This standard specifies the determination method of iron, nickel, titanium, zirconium, aluminum and manganese in niobium. This standard is applicable to the simultaneous determination of iron, nickel, chromium, titanium, zirconium, aluminum and manganese in niobium and its compounds. GB/T 15076.10-1994 Chemical analysis method of tantalum and niobium Determination of iron, nickel, chromium, titanium, zirconium, aluminum and manganese in niobium GB/T15076.10-1994 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis methods of molybdenum and niobium
Determination of iron, nickel, chromium, titanium, zirconium, aluminum and manganese contents in saws
Methods for chemical analysis oftantalum and niobium---Determinationof iron .nickel.chromium,titanium,zirconiumaluminum and manganese contents in niobiumSubject content and scope of application
This standard specifies the method for determination of iron, nickel, chromium, titanium, zirconium, aluminum and manganese contents in saws. GB/T 15076.1094
This standard is applicable to the simultaneous determination of iron, nickel, chromium, titanium, zirconium, aluminum and manganese contents in niobium and its compounds. The determination range is shown in Table 1. Table 1
Determined elements
Zirconium, manganese
Iron, nickel, chromium
2 Reference standards
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis method standards GB1467 General principles and general provisions for chemical analysis method standards for metallurgical products 3 Principle of method
Determination range, %
0.0001~~0.010
0. 0001~-0. 020
0. 0002 ~~0. 010
0.0003~0.030
Convert metal saw pentoxide or its compounds into saw pentoxide, and use DC arc carrier fractionation method for spectral determination. 4 Reagents and Materials
4.1 Niobium pentoxide, greater than 99.99%, of which the iron content should be less than 0.0002%, and the content of other measured elements should be less than 0. 000 05%.
4.2 Ferrous oxide, greater than 99.99%,
4.3 Nickel oxide, greater than 99.99%.
4.4 Chromium oxide, greater than 99.99%.
4.5 Titanium dioxide, greater than 99.99%
Approved by the State Administration of Technical Supervision on May 9, 1994 and implemented on December 1, 1994
4.6 Zirconium dioxide, greater than 99.99%.
4.7 Aluminum oxide, greater than 99.99%.
4.8 Manganese dioxide, greater than 99.99%.
4.9 Sodium fluoride, greater than 99.99%.
4.10 Graphite powder, spectrally pure.
4.11 Metal palladium, greater than 99.95%.
GB/T 15076.10-94
4.12 Palladium internal standard solution: weigh 0.250g metal palladium, place in a 150mL beaker, add 40mL aqua regia to dissolve, transfer to a 250ml volumetric flask, dilute to scale with water, mix well, this solution contains 1mg palladium per ml. 4.13 Carrier: weigh 9.40g graphite powder (4.9), add 1.5mL palladium internal standard solution (4.11), dry, add 0.60g sodium fluoride (4.9), grind well.
4.14 Graphite electrode: spectrally pure, 6mm.
4.15 Photosensitive plate: UV type I.
5 Instruments and equipment
5.1 Plane grating spectrograph: reciprocal linear dispersion is not greater than 0.35nm/mm. 5.2 Light source: DC arc.
5.3 Microphotometer.
5.4 Stamping die: made of organic glass rod, top ×h, mm: 2.9×2. 5.5 Electrode: lower electrode, ordinary type, ×h, mm: 3×10; upper electrode, flat-top cone, cone top cross section $2mm. 6 Analysis steps
6.1 Sample preparation
Take about 1g of laboratory sample in a high-temperature furnace, gradually heat it to 800℃ and burn it to make it completely oxidized, cool it to room temperature, and grind it evenly. For laboratory samples of metal rods, plates and wires, they should be hydrogenated first, ground, and then converted into saw pentoxide. Laboratory samples of saw hydroxide should be burned in a platinum crucible.
6.2 Preparation of spectral samples
6.2.1 Mix 2 parts of sample (6.1) with 1 part of carrier (4.13) and grind them evenly. 6.2.2 Place the sample (6.2.1) in the lower electrode (5.5) and press it with a die (5.4) so ​​that the sample is 1 mm below the electrode gate for spectrum recording. 6.3 Determination
6.3.1 Preparation of standard samples
Put pentoxide (4.1) in a high-temperature furnace and burn it at 850℃ for 2h. Put it in a dryer and cool it to room temperature. Add the dried single oxide (4.2~4.8) according to the calculated amount to prepare the main standard sample with a content of 1% of each element to be measured. Then gradually dilute it with pentoxide to form a standard series. The content is shown in Table 2. Add it to the carrier according to 6.2.1 and load it into the electrode according to 6.2.2. Table 2
Measured elements
Iron, nickel, chromium, titanium, zirconium, aluminum, manganese
Impurity content of main standard samples, %
The content of measured elements in the matrix should be corrected by the incremental method if necessary. 6.3.2 Determination conditions
Impurity content of standard sample series, %
Spectrograph: central wavelength 300.0nm, three-lens illumination system, slit width 12μm, middle light bar height 3.2mm. Light source: DC arc anode excitation, current 14A, pole distance 3mm. Exposure time: 60s.
10. 000 1
GB/T 15076.10-94
Darkroom treatment: developer A+B formula, diluted with equal amount of water, developed at 20±1℃ for 3~~4min, fixed, washed with water, dried. Blackness measurement: S scale.
Analysis line pairs are shown in Table 3.
Analysis line
Fe302.107
Fe 259.837
Ni300.249
Cr 302.156
Ti307.865
Zr339.198
Al308.216
A1 257.510
Mn 280.106
Mn 265.568
6.3.3 Spectroscopy
Internal standard linebZxz.net
Pd 325.878
Pd325.878
Pd 325. 878
Pd325.878
Pd 325.878
Pd325.878
Background measurement position
Long wave direction
Long wave direction
Long wave direction
Short wave direction
Short wave direction
Long wave direction
Short wave direction
Long wave direction
Short wave direction
Long wave direction
Short wave direction
Photograph the spectrum sample (6.3) and the standard sample (6.4.1) on the same photographic plate, measure the spectral line blackness after processing in a darkroom, and convert it into intensity ratio.
7 Calculation and expression of analysis results
7.1 Draw the working curve with IgR～lgc and IgIlgc, and calculate the percentage of the measured element. 7.2 Calculate the percentage of the measured element in saw according to the following formula: X(%)-1. 43c
Wherein: c—the percentage of the measured element found from the working curve; 1.43-
—the coefficient of converting saw pentoxide into saw.
The obtained result is expressed to 3 decimal places; if the content is less than 0.01%, it is expressed to 4 decimal places; if it is less than 0.001%, it is expressed to 5 decimal places. 8 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 4. Table 4
Content of measured elements
0. 000 10~0. 000 30
>0,000 30～0.000 80
≥0. 000 80 ~ 0. 001 5
0. 001 5~0. 003 0
>0. 003 0~0. 007 0
>0. 007 0~0. 010
>0. 010~-0. 020
>0.020~~0.030
0. 000 15
Additional remarks:
GB/T 15076.10--94
This standard is proposed by China National Nonferrous Metals Industry Corporation. This standard is drafted by Ningxia Nonferrous Metals Smelter. This standard is drafted by Ningxia Nonferrous Metals Smelter. The main drafter of this standard is Tian Kongquan.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry of the People's Republic of China issued the Ministry of Standard YB942 (14)-78 "Emission Spectrum Determination Method for Impurities in Copper" will be invalid.
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