This standard specifies the determination method of arsenic, antimony, lead, tin and bismuth in niobium. This standard is applicable to the simultaneous determination of arsenic, antimony, lead, tin and bismuth in niobium and its compounds. GB/T 15076.11-1994 Chemical analysis method of tantalum and niobium Determination of arsenic, antimony, lead, tin and bismuth in niobium GB/T15076.11-1994 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis methods of tantalum and niobium
Methods for chemical analysis of tantalum and niobium-Determination of arsenic antimony, lead, tin and bismuth contents in niobium 1 Subject content and scope of application
This standard specifies the method for the determination of arsenic, antimony, lead, tin and bismuth contents in niobium GB/T 15076.11-94
This standard is applicable to the simultaneous determination of arsenic, antimony, lead, tin and bismuth contents in niobium and its compounds. The determination range is shown in Table 1. Table 1
Measured elements
2 Reference standards
GB1.4 Standardization work guidelines Chemical analysis method standard preparation regulations GB1467 General principles and general provisions for chemical analysis methods of metallurgical products 3 Principles of methods
Measurement range, %
0.0010~0.030
0. 000 4 ~~0. 010
0. 000 3~0. 010
0. 000 1 -~ 0. 010
0, 000 1~0. 030
Convert metal saw or its compound into saw oxide, adopt carrier fractionation method, DC arc anode excitation, spectrum photography, and perform spectrum measurement. Reagents and materials
Wax oxide, greater than 99.99%. Arsenic, lead, tin and content are all less than 1×10-1%. Antimony is less than 3×10-4%. Arsenic trioxide, greater than 99.9%.
Antimony trioxide, greater than 99.9%.
Lead dioxide, greater than 99.9%.
Tin dioxide, greater than 99.9%.
Bismuth trioxide, greater than 99.9%.
Gallium trioxide, greater than 99.9%.
4.8Sulfur powder, spectrally pure
Approved by the State Administration of Technical Supervision on May 9, 1994 and implemented on December 1, 1994
4.9Carbon powder, spectrally pure.
GB/T15076.11-94
4.10Carrier: Mix 93 parts of carbon powder, 5 parts of gallium trioxide and 2 parts of sulfur powder and grind them evenly. 4.11 Stone electrode, spectrally pure, g6mm.
4.12 Photosensitive plate: UV type.
5 Instruments and devices
5.1 Plane grating spectrograph: reciprocal line dispersion not more than 0.4nm/mm5.2 Light source: DC arc.
5.3 Microphotometer.
5.4 Stamping die: made of organic glass rod: $×h, mm: 3.9×12, with a pointed cone at the top. 5.5 Electrode: The lower electrode is cup-shaped: inner diameter 4ml, hole depth 10mm, wall thickness 0.8mm, neck diameter 3mm, height 4mm. The upper electrode is a flat-top cone with a cross section of $2mm.
6 Analysis steps
6.1 Preparation of samples
Take 1g of laboratory sample, place it in a high temperature furnace, and burn it at 700℃ for 1h (saw wire and saw blade need to be burned for more than 4h). It is completely converted into dioxide pentoxide.
6.2 Preparation of spectral samples
Take six samples (6.1) and one carrier (4.10) and mix and grind them evenly. Weigh 100mg and put it into the lower electrode (5.5), press it with a die (5.4) for spectrum recording.
6.3 Preparation of saw matrix
The preparation method of saw matrix (4.1) is carried out according to 6.2, and the average value of four spectrum is taken. It is used to measure the blackness of the weak molecular band at 234.9nm.
6.4 Determination
6.4.1 Preparation of standard samples
Dry the saw pentoxide (4.1) and each single oxide (4.2-4.6) in an oven and cool to room temperature. Add each single oxide (4.2-4.6) to the saw pentoxide (4.1) according to the calculated amount to prepare a main standard sample with an arsenic content of 3% and a lead, antimony, and tin content of 1%. Then gradually dilute with saw pentoxide (4.1) to form a standard series. The content of the standard sample is shown in Table 2. The ratio of each standard sample to the carrier and the sample loading are carried out according to the method in Section 6.2.
Antimony, lead, tin, bismuth
6.4.2 Determination conditions
Main standard sample
Content, %
Content of elements in standard series, %
Spectrometer: Band range 230.0~310.0nm, three-lens illumination system, slit width 15μm, middle light bar height 5.0mm. Light source and exposure time: DC arc anode excitation, 5A arc start, exposure 10s, immediately increase to 12A exposure 50s. 0.000 3
Darkroom treatment: Developer A+B formula, develop the short-wave band sensitive plate (assay arsenic) at 26±1C for 6min. The long-wave sensitive plate is developed at 20±1C for 4~5min. F-5 fixer. Fixing, rinsing, drying. Blackness measurement: S scale.
Analysis line pairs are shown in Table 3.
Analysis line
Ph 283.30
6.4.3 spectrum
GB/T 15076.11-94
Internal standard line
Ga 262. 48
Ga 262.48
Ga 262. 262. 48
Ga 262. 48
Background measurement position
234.98nm molecular band
Short wave direction
Long wave direction
Short wave direction
Short wave direction
Long wave direction
Photograph the saw substrate (6.3), the spectrum sample (6.2) and the standard sample (6.4.1) on the same photosensitive plate, and measure the blackness of the spectrum line after darkroom treatment.
7 Calculation and expression of analysis results
The working curve of arsenic is lg (IAs+ molecular band - I molecular band) ~ lgc, and the working curves of antimony, lead, tin and bismuth are all drawn with IgR ~ lgc. The percentage of the measured element in saw pentoxide can be obtained from the working curve. Calculate the percentage of the measured element in saw according to the following formula: X(%)-1.431c
Wherein: X--the measured element in saw;
the percentage of the measured element in saw pentoxide; 1.431-
-the conversion factor from saw pentoxide to saw. The result is expressed to three decimal places; if the content is less than 0.01%, it is expressed to four decimal places; if it is less than 0.001%, it is expressed to five 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 range
0. 000 10 ~ 0. 000 30
>0.00030~0.00080
>0. 000 80~0.001 0
>0. 001 0~0. 003 0
>0. 003 0~0. 007 0
≥>0. 007 0~0. 010
>0.010~0.020wwW.bzxz.Net
>0.020~0.030
Tolerance
0. 000 15
Additional instructions:
GB/T 15076.11—94
This standard was proposed by China Nonferrous Metals Industry Corporation. This standard was drafted by Ningxia Nonferrous Metals Refinery. This standard was drafted by Beijing Nonferrous Metals Research Institute. The main drafter of this standard is Kong Lingxian.
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 (15)-78 "Emission Spectrum Determination of Bismuth, Tin, Lead, Antimony and Arsenic in Niobium" will be invalid. 526
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