This standard applies to the determination of silicon, aluminum, iron, calcium, cobalt, nickel, manganese, magnesium, lead, vanadium, tin, titanium, antimony, cadmium and other elements in molybdenum materials (powder, blank, rod, wire, strip, belt) for
electronic devices and electric light sources, molybdenum trioxide (without additives), ammonium molybdate and molybdic acid. SJ 2657-1986 Spectral analysis method for molybdenum SJ2657-1986 standard download decompression password: www.bzxz.net This standard applies to the determination of silicon, aluminum, iron, calcium, cobalt, nickel, manganese, magnesium, lead, vanadium, tin, titanium, antimony, cadmium and other elements in molybdenum materials (powder, blank, rod, wire, strip, belt) for electronic devices and electric light sources, molybdenum trioxide (without additives), ammonium molybdate and molybdic acid.

Ministry of Electronics Industry of the People's Republic of China Standard SJ2657-86
Mothod of molybdenum spectral analysis
Mothod of molybdenum spectral analysis1986-01-21Promulgated
Implementation on 1986-10-01
Ministry of Electronics Industry of the People's Republic of China
Ministry of Electronics Industry of the People's Republic of China Standard of Molybdenum Spectral Analysis
Mothod of molybdenum spectral analysisSJ2657-86
This standard applies to the determination of molybdenum materials (powder, bad, rod, wire, strip, ribbon) for electronic devices and electric light sources, molybdenum trioxide (without additives), ammonium molybdate and molybdic acid, such as silicon, aluminum, iron, calcium, cobalt, nickel, manganese, magnesium, bismuth, lead, vanadium, tin, titanium, antimony and cadmium.
1 Summary of the method
Convert the sample into molybdenum trioxide, grind it thoroughly with the mixed carbon powder, place it in a cup-shaped graphite electrode and use DC arc anode excitation to make molybdenum anhydride form a non-volatile compound to suppress the spectral line of molybdenum. Potassium iodide in the mixed carbon powder helps to reduce the detection limit of the element to be measured and improve the density precision of the method. The internal standard elements are and lock. 2
Instruments, equipment, materials and reagents
Medium or large spectrometer;
DC arc generator (voltage not less than 220V, current 220A): Microphotometer:
Spectrometer:
Analytical balance (minimum division value 0.1mg: maximum weighing 200g); Torsion balance (minimum division value 0.1mg: maximum weighing 500mg): Rack balance (minimum Graduation value 0.1g: maximum weighing 1.000g): Muffle furnace (with thermocouple: maximum temperature rise can reach 1100℃) Small lathe or other device for turning electrodes: Dust-proof device for grinding samples;
Hard alloy mortar and pounding chain;
Agate mortar and pestle:
Organic glass mortar and pestle
Stopwatch (accuracy 0.1s);
Press needle (stainless steel): ||tt| |Organic glass funnel:
Infrared lamp:
Photosensitive plate (UV I type, straight type);
Graphite electrode (spectrally pure, diameter 6mm):Carbon powder (spectrally pure):
Potassium iodide (spectrally pure):
Barium oxide (spectrally pure);
Gallium trioxide (spectrally pure);
Standard sample of synthetic pinium (set);
Approved by the Ministry of Electronics Industry of the People's Republic of China on January 1, 1986 and implemented on October 1, 1986
Deionized water;
Developer (prepared according to the instructions for the photosensitive plate):Fixing solution (prepared according to the instructions for the photosensitive plate): 3 Sample treatment
SJ2657-86
: Molybdenum wire and molybdenum rod: Boil with 20% sodium hydroxide solution to remove the surface graphite emulsion until it is glossy, then wash with water and dry at 105-110℃. Fold the wire into segments, rods and blocks and crush them with a carbide mortar. Take 1g of the above sample and put it into a covered porcelain, place it in a muffle furnace and burn it at about 500℃ until it is completely converted into molybdenum trioxide. Ammonium molybdate and molybdenum powder can be directly converted. 4 Analysis steps
4.1 Sample loadingbZxz.net
After the standard sample and the sample are ground evenly with the mixed carbon powder in a ratio of 2:1 in an agate mortar or a plexiglass mortar, use a torsion balance to weigh three samples of each number, each with 100mg. Use a plexiglass funnel to load the sample into the electrode, use a pressure needle to press the sample tightly and use a scraper to remove the sample around the lower electrode mouth, and place it under an infrared lamp to bake for half an hour for use. The pressure needle, electrode and scraper are as shown in the figure below:
一中
4.2 Spectroscopy
On the electricity charge
The sample to be tested is spectrographically photographed under the following conditions:
Down the telegraph
Use a plane grating spectrograph, with a dispersion rate of 0.74nm/mm, a central wavelength of 310nm, a three-lens illumination system, a slit width of 12nm, a middle light bar of 5mm, and a pole distance of 2.5mm. The sample is placed on a DC arc anode, with a current of 3A, pre-burned for 10S, and then converted to 13A, and the cathode area is intercepted. The daylight of 25S is intercepted. The photosensitive plate is ultraviolet type I or type 1. Each standard sample is spectrographically photographed three times in parallel with the sample. 4.3 Photosensitive plate processing
The photosensitive plate for spectrum is developed in a developer at 18-20℃ for 4min, then fixed in a fixer, washed with water, and dried.
4.4 Photometry and result processing
Measure the blackness of the analytical line pair on a microphotometer. Draw a working curve with △P-1ogC, and find the percentage content of the element to be measured in the sample on the working curve.
△P-blackness difference of the analytical line pair
logC-logarithm of the content of the element to be measured in the standard sample. The wavelength of the analytical line pair, the range of measured content and the percentage mean square error are shown in the table below. 2.
Measured element
Analytical line wavelength (nm)
Precision calculation
Precision is calculated according to the formula
Standard deviation m=
Percent mean square error
Where:
SJ2657-86
Internal standard line wavelength (nm)
Ba233.527
Ga265.937
Ba307.159
Ga265.937
Ba307.159
ix)2
xi——Values ​​of each measurement:
-the average value of multiple measurements;
-the number of measurements;
-the content of the element to be measured.
Determination content range (%)
2.0×10-4-2.0×10-2
2.0×10-42.0×10-3
2.0×10-4-2.0×10-2
2,0×10~4-2.0×10-2
2.0×10~4-2,0×10-2||tt ||2.0×10-4-2.0×10-3
2.0×104-2,0×10-2
2.0×10*42.0×10-2
2.0×10-4—2.0×10-3
2.0×10-+2.0×10-2
2.0×10-4- 2.0×10-2||t t||2.0×10-4-2.0×10-2
6.7×10-5-6.7×10-8
6.7×10-5-6.7×10*8
6.7×10--6,7×10~8
6.0×10-5-6.7×10-s
Mean square error|| tt||(1)||tt ||The content range of molybdenum standard samples is shown in the following table
Contains the most g
1657-86
Appendix A
The content range of molybdenum standard samples
(reference)
0,00067
Additional instructions:
SJ2657-86
This standard was proposed by the Standardization Research Institute of the Ministry of Electronics Industry. This standard was drafted by the 741 Factory and 774 Factory of the Ministry of Electronics Industry. The main drafters of this standard are Li Zhong and Wang Jinxue.
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