Method for spectral analysis of Nickel and Nickel aloy for vacuum tubes

SJ 1543-1988 Spectral analysis method for nickel and nickel alloys for vacuum devices SJ1543-1988 standard download decompression password: www.bzxz.net

Standard of the Ministry of Electronics Industry of the People's Republic of China SJ1543-88
Spectral analysis method of nickel and nickel alloys for vacuum devices
Published on March 17, 1988
Implemented on December 1, 1988
Published by the Ministry of Electronics Industry of the People's Republic of China Standard of the Ministry of Electronics Industry of the People's Republic of China Spectral analysis method of nickel and nickel alloys for vacuum devices 51 1543-88
Replaces SJ 1543-79
This standard is applicable to the determination of the following elements in wire and alloy (N, NSi, NM·pre-i) for vacuum devices:
1 Method
Content range (%)
0.02~0.3d
0. 02~0. 20
. 02~0,do1
我人,
0.02-0.20
0. 02~0,20
0.01~0,10
心,期oto,
0. 001 0. 01
0.001~0.01
0. 0010. 01
The "powder spherical arc method" with high sensitivity, stable emission and no limitation on sample shape is used for analysis. According to the different excitability of the elements to be tested, the easily excited elements arsenic, arsenic, antimony, arsenic, zinc, and arsenic are determined under DC cathode excitation; the difficultly excited elements silicon, magnesium, iron, manganese, cobalt, and aluminum are determined under DC cathode excitation. Instruments and equipment
a. Large or medium-sized camera
b. Direct arc generator (voltage not less than 22, secondary voltage regulator)c. Non-recording microphotometer with secondary voltage regulatord. Spectrometer;
, analytical balance or torsion balance (sensitivity is 0.1g)f. Rack balance,
9. Muffle furnace (maximum temperature rise is not less than 1000℃)h. Small lathe or other lathe for turning electrodes Device, 1, agate grinding body,
Ministry of Electronics Industry of the People's Republic of China approved on 1988-0%-17 and implemented on 1988-12-01
small, infrared lamp;
k, stopwatch;
1, press;
m, gold-containing die (than schematic diagram 1),
3 Materials and reagents
a, nitric acid (analytical grade):
b, nitrate (1+5):
c, slightly (3+2);
d, deionized water:
e, spectrally pure graphite electrode (Figure 2):
$11543-88
E, photosensitive plate (Tianjin UV type 1, type (or straight type): 9, developer and fixer (according to 4. Analysis steps
4.1 Sample treatment
Weigh 3g of sample, place in an evaporator, add nitric acid (1+5) to wash, rinse twice with deionized water, then add 25-30ml nitric acid (3+2), heat and dissolve (keep slightly boiling), evaporate to low, move the evaporator into a muffle furnace, burn at B0-800℃ for 20min, take out and cool, grind the generated oxide in a mortar, weigh three portions of the oxide powder of the sample and standard, each weighing 300mg, use a press to press into a die (the inner diameter of the die is 5m as shown in Schematic 1) to press into a block, and bake under an infrared lamp for 20min45
Electricity fee
Schematic diagram 1
4.2 Anode excitation spectrum
Put the block on the lower electrode and take spectrum according to the conditions shown in Table 1 2.
Lower electrode
Analysis elements
Direct current anode excitation
SJ1543-88
Three-fin illumination system, central wavelength 201mm, width 0.012mm
Shade board 5mm
North fence height 1mm
Interpolar distance 3mm
Current 5~7A
Photosensitive plate: UV type I, type I
4.3 Cathode excitation spectrum
When the blue anode spot is on the block, immediately expose it for 15~2OS, and keep the interpolar distance unchanged during the spectrum. The standard sample and the test sample are parallelly spectrumed three times.
Put the sample molten bead generated after anode excitation on the lower electrode, and take a spectrum according to the conditions shown in Table 2
Analysis elements
DC motor cathode excitation
Three-way mirror illumination system
Center wavelength 2
Gain width 0.010m
Light selection plate height 3.2mm
Two-step or three-step photoreceptor
Interpolar distance 3
Current 58A
Photosensitive plate, tight outer shape
4.4 Processing of photosensitive plate
When negative spots appear on the molten bead, immediately illuminate for 15~20S, and control the distance to a small change during the spectrum recording process. The standard sample and the test sample are parallelly spectrographically three times.
The photosensitive plate after spectrum recording is developed in a developer at a temperature of 19±1℃ for 1min and fixed to a transparent water mark. Cool and level. 4.5 Blackness measurement
Measure the point degree S or the converted cumulative value P of the analysis line pair of each element on the microphotometer. The wavelengths of the analysis line pairs are listed in the table below: 3
Analysis element
S164 3±
23t,98
283,30
251,92
259,86
307,23
Treatment, or learning
308,23
Vernier length (
283,22
311,6 days
329,61
252,80
287,62
287,82
Main country t
4. 6 Result calculation
According to the measurement results, calculate the average value of the difference between the standard sample and the sample, △S or AP, and use the △S or P of the standard sample and the logarithm of the content of the corresponding element iogc to draw a working curve. According to the AS or △P of the sample, find the logarithm of the content of the element to be measured from the working curve, and then calculate the content of the element to be measured. 5 Purity
Accuracy is expressed by the relative standard deviation Sr value of a single measurement, which is engraved in Table 4. Table 4
contains the maximum range
determined elements
0 .001--0.003wwW.bzxz.Net
Sr value is calculated as follows:
0.c030.010
Content range
Determining elements
(xi-x)2
Xi—i-time measurement value (i1, 2, 3, n):——.-Number of measurements:
—Arithmetic mean of n-time measurements
S—Standard deviation:
—Relative standard deviation,
0.02~0,10
0.10~0,30
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.