SJ/T 10939-1996 Analysis of cerium oxide in color picture tube glass SJ/T10939-1996 standard download decompression password: www.bzxz.net

UDC621.38.032.7:543.06
National Standard of the People's Republic of Chinabzxz.net
GB9474.4—88
Reduced to SJ/T10939-96
Chemical analytic methods for someelemencntsofcolorpicturetubeglassPublished on 1988-06-27
Published by the State Bureau of Standards
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Implemented on 1988-12-01
National Standard of the People's Republic of China
Analysis of cerium oxide in
color picture tube glass glass
GB9474.4—88
This standard specifies the analysis of electronic glass with an antimony oxide content of less than 0.3%, and is applicable to the analysis of electronic glass such as the glass shell of color picture tubes and black and white picture tubes.
This method should be analyzed in accordance with the provisions of GB9000.1 "General Principles of Chemical Analysis Methods for Electronic Glass". 1 Method Summary
The sample is dissolved in hydrofluoric acid and perchloric acid, and antimony is extracted with PMBP-petroleum ether solution under the condition of pH=5.5, and then cerium is back-extracted with 1mol/L hydrochloric acid solution. Then dibrominonitrochlorophosphonazo is used for color development and the determination is carried out on a spectrophotometer. 2 Reagents and solutions
2.1 Hydrochloric acid 1mol/L, 12mol/L
2.2 Hydrofluoric acid 40%,
Perchloric acid 70%,
Ammonia 25%,
2.5 Hydrogen peroxide 30%
2.6 Oxalic acid solution 5%
Potassium sodium tartrate solution 10% (prepared before use); 2.7
2.8 Methyl thiocyanate 0.05%,
2.9 Isocyanuric acid
2.10 Dinitrochlorophosphonazo (DBNCPA) solution 0. 04%; 2.11 Acetic acid-sodium acetate buffer solution pH = 5.5 Weigh 164g of anhydrous sodium acetate and dissolve it in water, add 16ml of glacial acetic acid, and dilute it to 1L with water. The pH value of the solution is checked with a pH meter and adjusted with acetic acid or sodium acetate;
2.12PMBP--petroleum ether solution 0.01mol/L Weigh 2.78B of PMBP (1-phenyl-3-methyl-4-benzoylpyrazolone-[5)), dissolve it in 1L of petroleum ether ( Boiling range 60~90C), release overnight, and absorb the upper clear liquid for use; 2.13 Antimony dioxide standard solution 0.50mg/ml Weigh 0.1250g of spectrally pure antimony dioxide that has been calcined at 750C for 30min, measure it in a beaker, add 30ml (1:1) nitric acid and 2ml 30% hydrogen peroxide, heat to dissolve, boil to destroy excess hydrogen peroxide, cool to room temperature, transfer to a 250ml volumetric flask, dilute with water to scale, mix well and set aside.
2.14 Antimony dioxide standard dilution 10ug/ml Transfer 10.00ml (2.13) antimony dioxide standard solution to a 500ml volumetric flask, add 5ml 12mol/L hydrochloric acid, dilute with water to scale, and mix well.
Approved by the Ministry of Electronics Industry of the People's Republic of China on April 29, 1988 YYKAONYKCa
Implemented on December 1, 1988
3 Analysis steps
GB9474.4—88
3.1 Accurately weigh 0.1000g of sample in a platinum dish, add a small amount of water to moisten it, add 5ml of hydrofluoric acid and 5ml of perchloric acid, heat and dissolve in a fume hood, smoke and dry it (be careful to prevent the sample from splashing), then add 5ml of hydrofluoric acid and perchloric acid respectively, heat the gastric smoke, and evaporate it to dryness. Use a little water to wash the four walls, add 1ml of 30% hydrogen peroxide, heat and evaporate to dryness. Add 7ml of 12mol/L hydrochloric acid to dissolve the residue (if it is difficult to dissolve, heat it slightly), then transfer it completely to a 50ml volumetric flask, dilute it to the scale with water, and shake it well. 3.2 Accurately transfer 2 ml of the sample solution in 3.1 to a separatory funnel, add 1 drop of 0.05% methyl orange indicator, 2 ml of 10% potassium sodium tartrate solution, adjust the solution with nitrogen water until it just turns yellow, add 4 ml of pH=5.5 buffer solution, add water to make the total volume of the solution 10 ml, extract once with 10 ml PMBP-petroleum ether solution and 0.5 ml of isoalcohol, shake vigorously for 1 min during extraction, let stand and separate, and discard the aqueous phase. Back-extract once with 10 ml 1 mol/L hydrochloric acid. Shake vigorously for 1 min during back-extraction, let stand and separate, transfer the aqueous phase completely to a 25 ml volumetric flask, add 2 ml 5% oxalic acid solution, shake well, then add 5 ml 0.04% dibromonitroazidophosphine solution, dilute to scale with water, and shake well. Use the reagent blank as a reference, and measure the absorbance at a wavelength of 640 nm using 1 cm colorimetry on a spectrophotometer. Note: ① Collect the organic phase, distill, and intercept the petroleum ether fraction at 60-90℃ for reuse. ② This reagent is a dilute needle colorimetric agent. Since the glass only contains cerium, this method is feasible. 3.3 Plotting the standard curve
Transfer 0, 0.2, 0.4, 0.60.8, 1.0 ml of the standard dilution of antimony dioxide to the separatory funnel respectively, and operate according to the following analysis steps. Take the No. 0 solution as the reference to determine the absorbance. And draw the antimony dioxide amount-absorbance curve as the standard curve. 4 Calculation
According to the absorbance of the sample solution, check the corresponding amount of antimony dioxide from the standard curve, and calculate the antimony dioxide content in the sample according to the following formula X
2×10-6
CeO2%=
Where: X is the corresponding amount of antimony dioxide found from the standard curve, u8W sample weight, g.
Additional Notes:
This standard was drafted by East China Normal University and the Institute of Electronics of the Academy of Sciences.
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