GB/T 8762.6-1988 Determination of lead oxide, nickel oxide, iron oxide and copper oxide in fluorescent grade europium oxide - Emission spectrometry

GB/T 8762.6-1988 Determination of lead oxide, nickel oxide, iron oxide and copper oxide in fluorescent europium oxide - Emission spectrometry GB/T8762.6-1988 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Europium oxide of phosphorus grade- Determination of lead oxide,nickel oxide,iron oxide and copper oxide contents-Emission spectrographic methodUDC 661-866. 1
GB 8762. 6
This standard is applicable to the simultaneous determination of lead oxide,nickel oxide,iron oxide and copper oxide in fluorescent europium oxide. The determination range is shown in Table 1Table 1
Method SummarybZxz.net
Determination range
0. 000 10 ~ 0. 003 0
0. 000 10 ~~ 0. 003 0
0.000 10~0.003 0
0. 000 10~ 0. 003 0
Add a small amount of lithium carbonate and graphite powder to the sample of tin oxide as carriers, use DC arc excitation, and perform spectral determination. 2 Reagents
Europium oxide, greater than 99.99%.
Lead oxide, spectrally pure.
2.3 Nickel oxide, spectrally pure.
Iron oxide, spectrally pure.
Copper oxide, spectrally pure.
Lithium carbonate, spectrally pure.
Charcoal powder, spectrally pure.
Mixed carrier: Mix carbon powder and lithium carbonate in a ratio of 3:5, grind evenly in an agate mortar, and set aside. 2.8
3 Instruments, equipment and materials
3.1 Grating spectrometer: reciprocal linear dispersion 0.37~0.45nm/mm3.2 Light source: DC arc, rectifier output 280~300V, current intensity 20A, equipped with low and high current conversion device. 3.3 Spectrometer.
3.4 ​​Microphotometer.
Approved by China Nonferrous Metals Industry Corporation on February 4, 198822
Implementation on February 1, 1989
3.5 Graphite electrode cutting lathe.
3.6 Graphite electrode, spectrally pure, 6mm.
GB 8762.6—88
3.7 Stamping die: Turned from plexiglass, dimensions see Figure 1. 3.8 Photosensitive plate, UV type II I.
3.9 Equipment for developing, fixing and darkroom processing. 3.10 Computing board or calculator.
3.11 Agate mortar.
Figure 1 Stamping mold
4 Analysis steps
4.1 Determination quantity
Take three parallel spectra and take the average value.
4.2 Sample quantity
Weigh 92 mg of sample.
4.3 Determination
4.3.1 Sample preparation
Grind the sample (4.2) and 8 mg of mixed carrier (2.8) in an agate mortar and set aside. 4.3.2 Preparation of standard series
First, prepare a main standard sample containing 1% of lead oxide, nickel oxide, iron oxide and copper oxide, weigh each impurity oxide (2.2-2.5) and the oxidized lead matrix (2.1) according to the pre-calculated amount, mix and grind, and then dilute with the oxidized lead matrix (2.1) to form a standard series: 1%, 0.3%, 0.1%, 0.03%, 0.01%, 0.003%, 0.001%, 0.0003% and 0.0001%. Then weigh and mix the above standard series with the mixed carrier (2.8) according to the standard sample: carrier = 92:8, grind and mix, and wait for analysis. 4.3.3 Spectral measurement
Spectrometer: band range 250.0~~340.0nm, three-lens illumination system, slit width 10um, middle light bar height 5mm, two-step transmittance 100%, 10% or 15%.
Light source: DC arc anode excitation, working voltage 280V, current 5A and 14A, equipped with low and high current conversion device. Exposure mode: current 5A, light 5s, switch to current 14A exposure 35S, no pre-burning. Counter electrode: The sample electrode is used as the anode, its shape is Φ4×6×0.8.mm cup (as shown in Figure 2(1)), before loading the sample, use the arc 20A to burn for 5s, weigh 40mg of the sample (4.3.1) and the standard sample (4.3.2) respectively, put them into the electrode hole, and press them with a pressing mold (3.7). The cathode is turned into a flat cone with a stone electrode, and the top diameter is 1mm (see Figure 2(2)). 23
GB 8762.6—88
Figure 2 Graphite electrode
(1) - Anode: (2) - Cathode
Photosensitive plate processing: Prepare the developer and fixer according to the instructions of the photosensitive plate used. Develop and fix at 20±1°C, rinse in running water and dry.
Blackness measurement: Use a microphotometer (3.4) to measure the blackness S value of the analysis line pair (see Table 2), where the lead, nickel and iron analysis lines measure the blackness value of 100% transmittance, and the copper analysis line measures the blackness value of 10% transmittance. And measure the background blackness value at the specified direction of each analysis line (see Table 2).
5 Calculation of analysis results
Analysis line
Measurement base background direction
Use the plotted emulsion characteristic curve, use a calculation board or calculator (3.10) to convert the black value of the analysis line into the logarithmic value of the intensity, and use the background as the internal standard to draw the 1gRIgC working curve. When the matrix is ​​impure, use the incremental method to correct the working curve. The analysis result is the 1gR value corresponding to the sample, and the percentage content is directly found on the working curve. 6 Allowable difference
The allowable relative deviation of the analysis results between laboratories should not be greater than that listed in Table 3. 24 | | tt | 003 0
0. 000 10~0. 000 50
≥>0. 000 50 ~ 0. 001 5
>0. 001 5~0. 003 0
0. 000 10 ~ 0. 000 50
0. 000 50 ~~0. 001 5
>0. 001 5 ~~ 0. 003 0
0. 000 10 ~ 0. 000 50
>0. 000 50 ~ 0. 001 5
>0. 001 5 ~ 0. 003 0
This standard was drafted by Beijing General Research Institute of Nonferrous Metals and Shanghai Yuelong Chemical Plant. This standard was drafted by Beijing General Research Institute of Nonferrous Metals. The main drafter of this standard is Li Li.
Permissible relative deviation
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