Methods of chemical analysis for glass raw materials for colour picture tubes-Methods for chemical analysis of litharge
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 lead oxide
Methods for chremicel tnalysis of litbatre1 Subject content and applicable scope
1.1 Content
/R 10087.5: 91
This standard specifies the analysis items and analysis methods of lead oxide, the raw materials used for the glass end of color picture tubes. 1.2 Scope of application
This standard is suitable for routine analysis or secondary analysis of the chemical content of color display tube glass materials. It is also suitable for the analysis of other raw materials for glass with similar technical requirements as follows: 2 Reference standards
GB9000. General principles for chemical analysis of electronic glass 3 Analysis methods
3.1 Analysis of lead monoxide
3.1.1 Summary of the method
The sample is dissolved in acetic acid. When pH is ~5, dimethylformamide is used as the indicator. EDTA standard is used for complex screening. 3.1.2 Reagents and liquids
. Acetic acid: 1:2;
b. Water. 1+1,
pH 5
Dissolve 250g of acetic acid in water, add 50ml of acetic acid, and dilute to 1nDam with water. 4. Dicresol solution: 0.1%
Dissolve the reagent 1 in 1ml 2% (source %) standard solution: 1.1m
Weigh 0.6538g of pure (99.99%) phenol, put it in a 300ml beaker, add 100ml water, 15ml 24% acetic acid, and add water dropwise. Heat to dissolve, cool and add to 1000° isotropic concentration, add to the scale. TH1TA standard solution 0.1 M amine aldehyde 3 solution in 1000% water 20 ml standard zinc absorption standard solution in 300 ml of non-burning solution, add about 90 l of water, oxidize with oxygen to pH = 5, add 1 ml of H5 buffer, add 20 ml of EDTA standard solution, titrate with EDTA standard solution, the color turns from yellow to yellow when the filter is full: A standard solution is calculated according to the formula: M = Mor
In the formula: - the density of EDTA standard solution: 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The concentration of zinc standard solution is 1. The volume of the standard solution is ml. 3.1.3 Test
Take the sample and dig it into a small amount (with a finger to check if there is no burning sensation for a long time), dry it in a 10:10 mixing oven for 21 minutes, and cool it in a tube. 3.1.4 Analysis steps
Accurately collect the sample 5.4 and put it in a 200ml beaker. Moisten it with water, add 20ml of 1:2 acetic acid, add solution, cool it, put it into a 20ml bottle, add water to the degree, absorb 26ml of 1260ml from the cup, add water to about 0.05, and adjust the drop to ~5 level with 10 drops of indicator. When the EDTA standard solution changes from purple to blue, it is the drop point. 3.1.5 Calculation of analysis results
The lead oxide content in the test is calculated by the following formula: D-3232 ×#××350 × 100bzxZ.net
Wherein, M》EDTA standard selected by W × 25
The width of the EDTA standard must be one volume.
1.
3.1.6 Precision or allowable error
The standard deviation is not more than 0.15%
3.2 Analysis of lead ions
3.2.1 Method report
The sample is aldehyde-free, exposed to acid, and the original manual absorption method is used to measure the actual content. 3.2.2 Reagents and solutions
. Enzyme acid:] 1 10,
h. Nitric acid, 1:1;
c. Standard sieve; 0.5m/m
Your stock has been cleaned to remove the surface aluminum. Use 1:1 to dissolve 15m, then add 1:1 acid, heat and wait until the store is enough to enter the latest water to help release the empty scale. 3. 2. 3 Receiver
Original light receiving diameter.
Hollow core alarm lamp,
Transmitter work new parts to the table!
New products
3. 2. 4 Try
SJ/I 10087.5-9:
Table Shangjin., 3 original absorption tooth treatment photometer this real work soft parts are real flow
[] 3. 1. 3 3.2.5 Analysis of the release of the sample. Accurately weigh 1.0% of the sample and place it in a 200°C oven. Add 1% water to moisten it and heat it to dissolve it. The slow wave is passed through with 1% vinegar until there is no reaction. Use 1% strong micro-particles! Dissolve nitric acid in a beaker and rinse the wave paper. Heat the paper in a heating box and cool it down. Then put it into a 100 μm plate and dry it with water until the sample is emulsified. According to the instrument conditions listed in the table, measure the single-line absorption of the sample in the dense liquid. 3.2.6 Calculate the absorbance of the sample according to the measured absorbance of the sample liquid. Calculate the height of the sample according to the following formula:
X=WVRE||tt| ... 7. The reagent is recommended to be less than 15% of the standard. 3.3 Analysis of chemical reaction The sample is dissolved in rutile acid, and the lead tetroxide is reduced by saturation. The precipitate is separated by saturation with acetic acid standard solution. The tetroxide is determined by saturation. 3.31 Reagents and reagents Glacial acid solution, 1:3; rutile: sodium thiosulfate standard solution ... 1. 3 Xi.
