ratio of the relative concentration of the high-potassium hydroxide standard melt to 1; when dripping, the volume of the commercial potassium hydroxide standard liquid is 1, the blank test is based on the new fan to evaluate the volume of the standard liquid, mlF sample amount..
3.1.6 Precision
The relative difference is less than 0.2%
5.2 Analysis of dichloromethane (please use the acid concentration) This method is used for routine analysis of three-carboxylic acid dichloride: 3.2.1 Summary of the method
Dissolve the sulfuric acid with flowing acid until the decavalent ions are reduced to trivalent, and then titrate with a monovalent standard solution in a hydrochloric acid mass.
3.2.2 Reagents and solutions
Phytic acid:
Salt:
Sulfuric acid: Solid:
Conical acid:
Sulfuric acid pure standard solution, 0.1M
Take potassium sulfate Ce(S02:1H00.g) and place it in a 1m beaker, such as 20l of sulfuric acid, and heat to reduce the concentration. 33
SI/T 10087.891
After cooling, add 60ml of 1:1 brand slowly into 600ml of water and stir until completely dissolved, filter in 2 chambers, and dilute with water to 1000 nil.
Calibration: Accurately take 0.3g of pure 99.% or more in a 0.5ml beaker, add a small amount of water and 10ml of acid. Heat and cool to 3ml of 10ml acid and 30ml of 10ml of 10ml acid. Heat the solution to 80-90°C, and titrate with a standard titration under constant pressure. When the hour is approaching, heat the solution again to 80-90°C, and titrate until the red color disappears, which is the hour. The concentration of the acid standard solution (hours) is calculated as follows: M = Vx0.0B083
Where G
The volume of the sulfuric acid standard suspension during calibration, m. f. Formaldehyde: 0.1%.
Same as 3.1.3.
3.2.4 Analysis steps
Place the test piece in a 300 ml triangle oven, add 231° water, add 15 ml sulfuric acid. If the test piece is completely cooled, add 1 ml of hydrochloric acid, mix well, let stand for a few minutes, move to a high plate, heat the system for about 5 seconds, remove the cold water, and add 0.1 ml of hydrochloric acid. Heat the solution to 9°C, add 1M sodium hydroxide solution, and titrate with the standard solution. When the solution is close to the titration point, heat the solution to 80-90°C, and burn until the red color disappears as the end point. Perform the vacuum test under the condition of constant temperature.
3.2.5 Calculation of analytical results The maximum content of dioxide in the sample is calculated as follows: (2034%) = ± × (-) × 0. 07288 × 00
Change the concentration of the acid standard solution:
During the titration, the volume of the acid standard solution consumed is 1, and the volume of the acid standard solution consumed in the vacuum test chamber is 1, and the sample is weighed.
Relative standard value is less than 0.2%
3 Analysis of potassium oxide and sodium hydroxide
3.3.1 Method summary
The sample is treated with hydrogen peroxide and sulfuric acid and sealed in a weak jar to prevent the sieve salt from hydrolyzing. Phase atomic absorption and spectrometry. 3.5.2 Reagents and solvents
Hydroxyacid, chlorine:
Sodium hydroxide. Standard solution: Take N200.6n/ml. K: 0.1/i. Sodium chloride and chloride are heated to 500~0 for 5 minutes, then taken out and cooled in a desiccator. Weigh sodium hydroxide 34
S10087.8-91
0.425g and potassium hydroxide 0.1583g, add water to a 1D00ml volumetric bottle to dissolve and dilute to the scale. 3.2.3 Instruments and their working documents
Atomic absorption spectrophotometer.
Hollow cathode lamp.
Only for working documents, see Table 1.
According to the working plan agreed by the AA-640-13 atomic absorption spectrophotometer of the island ocean, see Table 1
Determination of elements
3.3.4 Samples
JM 3.1.3 Parent.
