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GB/T 20975.12-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 12: Determination of titanium content
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Methods for chemical analysis of aluminium and aluminium alloys - Part 12: Determination of titanium content
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GB/T 20975.12-2020
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| GB/T 20975.12-2008 | English | 674 |
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Methods for chemical analysis of aluminium and aluminium alloys -- Part 12: Determination of titanium content
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Basic data | Standard ID | GB/T 20975.12-2020 (GB/T20975.12-2020) | | Description (Translated English) | Methods for chemical analysis of aluminium and aluminium alloys - Part 12: Determination of titanium content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H12 | | Classification of International Standard | 77.120.10 | | Word Count Estimation | 10,166 | | Date of Issue | 2020-06-02 | | Date of Implementation | 2021-04-01 | | Older Standard (superseded by this standard) | GB/T 20975.12-2008 | | Quoted Standard | GB/T 8005.2; GB/T 8170-2008 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | | Summary | This standard specifies the diantipyridine methane spectrophotometric method and hydrogen peroxide spectrophotometric method for the determination of titanium content in aluminum and aluminum alloys. This standard applies to the arbitration determination of titanium content in aluminum and aluminum alloys. Determination range of diantipyridine methane spectrophotometry: 0.001 0%��0.50%; Determination range of hydrogen peroxide spectrophotometry: >0.50%��16.50%. | GB/T 20975.12-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 12: Determination of titanium content
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Methods for chemical analysis of aluminium and aluminium alloys--Part 12.Determination of titanium content
ICS 77.120.10
H12
National Standards of People's Republic of China
Replace GB/T 20975.12-2008
Chemical analysis methods of aluminum and aluminum alloys
Part 12.Determination of Titanium Content
2020-06-02 released
Implementation on 2021-04-01
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 20975 "Methods for Chemical Analysis of Aluminum and Aluminum Alloys" is divided into 37 parts.
---Part 1.Determination of mercury content;
---Part 2.Determination of arsenic content;
---Part 3.Determination of copper content;
---Part 4.Determination of iron content;
---Part 5.Determination of silicon content;
---Part 6.Determination of cadmium content;
---Part 7.Determination of manganese content;
---Part 8.Determination of zinc content;
---Part 9.Determination of lithium content by flame atomic absorption spectrometry;
---Part 10.Determination of tin content;
---Part 11.Determination of lead content;
---Part 12.Determination of titanium content;
---Part 13.Determination of vanadium content;
---Part 14.Determination of nickel content;
---Part 15.Determination of boron content;
---Part 16.Determination of magnesium content;
---Part 17.Determination of strontium content;
---Part 18.Determination of chromium content;
---Part 19.Determination of Zirconium Content;
---Part 20.Determination of Gallium Content Butyl Rhodamine B Spectrophotometry;
---Part 21.Determination of calcium content;
---Part 22.Determination of beryllium content;
---Part 23.Determination of antimony content;
---Part 24.Determination of total rare earth content;
---Part 25.Determination of element content by inductively coupled plasma atomic emission spectrometry;
---Part 26.Determination of carbon content by infrared absorption method;
---Part 27.Determination of cerium, lanthanum and scandium content by inductively coupled plasma atomic emission spectrometry;
---Part 28.Determination of cobalt content by flame atomic absorption spectrometry;
---Part 29.Determination of molybdenum content thiocyanate spectrophotometric method;
---Part 30.Determination of hydrogen content by heating extraction thermal conductivity method;
---Part 31.Determination of phosphorus content molybdenum blue spectrophotometric method;
---Part 32.Determination of Bismuth Content;
---Part 33.Determination of potassium content by flame atomic absorption spectrometry;
---Part 34.Determination of sodium content by flame atomic absorption spectrometry;
---Part 35.Determination of Tungsten Content Thiocyanate Spectrophotometric Method;
---Part 36.Determination of silver content by flame atomic absorption spectrometry;
--- Part 37.Determination of Niobium Content.
This part is Part 12 of GB/T 20975.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part replaces GB/T 20975.12-2008 "Methods for Chemical Analysis of Aluminum and Aluminum Alloy Part 12.Determination of Titanium Content", and
Compared with GB/T 20975.12-2008, the main technical changes except for editorial changes are as follows.