Weigh 5g of the sample and add 500ml of dry powder into a small glass bottle, add a little water to moisten the sample, add 10ml of acid to the test tube, add 1ml of iodine solution, cover it, start, wash the bottle and the bottle wall with water, and place it in a dark place for about 5 minutes. Use sodium thiocyanate standard to titrate the color of the material, and add about 2ml of starch solution, continue to add until it is colorless, which is the whole point. 3.5.5 Calculation of new results
The amount of the sample is calculated according to the following formula: .#0.3428×10C
Pb(%)
The volume of sodium thiocarbamide standard solution is 1.375 ml/min, and the validity of sodium thiocarbamide standard solution is 1.375 ml/min. The difference between the standard solution and the standard solution is less than 2%.
3.4 Analysis of three-step method
3.4.1 Summary
The sample is dissolved in iodine and the iodine is removed by YTA. After the iodine is reduced by hydroxylamine hydrochloride, the color is developed by isocyanate and the spectrophotometric method is used for determination.
3.4. 2 Reagents: 14% sodium chloride solution: 1% water. EDTA solution: 10% EDTA solution: 12% hydroxylamine hydrochloride solution: 1% hydroxylamine hydrochloride solution: 3.3% acetic acid solution: 1% acetic acid solution: 5mg/ml pure soft (9.UD0.1399 plus 1: [adjust acid 15ml heat solution. Boil to remove the carrier and cool, pour into a 5ml volumetric flask. Dilute to the mark with water, pipette 25 into a 1ml volumetric flask, add! ：【Hydrogen peroxide is dissolved in water to the mark. 3.2.3 Sample 3.1.8.
3.4.4 Step 3
Put 1.0g of the sample in a 10-mL beaker, add 1:1 molten acid, heat to dissolve, add hydrogen peroxide dropwise, and slowly evaporate until salts precipitate. Remove the beaker. After cooling, add 10ml of FDA solution, adjust the temperature to 5~=.5 with water, add 6ml of acetic acid, filter 1ml of acid, add 5ml of o-phenoxyethanol, bring to 1min in boiling water, cool to the bottom, transfer to a 5ml plate, add water to the scale, and add water. Select an appropriate colorimetric dish, use the reagent space as the ratio, and measure the absorbance at 510m. Drawing of standard solution: aspirate 0.2, 4.6, 10 ml of standard solution, add 10 ml of DTA solution, adjust the concentration to 5-5 with chlorinated water, add 5 ml of gelatin solution, 10 ml of hydrochloric acid solution, add 5 ml of 1% hygroscopic solution. Heat to 0.5 °C in a boiling water bath, cool, transfer to a 50 ml volumetric flask, dilute to 250 °C with water, shake to make a standard solution. Determine the absorbance of the standard solution under the same conditions as the sample solution: draw the curve between the absorbance and the change in light intensity of 22°C, which is the standard curve.
3.4.5 Calculation of analytical results
$./T 10087. 5.- - 91
From the absorbance data of the sample solution, find out its corresponding ferric oxide content from the standard curve, and calculate the corresponding ferric oxide content according to the following formula:
F0.0(5)-w10 × 100
Substituent 4: Find out the 1-B1 content of ferric oxide in the sample from the standard oil line.
3.4.E pin width
The relative standard error should be less than:
5.5 External determination of iron oxide
3.5. Method summary
Select a degradable chromogenic substance prepared by new sodium chromogen and determine it by spectrophotometry. 3.5.2 Reagents and saponins: 1:3, 1:3 nitric acid concentration: 33% Weigh 150 ml of saponin and dissolve it in 600 ml of water at a ratio of 1:1 to 1000 ml of nitric acid. Add 5 ml of hydrochloric acid sieve and 1 ml of new copper sulfate solution, and extract with ammonia until the color disappears. Remove the organic phase and set aside after filtration.
: Salt solution 1C% prepared on the same day according to the same method.