3.3.5 Steps
Analysis line wavelength
Light source
Heater temperature
Combustion gas standard, L/min
Accurately weigh the sample.5L/min in a platinum resistor, moisten with water. Add 10ml of hydrogen alcohol+, shake well, place on a plate for 6min, add 1ml of sulfuric acid, uncover, put sand on and heat (to prevent sudden violation) until white smoke appears, stop heating, cool to room temperature, add 20ml of dissolving acid, and water.Dissolve. Transfer to a 250ml volumetric flask and adjust to the scale with water: Determination of sodium chloride, take 5ml from the 250ml test solution and add it to a 100ml volumetric flask. Adjust to the scale with water. Instrument working requirements Determination of the absorbance of sodium oxide and potassium oxide in the test solution: Directly measure the absorbance of potassium chloride by the instrument working table after the remaining part of the test solution after the oxidation is removed. Drawing of standard curve: 1.3.3, 15ml of the standard solution of potassium chloride and sodium oxide are respectively added to 100ml, and the water is adjusted to the scale to form a mixed standard solution series. Connect the instrument working recorder, and adjust the absorbance of sodium oxide and potassium oxide in the mixed standard solution series together with the sample, and draw the relationship between the concentration of sodium oxide and potassium oxide and the absorbance, as the working curve of sodium oxide and potassium oxide. 3.3.6 Analysis of the results Based on the measured absorbance of the sodium fluoride and potassium fluoride in the sample, the corresponding sodium fluoride and potassium fluoride are obtained from the working curves of sodium oxide and potassium oxide respectively. Then the sodium oxide and potassium oxide content in the sample is calculated according to the following formula: 4 × 250 × 100 NaO3) (000 × 5 × F) Ko (%) Where: A = 1000 × W + mg potassium fluoride content found on the working line: A = mg potassium fluoride content found on the working curve + mg potassium fluoride content found on the working curve. 3.3.7 Density The relative standard deviation of the oxide is less than 3%. The relative standard deviation of oxidation inhibition is less than 7%, 34% analysis of trioxide monohydrate
3.4.1 Method summary
S3/T 10DB7, 8·-91
The sample is hydrolyzed with hydrochloric acid, potassium hydroxide is used to inhibit the hydrolysis, and the iron is reduced to monovalent iron with hydrochloric acid, and the obtained value is controlled to be between 4.6 and 6.5. The color is developed by Sulla colorimetry and the determination is performed by spectrophotometry. 3.4.-2 Reagents and solutions
A. Hydrobromic acid,
B. Phenanthroline solution: 25%
Weigh Phenanthroline G25 in 200 ml of boiling water and add 5 ml of water. Heat the solution and cool to room temperature, and dilute to 100 ml with water.
c. Potassium sodium tartrate solution: 25g potassium sodium tartrate (KNO3H2O2) 250g in a 1000ml beaker. Add about 550ml water, heat to dissolve, add 20ml saline solution and 20ml pyraclostrobin. Boil for 2min and cool to room temperature. Transfer 100ml of the 10% chemical solution to the flask, remove iron with a certain amount of water, until the organic phase is colorless, discard the organic phase, add the aqueous phase to a 15ml bottle, water to the scale, and accurately hook.
Continue with this article: Potassium tartrate monohydrate is coated in the same way as above, e. Salt solution: 10%
Weigh 100 g of hydroxylamine hydrochloride and place on a 1600 ml baking pan, add about 100 ml of water, and remove the residue with the same method as the potassium sodium tartrate solution in this article. Standard solution: FeO2, S/m
Weigh 3.1399 g of pure sodium hydroxide (9.99% or more), add 15 ml of 11% sodium hydroxide, heat and decompose, drain 1 ml, cool and weigh into a 10 ml volumetric flask, dilute with water to 60°C, standard solution. Take 2 ml of sodium hydroxide and place in 1000 ml of broth, dilute with water to 60°C.
5.4.3 Sample
Same as Article 1.3.
3.4.4 Steps
Collect 0.5g of indigo plant in 100ml flask, add hydrogen peroxide for 5m. Heat until completely dissolved, and heat at nearly boiling point until it falls off the filter. Remove and cool, add 2ml of sodium acetonide solution and 2ml of hydroxylamine solution to dilute with water to 30°C, heat in a water bath for 2 hours, remove and cool to room temperature, until the water content reaches 0.10°, follow the steps: make a blank test with the corresponding components, colorimetric blood around 3cm, measure the absorbance at 5.10° with the reagent blank as the comparison. Drawing of standard curve: Take 150ml of standard iron solution with concentrations of 0, 2, 1, 6, 8, 0.12m, etc., and add 5ml of 1:1 concentrated sodium hyaluronate solution of 1.5m, 2ml of concentrated hydroxylamine hydrochloride, etc. Dilute with water until smooth. Add 2m of water, cool to room temperature, mix with water, and form a series of standard solutions. Measure the absorbance of the standard solution under the same conditions as the sample solution, and draw the relationship between the absorbance and the standard curve as the standard curve. 3.4.5 Analyze the absorbance of the test solution, find out the corresponding amount of iron 2 oxide from the standard curve, and calculate the content of iron 2 oxide in the sample according to the following formula:Dilute with water until smooth. Add 2m of the solution, cool to room temperature, and mix with water to make a standard solution. Measure the absorbance of the solution under the same conditions as the sample solution, and draw the relationship between the absorbance and the standard curve. 3.4.5 Analyze the absorbance of the test solution, find out the corresponding amount of ferric oxide from the standard curve, and calculate the content of ferrous oxide in the sample according to the following formula:Dilute with water until smooth. Add 2m of the solution, cool to room temperature, and mix with water to make a standard solution. Measure the absorbance of the solution under the same conditions as the sample solution, and draw the relationship between the absorbance and the standard curve. 3.4.5 Analyze the absorbance of the test solution, find out the corresponding amount of ferric oxide from the standard curve, and calculate the content of ferrous oxide in the sample according to the following formula:0.1936B· After solution, transfer to a 1000ml volumetric flask. Dilute with water until mixed, draw 23ml of sample into a volumetric flask, dilute with water, shake well, and record. 3.5.3 Sample
3.i.3.
