SJ/T 10553-1994 Emission spectral analysis method for impurities in zirconium dioxide for electronic ceramics SJ/T10553-1994 standard download decompression password: www.bzxz.net

Electronic Industry Standard of the People's Republic of China
Method of emission spectrochemical analysis of impurities in ZrO,for use in electron ceramics Subject content and scope of application
1.1 Subject content
This standard specifies the emission spectrochemical analysis method of impurities in zirconium dioxide for use in electron ceramics. 1.2 Scope of application
SJ/T10553--94
This standard is applicable to the determination of oxide impurities of iron, silicon, phosphorus, calcium, magnesium and titanium contained in zirconium dioxide for use in electron ceramics. 2 Summary of the method
Zirconium dioxide and graphite powder mixture (containing 1% cobalt trioxide) are mixed evenly. The graphite powder acts as a buffer and diluent to stabilize the excitation. Cobalt and zirconium are used as internal standards. The spectra of the sample to be tested and the standard sample are photographed on the same spectrum dry plate. The impurity content is determined by the internal standard method.
3 Reagents or materials
Iron oxide
Silicon dioxide
Magnesium pyrophosphate
Calcium carbonate
Titanium dioxide
Zirconium dioxide
Cobalt oxide
Graphite powder
Spectral dry plate
Analytical pure;
Analytical pure;
Analytical pure;
Analytical pure;
Analytical pure Pure
Spectrally pure;
Analytically pure;
Spectrally pure;
Domestic Type 1;
Metol-Hydelu developer and fixer (prepared according to the recipe in the instruction manual of the spectral photographic plate); graphite electrode
Instruments or equipment
Medium-sized spectrograph;
AC arc generator;
Microphotometer:
Spectrally pure, diameter 6+mm.
Approved by the Ministry of Electronics Industry of the People's Republic of China on August 8, 1994, and implemented on December 1, 1994
Spectrometer:
Analytical balance
SJ/T10553-94
Sensitivity 10-*g:
Small lathe for turning graphite electrodes,
Agate mortar;
Stopwatch.
Preparation of standard samples
Zirconium dioxide and each oxide to be tested are burned at 900℃ for 2h, magnesium pyrophosphate is burned for 4h, and calcium carbonate is dried at 150℃ for 2h. According to the calculated amount, various impurity oxides and salts are added to the zirconium dioxide to prepare the main standard sample, and then diluted one by one with zirconium dioxide to prepare a set of standard samples, the content of which is shown in Table 1. Then mix with an equal amount of graphite powder (containing 1% cobalt trioxide). Table 1
Main standard sample
Standard sample No. 1
Standard sample No. 2
Standard sample No. 3
Standard sample No. 4
Standard sample No. 5
Standard sample No. 6
5.2 Sample treatment
Impurity content
The sample is mostly in lumps and should be carefully ground until the particle size is similar to that of the standard sample (can pass through a 200-mesh standard sieve) and mixed with an equal amount of graphite powder (containing 1% cobalt trioxide). 6 Analysis steps
6.1 Load the treated sample into the small hole of the lower electrode, fill it tightly and level it, bake it at about 200℃ for 2h, and take a spectrum immediately. The electrode shape is shown in the figure below:
Upper electrode
Lower electrode
SJ/T10553--94www.bzxz.net
6.2 Use a three-lens illumination system to take a spectrum, use a three-step dimmer with two steps of transmittance of 100% and 50%, DC arc anode excitation, current intensity of 10A, slit width of 15um, electrode gap of 2+mm, shading plate of 3.2mm, spectrum range of 250~320nm, light for 30s, take a spectrum for each sample three times, develop the type 1 photosensitive plate in Metol-Hydelu developer for 3min at a temperature of 18~20℃, then fix, wash and dry. Calculation of analysis results
Measure the blackness of the analysis line pair on the microphotometer, draw the △S (P, O, using △P)-1gc working curve, and find out the impurity content in the sample from the working curve.
△S is the difference between the blackness of the analysis line and the blackness of the internal standard line, and Igc is the logarithm of the content of the analysis element in the standard sample. The analysis line and the determination content range are shown in Table 2.
Analysis line pair
Determination composition
8Precision or tolerance
Analysis elements
Fe259.957
Si2251.921
Ca317.933
Mg277.983
TiO308.803
Comparison elements
Co258.084
Co251.982
Zr320.068
Zr278.686
Zr308.534||tt| |Co255.303
Determination range
0.01~0.32
0.04~1.28
0.05~0.80
0.01~0.45
0.025~0.80
0.05~0.80
8.1 Precision
Use zirconium dioxide containing SiO2 0.13%, FeO 0.017%, MgO 0.02%, TiO2, CaO and PO 0.04% respectively, and take 30 spectra according to this method. The relative standard deviation is within the data listed in Table 3. Table 3
Determination of components
Relative standard deviation
8-2Accuracy
When the particle size and organizational structure of the standard sample are similar to those of the test sample, the accuracy is close to the precision. Additional remarks:
This standard is under the jurisdiction of the Standardization Research Institute of the Ministry of Electronics Industry, and this standard was drafted by the Standardization Research Institute of the Ministry of Electronics Industry. The main drafters of this standard are: Wang Yugong, Liu Chenggou, Luo Shaotang, Wang Xiuwen, and Li Guoxi. Tio,
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