New Asian spirit. Day-two with odor > Standard solution: 91% ethanol; low
g peroxide, 1
copper standard solution, containing C0/m
weighing 99% pure 1598, add 111% of 1% of 1% of oxidizing agent in a 200ml beaker and heat it. Finally, after cooling, move it into a 100ml container, take the sample to the degree, accurately pipette 25 minutes and place it in a 50ml dish, and put it in the water. 3.5.3 Sample time 3.1.3.
3.5.4 Analysis steps
Weigh the sample 5ml in a beaker, add 1cm3 of kinetic acid, heat and dissolve, add hydrogen peroxide dropwise to clarify, stir to remove the oxides, cool to 250°C, add about 40% water, use 1:1 acid or grade 1 water as the ratio of 5. Add 5ml of hydroxylamine hydrochloride and shake to remove the scale. The bottle is about 30% full and contains 5ml of 30% 30% 5ml of ... Put 250ml of water and alcohol in a bottle, take it once every 5 minutes, add organic solvent and dilute it with ethanol until the end of the test. When analyzing the sample, the reagent should be analyzed at the same time: select appropriate ratio of blood and put it on the spectrophotometer. Use the reagent blank as the control to measure the absorbance at 16m. For the preparation of the standard curve, absorb 0.1, 2, 3.1, 5ml of the standard drop, respectively, and put it in a 125ml separation bottle, add water to dilute to about 40ml, add 12ml of taurine, adjust the concentration to 5. Add 1ml of amine, operate for 30s. Add 1ml of new 23-
$I/T10087.591
Ping Shuling, press, place for 3m, divide the 30ml into 25ml volumetric bottles without water, and then use the collection method. Combine the organic phase and bring the band to the scale under the same conditions as the test sample to calibrate the absorbance pressure of the liquid series, draw the control curve of the oxidation concentration and the absorption, and calculate the luminous data of the sample according to the corresponding oxygen content from the standard line break process. Calculate the required chemical content in the following formula: wxiokxICcCao(%) = Where: 1-the amount of chemical steel contained in the sample: 1-the amount of chemical steel contained in the sample. 3.5.5 Additional remarks for standard instruments: The automobile standard is under the jurisdiction of the Mechanical and Electronic Industry Electronic Standardization Research Institute, and is drafted by the Automobile Standards Company and the Mechanical and Electronic Industry Electronic Standardization Research Institute. The main drafters of this standard are Li Guanghui and Meng Chengjun.Adjust pl to 5. Add 1 ml of amine, operate for 30s.j new 23 --
$I/T10087.591
Ping Shuling takes 1 ml, presses, and places for 3m, then the 30 ml water-free layer can be placed in a 25m volumetric bottle, and then use m anti-collection method. Combine the organic phase and bring the band to the scale under the same conditions as the test sample to calibrate the absorbance pressure of the liquid series, draw the control curve of the oxidation concentration and the absorption, and calculate the luminous data of the sample according to the corresponding oxygen content from the standard line break process, and calculate the required chemical content in the following formula: wxiokxICcCao(%) = Where: 1-the amount of chemical steel contained in the sample, 1-the sample. 3.5.5 Additional remarks for standard instruments: The automobile standard is under the jurisdiction of the Mechanical and Electronic Industry Electronic Standardization Research Institute, and is drafted by the Automobile Standards Company and the Mechanical and Electronic Industry Electronic Standardization Research Institute. The main drafters of this standard are Li Guanghui and Meng Chengjun.Adjust pl to 5. Add 1 ml of amine, operate for 30s.j new 23 --
$I/T10087.591
Ping Shu Ling takes 1 ml, presses, and places for 3m, then the 30 ml water-free layer can be placed in a 25m volumetric bottle, and then use m anti-collection method. Combine the organic phase and bring the band to the scale under the same conditions as the test sample to calibrate the absorbance pressure of the liquid series, draw the control curve of the oxidation concentration and the absorption, and calculate the luminous data of the sample according to the corresponding oxygen content from the standard line break process, and calculate the required chemical content in the following formula: wxiokxICcCao(%) = Where: 1-the amount of chemical steel contained in the sample, 1-the sample. 3.5.5 Additional remarks for standard instruments: The automobile standard is under the jurisdiction of the Mechanical and Electronic Industry Electronic Standardization Research Institute, and is drafted by the Automobile Standards Company and the Mechanical and Electronic Industry Electronic Standardization Research Institute. The main drafters of this standard are Li Guanghui and Meng Chengjun.
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