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GB/T 15076.4-2020: Methods for chemical analysis of tantalum and niobium - Part 4: Determination of iron content - 1, 10-Phenanthroline spectrophotometry
Status: Valid GB/T 15076.4: Evolution and historical versions
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| GB/T 15076.4-2020 | English | 119 |
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Methods for chemical analysis of tantalum and niobium - Part 4: Determination of iron content - 1, 10-Phenanthroline spectrophotometry
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GB/T 15076.4-2020
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| GB/T 15076.4-1994 | English | 239 |
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Methods for chemical analysis of tantalum and niobium. Determination of iron content
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GB/T 15076.4-1994
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Basic data | Standard ID | GB/T 15076.4-2020 (GB/T15076.4-2020) | | Description (Translated English) | Methods for chemical analysis of tantalum and niobium - Part 4: Determination of iron content - 1, 10-Phenanthroline spectrophotometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 6,617 | | 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 15076.4-2020: Methods for chemical analysis of tantalum and niobium - Part 4: Determination of iron content - 1, 10-Phenanthroline spectrophotometry
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Methods for chemical analysis of tantalum and niobium - Part 4.Determination of iron content--1, 10-Phenanthroline spectrophotometry
ICS 77.120.99
H14
National Standards of People's Republic of China
Replace GB/T 15076.4-1994
Tantalum-niobium chemical analysis method
Part 4.Determination of iron content
1,10-phenanthroline spectrophotometry
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 4 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 15076.4-1994 "Methods for chemical analysis of tantalum and niobium-Determination of iron content". This part and GB/T 15076.4-
Compared with.1994, the main technical changes except for editorial changes are as follows.
---Expanded the measurement range. the measurement range was changed from " >0.020%~0.30%" to " >0.020%~0.50%" (see Chapter 1,
Chapter 1 of the.1994 edition);
---The reference standard is deleted (see Chapter 2 of the.1994 edition);
--- Amend "Hydroxyamine Hydrochloride Solution" to "Ascorbic Acid Solution" (see 3.13, 4.5 in.1994 edition);
--- Added "acetic acid-ammonium acetate buffer solution" (see 3.14);
--- Modify the total volume of the test solution "50mL" to "100mL" (see 6.4.1,.1994 version 6.2);
---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 Dongfang Tantalum Co., Ltd., Guangdong Guangsheng Rare Metal Photoelectric New Material Co., Ltd., Northwest Rare
Metal Materials Research Institute Ningxia Co., Ltd., Jiujiang Nonferrous Metal Smelting Co., Ltd., Xi'an Hantang Analysis and Testing Co., Ltd., China Nonferrous Guizhou
Forest Mineral Geology Research Institute Co., Ltd., Guangdong Zhiyuan New Materials Co., Ltd.
The main drafters of this section. Xu Ninghui, Huang Shuang, Zhang Junfeng, Zhang Zhong, Wang Jiali, Xuan Hongjian, Li Tuo, Huang Huan, Yuan Hui, Wang Shumei, Xu Xiaona.
The previous versions of the standards replaced by this part are as follows.
---GB/T 15076.4-1994.
Tantalum-niobium chemical analysis method
Part 4.Determination of iron content
1,10-phenanthroline spectrophotometry
1 Scope
This part of GB/T 15076 specifies the 1,10-phenanthroline spectrophotometric method for the determination of iron content in tantalum and niobium.
This section applies to the determination of iron content in tantalum, niobium and their hydroxides and oxides. Measuring range. >0.020%~0.50%.
2 Principle
The sample is dissolved with hydrofluoric acid and nitric acid, tartaric acid-boric acid complexes the main body, fluorine and other impurity elements, and the ferric ion is reduced by ascorbic acid
It is a divalent iron ion. In a buffer solution with a pH of about 5, the divalent iron ion forms a red complex with 1,10-phenanthroline.
Measure the absorbance at 510nm with a meter.
3 Reagents and materials
Unless otherwise specified, only reagents and laboratory secondary water confirmed to be pure superior grade are used in the analysis.
3.1 Hydrofluoric acid (ρ=1.14g/mL).
3.2 Hydrochloric acid (ρ=1.18g/mL).
3.3 Nitric acid (ρ=1.42g/mL).
3.4 Acetic acid (ρ=1.05g/mL).
3.5 Hydrochloric acid (1 1).
3.6 Acetic acid (1 1).
3.7 Tartaric acid. analytically pure.
3.8 Boric acid.
3.9 Ascorbic acid. analytically pure.
3.10 Ammonium acetate. analytically pure.
3.11 1,10-phenanthroline. analytically pure.
3.12 Tartaric acid-boric acid solution. Weigh 10g tartaric acid (3.7) and 6g boric acid (3.8) into a 250mL beaker, add 80mL water, add
After hot dissolution, cool, transfer to a 100mL volumetric flask, dilute to the mark with water, and mix.
3.13 Ascorbic acid solution (20g/L). Weigh 2g ascorbic acid (3.9) into a 250mL beaker, add 50mL water, stir to dissolve it
After all, transfer to a 100mL volumetric flask, dilute to the mark with water, and mix well. Available now.
