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GB/T 15076.11-2020: Methods for chemical analysis of tantalum and niobium - Part 11: Determination of arsenic, antimony, lead, tin and bismuth contents in niobium - Direct current arc atomic emission spectrometry
Status: Valid GB/T 15076.11: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB/T 15076.11-2020 | English | 189 |
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Methods for chemical analysis of tantalum and niobium - Part 11: Determination of arsenic, antimony, lead, tin and bismuth contents in niobium - Direct current arc atomic emission spectrometry
| Valid |
GB/T 15076.11-2020
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| GB/T 15076.11-1994 | English | 239 |
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Methods for chemical analysis of tantalum and niobium. Determination of arsenic antimony, lead, tinand bismuth contents in niobium
| Obsolete |
GB/T 15076.11-1994
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PDF similar to GB/T 15076.11-2020
Basic data | Standard ID | GB/T 15076.11-2020 (GB/T15076.11-2020) | | Description (Translated English) | Methods for chemical analysis of tantalum and niobium - Part 11: Determination of arsenic, antimony, lead, tin and bismuth contents in niobium - Direct current arc atomic emission spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 10,141 | | Date of Issue | 2020-03-06 | | Date of Implementation | 2021-02-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 15076.11-2020: Methods for chemical analysis of tantalum and niobium - Part 11: Determination of arsenic, antimony, lead, tin and bismuth contents in niobium - Direct current arc atomic emission spectrometry
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Methods for chemical analysis of tantalum and niobium - Part 11.Determination of arsenic, antimony, lead, tin and bismuth contents in niobium - Direct current arc atomic emission spectrometry
ICS 77.120.99
H14
National Standards of People's Republic of China
Replace GB/T 15076.11-1994
Tantalum-niobium chemical analysis method
Part 11.Determination of arsenic, antimony, lead, tin and bismuth in niobium
DC arc atomic emission spectrometry
2020-03-06 released
2021-02-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 15076 "Methods for Chemical Analysis of Tantalum and Niobium" is divided into 16 parts.
---Part 1.Determination of tantalum content in niobium by inductively coupled plasma atomic emission spectrometry;
---Part 2.Determination of the amount of niobium in tantalum inductively coupled plasma atomic emission spectrometry and chromatography gravimetric method;
---Part 3.Determination of copper content by flame atomic absorption spectrometry;
---Part 4.Determination of iron content 1,10-phenanthroline spectrophotometry;
---Part 5.Determination of the amount of molybdenum and tungsten by inductively coupled plasma atomic emission spectrometry;
---Part 6.Determination of silicon content by inductively coupled plasma atomic emission spectrometry;
---Part 7.Determination of phosphorus content in niobium 4-methyl-pentanone-[2] extraction separation phosphomolybdenum blue spectrophotometry and inductively coupled plasma
Bulk atomic emission spectroscopy;
---Part 8.Determination of carbon and sulfur content by high-frequency combustion infrared absorption method;
---Part 9.Determination of the amount of iron, chromium, nickel, manganese, titanium, aluminum, copper, tin, lead and zirconium in tantalum by DC arc atomic emission spectrometry;
---Part 10.Determination of the content of iron, nickel, chromium, titanium, zirconium, aluminum and manganese in niobium by DC arc atomic emission spectrometry;
---Part 11.Determination of arsenic, antimony, lead, tin and bismuth in niobium by DC arc atomic emission spectrometry;
---Part 12.Determination of Phosphorus in Tantalum by Ethyl Acetate Extraction and Separation of Phosphomolybdenum Blue Spectrophotometry;
---Part 13.Determination of nitrogen content inert gas fusion thermal conductivity method;
---Part 14.Determination of oxygen content inert gas melting infrared absorption method;
---Part 15.Determination of hydrogen content inert gas fusion thermal conductivity method;
---Part 16.Determination of sodium and potassium content by flame atomic absorption spectrometry.
This part is Part 11 of GB/T 15076.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part replaces GB/T 15076.11-1994 "Methods for chemical analysis of tantalum and niobium. Determination of arsenic, antimony, lead, tin and bismuth in niobium". Headquarters
Compared with GB/T 15076.11-1994, the main technical changes except for editorial changes are as follows.
---The measurement method has been changed from "DC arc carrier fractionation atomic emission spectrometry" to "DC arc atomic emission spectrometry";
---Expanded the measurement range, the measurement range of antimony was changed from "0.0004%~0.010%" to "0.0004%~0.030%"; the measurement of lead
The setting range is changed from "0.0003%~0.010%" to "0.0003%~0.030%"; the measuring range of tin is changed from "0.0001%~
0.010%" is revised to "0.0001%~0.030%" (see Chapter 1, Chapter 1 of the.1994 edition);
---The reference standard is deleted (see Chapter 2 of the.1994 edition);
---Add sample clause (see Chapter 5);
--- Added precision clause (see Chapter 8);
---Added the test report clause (see Chapter 9).
This part was proposed by China Nonferrous Metals Industry Association.
This part is under the jurisdiction of the National Nonferrous Metals Standardization Technical Committee (SAC/TC243).
Drafting organizations of this section. Ningxia Oriental Tantalum Co., Ltd., Northwest Rare Metal Materials Research Institute Ningxia Co., Ltd., Xi'an Han and Tang Dynasties
Analysis and Testing Co., Ltd., Jiujiang Nonferrous Metal Smelting Co., Ltd., Northwest Nonferrous Metal Research Institute, National Standard (Beijing) Inspection and Certification Co., Ltd.
The main drafters of this section. Zhang Junfeng, Xu Ninghui, Wang Zhiping, Wang Daping, Wang Yubao, Wei Hongnan, Mo Shumin, Xie Yuqin, Sun Hongtao,
Zhang Lina.