3.5.4 Analysis step
Accurately weigh 1.08 of sample into 20ml of pre-irradiated solution with 1g of magnetic acid agent, then add 3g of sodium carbonate, mix for about 2 minutes, and then cover with sodium carbonate, and calcine in a muffle furnace at 70°C. Cool to a temperature of 1000, rinse with 40ml of water, heat the sample to boiling for 2~3 minutes, and cool to room temperature. Transfer to a 50ml bottle and dilute with water for two minutes. Mix and filter. Pipette 25ml of the filtrate into a 1ml beaker, neutralize with 1,1 mol of acid until no bubbles are generated, and then sieve for 5 minutes. That is: 1 mol of phosphoric acid (0.5M), add 2ml of solution, add permanganate solution (0.5ml), heat to a certain point, cool, add 2ml of urea solution, drop by drop, sodium nitrate solution, potassium permanganate solution, and then add dimethoate solution to the bottle until it becomes stiff, mix and place for 20ml.
The air test was carried out under the same conditions. Using 3 colorimetric methods, the test oil was used as the reference to determine the best absorbance and draw two lines: the absorption of 0.05% carbon dioxide and 12% carbon dioxide respectively in a 1mm beaker. Add water to 25% ir:l. Add 0.05% 1:1 sulfuric acid, 0.06% 1:1 phosphoric acid, 2ml ferrous solution and 0.2t molten manganese. Add 2ml of the cold solution, until the red color of the solution fades, transfer it to a 50% volume plate, add diphenylcarbazide, add water to the mixture, and place it in a standard series of solutions. Under the same conditions as the test oil, the standard series of solutions were determined and the optical density and light change of the standard series of solutions were determined. The relationship between the concentration and the absorbance was used as a marker. 3.5.5 Calculation of the analysis of the results
The corresponding content of carbon dioxide was found from the standard curve by the absorbance of the test solution. $1/r 10087.89:
Cr0(%)=WX10
Wherein: A-The content of chromium trioxide in the filter is determined by checking the standard curve: weigh the sample +
3.5.6 Precision
The relative standard error is less than 10%.
3.B Analysis of oxidation
3.6.1 Summary of method
The sample is decomposed with chlorine dioxide and dried, and the color is developed with a reagent. The colored complex is obtained and determined by spectrophotometry. 3.6.2 Reagents and solutions
Hydrogen flow,
EDTA Solution: 5%;
Copper reagent: 0.5%
Ammonia water;
Potassium tartrate solution: 10%
Weigh potassium tartrate (KaC.HO.4HO) 40g in a 100ml beaker, add about 500ml water. Heat to dissolve, cool and add 1% phenolic peptide solution 0.05ml, neutralize with nitrogen water until slightly red, transfer to a 1000ml decanter, add appropriate amount of other reagents, extract with nitric acid to remove chlorine, until the organic phase turns yellow, discard the organic phase - transfer the aqueous phase to a 1000ml container, dilute with water to several degrees, precipitate evenly.
h, ethyl acetate solution: 1%;
. Copper standard: us/m
Weigh 8g of pure chlorine above 99.9% in a beaker: 1% nitric acid, heat to dissolve, drive out nitrogen and oxygen. Remove the residue and put it into a 100ml container. Drain the sample with ethanol to the mark, filter, and absorb 25ml into a 5ml container. Dilute with water until the mark is wet. 3.6.3 Sample. Same as 1.3. 3.6.4 Analysis step. Take a 1.0% sample into a 16 ml beaker, add 4 ml of ethyl acetate. Heat and evaporate until dissolved. Remove and cool slightly, add 1 ml of nitric acid, heat to dryness, remove and cool slightly, add nitric acid. Heat and evaporate until the volume is about 1 m, remove and cool, add 1 ml of ethanol and 10 ml of water. Wait for half a minute and remove. Add LYTA to 60ml of the source, add 1ml of ethanol, and dilute to 30ml. Use water to neutralize until the red copper reagent is reduced to 2ml, shake for 2 minutes, and stratify. Use the corresponding system to do a blank test, transfer part of the organic matter into the colorimetric medium, and use the reagent blank as a reference to measure the absorbance width at 140mm. Preparation of the standard curve: absorb 0, 1.2, 3, and 1.5ml of the standard respectively in 60ml of the source, add 2ml of water, 2ml of hydrochloric acid, 2ml of EDA solution, and 0.11ml of phenol and ethanol solution. Neutralize with water until the red copper reagent is reduced to 15ml, and the bacteria are 3mm. Measure the absorbance of the standard solution under the same conditions as the sample: draw the relationship between liquid concentration and absorbance as the standard curve, calculate the absorbance of the sample solution, and use the standard curve to calculate its concentration. Then calculate the content of oxides in the sample: Cuot%wxi. Use the standard curve to calculate the melting point of the sample. 8 Special envoys
batch standard adjustment small 16 devices
additional instructions:
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