GB/T 8762.4-1988 Determination of iron oxide, lead oxide, nickel oxide and copper oxide in fluorescent grade yttrium oxide - Emission spectrometry

GB/T 8762.4-1988 Determination of iron oxide, lead oxide, nickel oxide and copper oxide in fluorescent grade yttrium oxide - Emission spectrometry GB/T8762.4-1988 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Determination of iron oxide, lead oxide, nickel oxide and copper oxide contents in fluorescent grade yttrium oxide
Emission spectrographic method
Yttrium oxide of phosphorus grade-- Determinationof iron oxide,lead oxide,nickel oxide and copper oxide contents-
Emission spectrographic methodUDC 661.866
GB 8762. 4
This standard is applicable to the simultaneous determination of iron oxide, lead oxide, nickel oxide and copper oxide in fluorescent grade yttrium oxide. The determination range is shown in Table 1. Table 1
1 Method Summary
Measurement 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
Oxidation Add a small amount of silver chloride, gallium oxide and stone powder to the sample as a carrier, use DC arc fractionation evaporation and excitation, and perform spectrum measurement.
2 Reagents
Oxidation, greater than 99.99%.
Iron oxide, spectrally pure.
Lead oxide, spectrally pure.
Nickel oxide, spectrally pure.
Copper oxide, spectrally pure.
Silver chloride, spectrally pure.
Gallium oxide, spectrally pure.
Graphite powder, spectrally pure.
2.9Mixed carrier: weigh and mix C:AgCl:Ga0, 2:2:1, and grind in an agate mortar. Spare instruments, equipment, materials
Grating spectrometer: reciprocal line dispersion 0.37~0.45nm/mm. 3.1
Light source: DC arc, rectifier output 220~380V, 20A, with high-frequency ignition device. 3.2
3.3Spectrometer.
China Nonferrous Metals Industry Corporation approved on February 4, 1988, implemented on February 1, 1989
3.4Microphotometer.
3.5Graphite electrode cutting lathe.
3.6 Graphite electrode, spectrally pure, $6mm.
GB8762.4-88
3.7 Stamping die: Turned from plexiglass, dimensions see Figure 1.924
Figure 1 Stamping die
Material: plexiglass
Unit: mm
Ratio: 2:1
3.8 Photosensitive plate, UV II type.
3.9 Developing, fixing, darkroom processing equipment. 3.10 Calculation board or calculator.
3.11 Agate mortar.
4 Analysis steps
4.1 Determination quantity
Take three parallel spectra and take the average value.
4.2 Sample quantity
Weigh 90mg of sample.
4.3 Determination
4.3.1 Sample preparation
Grind the sample (4.2) and 10 mg of mixed carrier (2.9) in an agate mortar and set aside. 4.3.2 Preparation of standard series
First, add the impurity oxides (2.2-2.5) to the pure graphite powder (2.8) to prepare the graphite powder standard series; then mix yttrium oxide (2.1) and the powder standard series in a ratio of 90:4 to prepare the standard series containing impurity oxides calculated based on the total amount of oxides. The calculation is shown in Cloth 2 and Table 3.
4.3.2.1 Preparation of graphite powder standard series
According to Table 2, weigh 80 mg of pure graphite powder (2.8) and add 1.8 mg of each impurity oxide (2.2-~2.5), and mix well in an agate mortar to prepare the No. 1 graphite standard series. The following graphite standard series are prepared by gradual dilution according to Table 2. 11
4.3.2.2 Preparation of standard series
GB8762.4—88
Amount of graphite powder
Impurity addition
7.20 (1.80 for each of the four impurity oxides) 42. 04(No1)
46.03(No2)
38. 99(No3)
45.18(No4)
38.63(No5)
45. 00(No6)
Impurity oxide content
Weigh Cnuxi in the ratio of 904:2:4 (where Cnoxi is No7~No4 in Table 2), and grind it evenly in a mortar according to the Y,O, + AgCl + Ga,O,
. Prepare a set of standard series containing 0.0001%, 0.0003%, 0.001% and 0.003% of iron oxide, lead oxide, nickel oxide and copper oxide in yttrium oxide.
Content of each impurity
4.3.3 Spectral determination
0. 000 27
0. 000 09
Weighing, single
0. 000 09
corresponding to the impurity content in stone powder under the condition of Y,0 :C=bzxZ.net
Spectrograph: band range 240.0～340.0nm, three-lens illumination system, slit width 10μm, middle light bar height 3.2mm, two steps 100%, 10% or 15%.
Light source: DC arc anode excitation, working voltage 280V, arc current 15A, exposure 20s, no pre-burning. Counter electrode: The size of the sample electrode is shown in Figure 2. Before loading, treat the sample electrode with an arc of 20A for 5s. Weigh 20mg of the sample (4.3.1, 4.3.2), put it into the electrode hole, and press it with a pressing mold (3.7) to serve as the anode. The cathode is turned into a flat cone with a top diameter of $1 mm using a graphite electrode.
Photosensitive plate processing: The developer and fixer are prepared according to the instructions of the photosensitive plate used. Develop and fix at 20±1℃, rinse in running water, and dry.
Blackness measurement: Use a microphotometer (3.4) to measure the blackness S of the analysis line. Listed in Table 4. Among them, the transmittance of Cu327.40nm is a step value of 10%.
5 Calculation of analysis results
GB8762.488
Figure 2 Sample loading electrode
Material: graphite
Unit: mm
Scale: 2; 1
Analysis line
Use the plotted emulsion characteristic curve, use a calculation board or calculator (3.10) to convert the blackness value of the analysis line into the logarithmic value of the intensity, and draw the working curve with 1gl~1gC. When the matrix is ​​impure, use the incremental method to correct the working curve. The analysis result is the 1gl value corresponding to the sample, and the content is directly found on the working curve.
6 Allowable difference
The relative deviation of the analysis results between laboratories should not be greater than that specified in Table 5. Table 5
Content range
0. 000 1 ~ 0. 000 5
>0. 000 5~ 0. 001 5
>0. 001 5 ~ 0. 003 0
0. 000 1 ~~ 0. 000 5
>0. 000 5~~ 0. 001 5
>0. 001 5~ 0. 003 0
Relative deviation
Iron compound
Additional remarks:
GB8762.4--88
Continued Table 5
Content range
0. 000 1~0. 000 5
>0. 000 5 ~ 0. 001 5
>0. 001 5~~0. 003 0
0. 000 1 ~ 0. 000 5
>0.0005~0.0015
>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 was Qian Boren.
Relative deviation
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