3.14 Acetic acid-ammonium acetate buffer solution (pH=5). Weigh.200g of ammonium acetate (3.10) into a 500mL volumetric flask, add.200mL of water, and add
Heat to dissolve completely, cool, add 50mL acetic acid (3.6), transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix.
3.15 1,10-phenanthroline ethanol solution (4g/L). Weigh 4g of 1,10-phenanthroline (3.11) into a 100mL beaker and add 20mL
After stirring and dissolving ethanol, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix well.
3.16 Niobium metal (wNb≥99.99%, wFe≤0.0001%).
3.17 Metal tantalum (wTa≥99.99%, wFe≤0.0001%).
3.18 Iron standard storage solution. Weigh 1.0000g of high-purity metallic iron (wFe≥99.99%), place it in a 250mL beaker, and add 50mL
Hydrochloric acid solution (3.5), dissolved at low temperature. After the dissolution is complete, cool, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. this
Solution 1mL contains 1mg iron.
3.19 Iron standard solution A. accurately pipette 10.00mL iron standard stock solution (3.18) into a 100mL volumetric flask, add 10mL hydrochloric acid
(3.5), dilute to the mark with water, and mix well. This solution 1mL contains 100μg iron.
3.20 Iron standard solution B. accurately pipette 10.00mL iron standard solution A (3.19) into a 100mL volumetric flask, add 10mL hydrochloric acid
(3.5), dilute to the mark with water, and mix well. This solution 1mL contains 10μg iron.
4 Equipment
Spectrophotometer.
5 samples
5.1 The particle size of tantalum powder is less than 700μm; the particle size of niobium powder is less than 180μm.
5.2 Tantalum powder should be dried in vacuum at 80℃~150℃ for 4h in advance, cooled to room temperature, and vacuum packaged in a composite aluminum foil bag;
Substances and oxides should be pre-baked at 105℃~110℃ for 2h, and placed in a desiccator to cool to room temperature for later use.
5.3 From the top 10cm of the tantalum ingot or niobium ingot to any part of the middle, use a planer to remove the skin and sample the shavings. The size of the debris should be
Uniform, and the particles should be as small as possible.
6 Test procedure
6.1 Sample
Weigh 0.20g sample, accurate to 0.0001g.
6.2 Parallel test
Do two tests in parallel and take the average value.
6.3 Blank test
Do a blank test with the sample.
6.4 Determination
6.4.1 Place the sample (6.1) in a 30mL platinum crucible and wet it with water. Add 2mL of hydrofluoric acid (3.1) to the tantalum sample or 4mL of the niobium sample
Hydrofluoric acid (3.1), add nitric acid (3.3) dropwise, heat at low temperature until the sample is completely dissolved, remove and cool to room temperature, add 20mL tartaric acid-boric acid to dissolve
Solution (3.12), transfer the solution into a 100mL polyethylene volumetric flask pre-added with 10mL tartaric acid-boric acid solution (3.12), dilute with water to
Scale and mix well. When the oxide is not easy to dissolve to clarification by this method, a hot-pressure digestion device can be used to dissolve the sample.
6.4.2 Divide the above solution (6.4.1) according to Table 1 into a 25mL colorimetric tube, add 2mL ascorbic acid solution (3.13), 5mL acetic acid-ethyl
Ammonium acid buffer solution (3.14), 2.5mL 1,10-phenanthroline ethanol solution (3.15), (each reagent needs to be mixed), diluted with water to
Shake well and place for 5min.
6.4.3 Move part of the solution (6.4.2) into a cuvette according to Table 1, take water as a reference, and measure its absorption at a wavelength of 510 nm on a spectrophotometer.
Luminosity.
6.4.4 Subtract the absorbance of the blank solution accompanying the sample, and check the corresponding iron content from the working curve.
6.5 Drawing of working curve
6.5.1 Pipette 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL iron standard solution B (3.20) into
In a 25mL colorimetric tube, add 5mL tartaric acid-boric acid solution (3.12), and the rest of the operation is carried out according to 6.4.2~6.4.3.
6.5.2 Subtract the absorbance of the reagent blank, use the iron content as the abscissa and the absorbance as the ordinate to draw the working curve.
7 Test data processing
The iron content is calculated as the mass fraction of iron wFe, calculated according to formula (1).
The result is to three decimal places.
8 Precision
8.1 Repeatability
The measured values of two independent test results obtained under repeatability conditions are within the average range given in Table 2.These two test results
The absolute difference does not exceed the repeatability limit (r), and the repeatability limit (r) does not exceed 5%. The repeatability limit (r) is based on the data in Table 2.
Obtained by sexual interpolation or extension method.
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 3.
The absolute difference does not exceed the reproducibility limit (R), and the case of exceeding the reproducibility limit (R) does not exceed 5%. Reproducibility limit (R) adopts the line according to the data in Table 3
Obtained by sexual interpolation or extension method.
9 Test report
The test report should include the following.
---Test object;
---This part number;
---result;
--- Anomalies observed;
---Test date.
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