--- Added standard use safety warnings;
---Modified the measurement range of "Hydrogen Peroxide Spectrophotometry" from 0.5%~7.0% to >0.50%~16.50% (see
Chapter 1, Chapter 10 of the.2008 edition);
---Added normative reference documents (see Chapter 2);
---Modified the “diantipyrylmethane spectrophotometric method” weighing and the amount of reagents to dissolve samples (see 4.5,.2008 edition
6.3.1);
---Modified the pipetting volume of "Diantipyrylmethane spectrophotometry" (see 4.5.3, 6.3.2 of the.2008 edition);
--- Modified the weighing mass of "Hydrogen Peroxide Spectrophotometry" (see 5.5.1, 15.1 of the.2008 edition);
---Modified the pipetting volume and constant volume volume of "Hydrogen Peroxide Spectrophotometry" (see 5.5.3, 15.3 of the.2008 edition);
---Modified the working curve of "hydrogen peroxide spectrophotometry" (see 5.5, 15.4 of.2008 edition);
--- Deleted "Quality Control and Assurance" (Chapter 9 and Chapter 18 of the.2008 edition);
--- Added "Test Report" (see Chapter 6).
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. National Standard (Beijing) Inspection and Certification Co., Ltd., National Recycled Non-ferrous Metal Rubber and Plastic Materials Quality Supervision and Inspection Center,
Non-ferrous Metal Technology and Economic Research Institute, China Aluminum Materials Application Research Institute Co., Ltd., Beijing Non-ferrous Metals and Rare Earth Application Research Institute, Shan Dong Nanshan
Aluminum Co., Ltd., Chinalco Luoyang Copper Processing Co., Ltd., Guizhou Analysis and Testing Research Institute, Guangxi Liuzhou Yinhai Aluminum Co., Ltd.
Company, Xi’an Hantang Analysis and Testing Co., Ltd., Kunming Metallurgical Research Institute, Yingkou Zhongwang Aluminum Co., Ltd., South China University of Technology, Northeast Light Alloy
limited liability company.
The main drafters of this section. Song Yiyun, Wang Lele, Chen Xiongfei, Liu Ying, Wang Guiling, Xi Huan, Zhang Jine, Su Yulong, Zhang Juan, Xu Haiyan,
Liu Yingtao, Zhu Feng, Li Jiahua, Zhou Kai, Dai Fengying, Luo Fen, Liu Weili, Zheng Wei, Shang Yanyan, Zhang Yanbo, Wang Xue, Lu Ni, Song Guosheng, Zhou Bing.
The previous versions of the standards replaced by this part are as follows.
---GB/T 6987.12-1986, GB/T 6987.12-2001;
---GB/T 6987.31-2001;
---GB/T 20975.12-2008.
Chemical analysis methods of aluminum and aluminum alloys
Part 12.Determination of Titanium Content
Warning---Personnel using this section should have practical experience in formal laboratory work. This section does not point out all possible safety issues
question. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.
1 Scope
This part of GB/T 20975 specifies the diantipyrylmethane spectrophotometric method and hydrogen peroxide spectrophotometric method for the determination of aluminum and aluminum alloys
Medium titanium content.
This section applies to the arbitration determination of titanium content in aluminum and aluminum alloys. Diantipyrylmethane spectrophotometric determination range. 0.0010%~
0.50%; hydrogen peroxide spectrophotometric determination range. >0.50%~16.50%.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 8005.2 Terminology of Aluminum and Aluminum Alloy Part 2.Chemical Analysis
GB/T 8170-2008 Numerical rounding rules and the expression and determination of limit values
3 Terms and definitions
The terms and definitions defined in GB/T 8005.2 apply to this document.
4 Diantipyrylmethane spectrophotometry
4.1 Method summary
The sample is dissolved in hydrochloric acid and hydrogen peroxide, and ascorbic acid is used to reduce interference ions such as Fe3 and V5 in the presence of copper sulfate. In sulfuric acid
In the medium, add diantipyrylmethane solution to develop color, and measure the absorbance of the solution at the wavelength of 400.0nm in the spectrophotometer to determine the titanium
content.
4.2 Reagents
Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis.
4.2.1 Sulfuric acid (ρ=1.84g/mL)
4.2.2 Nitric acid (ρ=1.42g/mL).
4.2.3 Hydrofluoric acid (ρ=1.14g/mL).
4.2.4 Hydrogen peroxide (ρ=1.10g/mL).
4.2.5 Sulfuric acid (1 1).
4.2.6 Hydrochloric acid (1 1).
4.2.7 Copper sulfate solution (50g/L).
4.2.8 Ascorbic acid solution (20g/L), prepared immediately when used.
4.2.9 Diantipyrylmethane solution (50g/L). Dissolve 5g of diantipyrylmethane in about 17mL of hydrochloric acid (4.2.6) and 70mL of water
Alkane, diluted to 100mL with water and mixed.