The previous versions of the standards replaced by this part are as follows.
---GB/T 15076.11-1994.
Tantalum-niobium chemical analysis method
Part 11.Determination of arsenic, antimony, lead, tin and bismuth in niobium
DC arc atomic emission spectrometry
1 Scope
This part of GB/T 15076 specifies the determination of arsenic, antimony, lead, tin and bismuth in niobium by DC arc atomic emission spectrometry.
This section applies to the determination of arsenic, antimony, lead, tin and bismuth in niobium and niobium hydroxide, niobium oxide and niobium carbide. The measurement range is shown in Table 1.
2 Principle
The metal niobium and its hydroxides and carbides are burnt to convert into niobium pentoxide, and a certain proportion of graphite powder and sodium fluoride are mixed as a buffer.
Granules, DC arc anode excitation, spectrometry.
3 Reagents or materials
3.1 Niobium pentoxide. wNb2O5≥99.99% (wAs≤0.0001%, the content of other single measured elements wx≤0.00001%), in muffle
Burn in the furnace at 850°C for 2h~3h, put it in a desiccator and cool to room temperature for later use.
3.2 Arsenic trioxide (wAs2O3≥99.99%).
3.3 Antimony trioxide (wSb2O3≥99.99%).
3.4 Lead dioxide (wPbO2≥99.99%).
3.5 Tin dioxide (wSnO2≥99.99%).
3.6 Bismuth trioxide (wBi2O3≥99.99%).
3.7 Sodium fluoride. pure superior grade.
3.8 Graphite powder. pure spectrum.
3.9 Buffer. Weigh 9.40g graphite powder (3.8), add 0.60g sodium fluoride (3.7), and grind well.
3.10 Compression mold. made of plexiglass rod car, the top is 2.9mm×2mm.
3.11 Argon (volume fraction not less than 99.99%).
3.12 Graphite electrode. pure spectrum, the structure and size of the upper electrode and the lower electrode are shown in Figure 1.
Unit is mm
a) Upper electrode b) Lower electrode
Figure 1 Graphite electrode structure and size
4 Equipment
DC arc atomic emission spectrometer.
5 samples
5.1 The particle size of niobium carbide is less than 150μm, and the particle size of niobium powder is less than 180μm.
5.2 Niobium hydroxide and niobium oxide should be pre-baked at 105°C~110°C for 2h, placed in a desiccator and cooled to room temperature for later use.
5.3 From the top 10cm of the niobium ingot to any part of the middle, use a planer to remove the skin and sample the shavings. The size of the shavings should be uniform, and
And the particles should be as small as possible.
6 Test procedure
6.1 Sample processing
Take about 1g of the sample and place it in a porcelain crucible or platinum crucible, in a box-type resistance furnace, heat up to 900 ℃ and burn for 1 hour (niobium wire and niobium ingot need to be burned
4h or more), make it completely converted into niobium pentoxide, take it out, and cool to room temperature.
6.2 Parallel test
Do two tests in parallel and take the average value.
6.3 Preparation of Spectral Sample
6.3.1 Weigh an appropriate amount of oxide sample (6.1) and buffer (3.9), mix at a ratio of 2.1, and grind uniformly.
6.3.2 Load the mixture (6.3.1) into the graphite electrode (3.12) and press it with a compression mold (3.10) to make the sample 1mm lower than the electrode port for measurement.
6.4 Determination
6.4.1 Standard sample preparation
Accurately weigh 9.3944g niobium pentoxide (3.1) in an agate mortar, and add 0.1320g arsenic trioxide (3.2) in sequence,
0.1197g antimony trioxide (3.3), 0.1154g lead dioxide (3.4), 0.1270g tin dioxide (3.5), 0.1115g bismuth trioxide
(3.6), grind well, prepare a master standard sample with a content of 1% of each measured element, and then gradually dilute it with niobium pentoxide (3.1) into a standard sample series.
See Table 2 for sample element content.
Weigh appropriate amounts of each standard sample and buffer (3.9) and treat them as per 6.3.
6.4.2 Recommended measurement conditions
The measurement conditions of the instrument are as follows.
---Light source. DC arc, current 15.5A;
--- Electrode spacing. 2mm;
---Pre-burning time. 2s;
---Exposure time. 50s;
---Refer to Table 3 for the recommended analysis spectrum of each element.
6.4.3 Measurement
In the DC arc atomic emission spectrometer (4), according to the recommended analysis line, determine the working curve standard (6.4.1) and analyze the sample
(6.3.2), check the background of the spectral lines of each element and correct it at the appropriate position, and the computer will automatically give each measured element in the niobium pentoxide
The quality score of the element.
7 Test data processing
The content of the measured element is calculated as the mass fraction wM of the measured element, calculated according to formula (1).
8 Precision
8.1 Repeatability
The measured values of two independent test results obtained under repeatability conditions are within the range of the average value given in Table 4.
The absolute difference does not exceed the repeatability limit (r), and the repeatability limit (r) does not exceed 5%. The repeatability limit (r) is linear according to the data in Table 4.
Obtained by interpolation or extension.
8.2 Reproducibility
The measured values of two independent test results obtained under reproducibility conditions are within the range of the average value given in Table 5.
The absolute difference does not exceed the reproducibility limit (R), and the reproducibility limit (R) does not exceed 5%. The reproducibility limit (R) is linear according to the data in Table 5.
Obtained by interpolation or extension.
9 Test report
The test report should include the following.
---Test object;
---This part number;
---result;
--- Anomalies observed;
---Test date.
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