GB/T 15076.9-1994 Chemical analysis method of tantalum and niobium Determination of iron, chromium, nickel, manganese, titanium, aluminium, copper and zirconium in tantalum GB/T15076.9-1994 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of tantalum
Determination of iron, chromium, nickel, manganese, titanium, aluminum, copper and zirconium contents in tantalum
Methods for chemical analysis of tantalum and niobium-Determinationof iron, chromium, nickel, manganese, titanium, aluminum, copper and zirconium contents in tantalum Subject content and scope of application
This standard specifies the method for determination of iron, chromium, nickel, manganese, titanium, aluminum, copper and zirconium contents in tantalum. GB/T 15076.9—94
This standard is applicable to the determination of iron, chromium, nickel, manganese, titanium, lead, copper and zirconium contents in molybdenum and its oxides. The determination range is shown in Table 1. Table 1
Aluminum, zirconium
Chromium, nickel, titanium
Cited 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. 00005~~0.0010
0. 00010~0. 0030
0. 00010 ~~0. 010
0. 00020～0. 010
0.00050~0.020
The metals and their compounds are burned and converted into oxides, and a certain proportion of carbon powder and sodium chloride mixture is used as a carrier and excited by DC arc anode for spectral quantitative determination.
4 Reagents and Materials
4.1 Molybdenum pentoxide, 99.99%, two matrices are prepared by calcining molybdenum powder and molybdenum hydroxide at 1000℃, respectively, and stored separately. 4.2 Ferrous oxide, ≥99.99%.
4.3 Chromium oxide, ≥99.99%.
4.4 Nickel oxide, >99.99%.
Approved by the State Administration of Technical Supervision on May 9, 1994 and implemented on December 1, 1994
Manganese dioxide, >99.99%.
4.6 Titanium dioxide, ≥99.99%.
Aluminum oxide, ≥99.99%.
Copper oxide, 99.99%.
Zirconium dioxide, >99.99%.
Germanium dioxide, >99.99%.
GB/T 15076.9—94
Sodium chloride, >99.99%, calcined at 500℃ for 2h. Metal palladium, ≥99.95%.
4.13 Palladium internal standard solution: weigh 0.250g of metal palladium and place it in a small beaker, add 40mL of aqua regia, transfer the palladium into a 100mL volumetric flask after it is completely dissolved, dilute to scale with water, mix well, this solution contains 2.5mg palladium per mL. 4.14 Carbon powder (or graphite powder), spectrally pure. 4.15 Preparation of carrier.
Add 2.00mL of palladium internal standard solution (4.13) to 20.000g of carbon powder (4.14), dry in an oven, and grind evenly. Add germanium dioxide (4.10) to a certain amount of sodium fluoride (4.11) so that the sodium chloride contains 0.03% germanium dioxide, and grind evenly. 4.15.2
4.15.3 Take one part of sodium chloride (4.15.2) and seven parts of carbon powder (4.15.1) and grind them evenly. 4.16 Graphite electrode, spectrally pure, $6mm. 4.17 Photosensitive plate, ultraviolet type I.
Instruments and devices
5.1 Plane grating spectrograph: reciprocal linear dispersion not greater than 0.37nm/mm. 5.2 Light source: DC arc, voltage 220～380V. 5.3 Microphotometer.
5.4 Electrode: F electrode $×h, mm: 3×4, cup-shaped, see Figure 1; the upper electrode is a flat-top cone with a cone top cross section of g2mm. 40
6 Analysis steps
6.1 Sample preparation
Take about 1g of molybdenum powder or molybdenum hydroxide laboratory sample, place it in a porcelain crucible or platinum crucible, and heat it to 900°C in a box-type electric furnace and burn it for about 30 minutes. Molybdenum wire, sheet, and chip laboratory samples must be hydrogenated, ground, and then placed in porcelain to burn into molybdenum oxide. 62 Preparation of spectral samples
Take 3 parts of sample (6.1) and 1 part of carrier (4.15.3), grind them evenly, and put them into F electrode (5.4) for spectrum recording. 6.3 Determination
6.3.1 Preparation of standard samples
Add calculated amounts of monoxides (4.2-4.9) to two molybdenum pentoxides (4.1) respectively to prepare two master standards, which are gradually diluted with the corresponding matrix to form the required standard series. The contents are shown in Table 2. The 516
standard series is prepared according to the method (6.2).
GB/T 15076.9-94
Master standard sample
Impurity content, %
Aluminum, copper
Chromium, nickel, manganese, titanium, zirconium
The measured elements contained in the matrix are corrected by the incremental method when necessary. 6.3.2 Determination conditions
Impurity content of standard sample series, %
Spectrograph: Band range 260～345nm, three-lens illumination system, middle light bar height 3.2mm, slit width 10um. Light source: Power supply voltage 220V, current 18A, DC arc anode excitation, electrode distance 2mm. Exposure time: 35s.
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.
6.3.3 Spectroscopy
Analysis lines, nm
Spectrum the standard sample (6.3.1) and the spectrum sample (6.2) on the same photosensitive plate. Calculation and expression of analysis resultsbZxz.net
Draw a working curve with △S～lgc, and calculate the percentage of the measured element. Calculate the percentage of the measured element in molybdenum according to the following formula; X(%)=1.221c
Where: - the percentage of the measured element obtained from the working curve; - the conversion factor from molybdenum pentoxide to molybdenum. 1,221—
Internal standard line.nm
Pd 276.309
Pd325.164
Pd 325.164
Pd 325.164
Pd 325. 164
Pd325.164
Ge 275.46
Ge 303.91
Ta 338.20
The results are 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
GB/T15076.9—94
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. Table 4
Impurity content
0. 000 05 ~0. 000 10
>0. 000 10-~0. 000 30
>0. 000 30 ~0. 000 80
>C. 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
Additional remarks:
This standard was proposed by China Nonferrous Metals Industry Corporation. This standard was drafted by Ningxia Nonferrous Metals Smelter. This standard was drafted by Ningxia Nonferrous Metals Smelter. The main drafter of this standard is Hua Feng.
Allowance
0. 000 15
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 (13)-78 "Emission Spectrum Determination Method for Impurities in Molybdenum" will be invalid.
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