4.2.10 Aluminum solution (10mg/mL). Weigh 10.00g pure aluminum (wAl≥99.99%, wTi≤0.0010%) into a.200mL beaker,
Cover the watch glass. Add 300mL hydrochloric acid (4.2.6) in batches, and slowly heat until the aluminum is completely dissolved. Take it off and let it cool. Move into 1000mL
In a volumetric flask, dilute to the mark with water and mix well.
4.2.11 Titanium standard storage solution. Weigh 0.1000g metallic titanium (wTi≥99.9%), add 50mL sulfuric acid in a 300mL beaker
(4.2.5) and 10mL of hydrochloric acid (4.2.6), add 1mL of nitric acid (1 1) after heating to decompose, heat until the titanium is completely dissolved, and continue to heat to evaporate
When the white smoke has just come out, remove it, cool it, carefully add about 10mL of water, dissolve the soluble salts, cool to room temperature, and transfer to a 1000mL volumetric flask
Dilute to the mark with water and mix well. 1mL of this solution contains 0.1mg of titanium.
4.2.12 Titanium standard solution A. Pipette 50.00mL titanium standard stock solution (4.2.11) into a 500mL volumetric flask and dilute to the mark with water.
Mix well (prepared when used). 1mL of this solution contains 0.01mg of titanium.
4.3 Apparatus
Spectrophotometer.
4.4 Sample
Process the sample into chips with a thickness not exceeding 1 mm.
4.5 Analysis steps
4.5.1 Sample
Weigh the mass (m0) to 0.50g sample (4.4), accurate to 0.0001g.
4.5.2 Parallel test
Do two tests in parallel and take the average value.
4.5.3 Determination
4.5.3.1 Place the sample (4.5.1) in a 250mL beaker, add 15mL of water, add 15mL of hydrochloric acid (4.2.6) in batches, drop by
Add 1.5mL hydrogen peroxide (4.2.4) or 0.5mL nitric acid (4.2.2), cover with a watch glass, slightly heat to dissolve the sample completely, boil for about 10min, use
Rinse the watch glass and cup wall with water, remove and cool. Transfer to a 100mL volumetric flask (V0), dilute to the mark with water, and mix. If there is insoluble matter (silicon
Etc.) Then filter in a 100mL volumetric flask (V0), put the precipitate and filter paper in a platinum crucible, ash (do not burn the filter paper), burn at 550℃
Boil for 30min, take out, and cool. Add 2mL sulfuric acid (4.2.1), 5mL hydrofluoric acid (4.2.3), dropwise add nitric acid (4.2.2) until the test solution is clear, steam
Let it dry, burn it at 700°C for a few minutes, take it out, and cool. Use a small amount of hydrochloric acid (4.2.6) to dissolve the residue (filter if it is turbid), and combine
In a 100mL volumetric flask (V0), dilute to the mark with water and mix well.
4.5.3.2 Pipette two portions of the test solution (4.5.3.1) of the corresponding volume (V1) according to Table 1, and place them in a 100mL volumetric flask, and add the corresponding volume
Aluminum solution (4.2.10). Add 25mL sulfuric acid (4.2.5), add water to about 80mL, add 2 drops of copper sulfate solution (4.2.7), 2mL ascorbic acid
Blood acid solution (4.2.8), mix well.
4.5.3.3 One part does not add diantipyrylmethane solution (4.2.9), this is the compensation solution; the other part is added with 10mL diantipyrylmethane solution
Alkane solution (4.2.9). After cooling the two solutions to room temperature, dilute to the mark with water and mix well. Leave it for 30 minutes.
4.5.3.4 Move a part of the solution (4.5.3.3) into the absorption cell, use the compensation solution as the reference solution, and measure at 400.0nm of the spectrophotometer
Absorbance, check the corresponding amount of titanium (m1) from the working curve.
4.5.4 Drawing of working curve
4.5.4.1 According to the titanium mass fraction in the sample, the preparation of the series of standard solutions is divided into the following two types.
a) When the titanium mass fraction is 0.0010%~0.010%. pipette 0mL, 0.25mL, 0.50mL, 1.00mL, 2.00mL,
3.00mL titanium standard solution A (4.2.12) in a set of 100mL volumetric flasks, respectively add 25.0mL aluminum solution (4.2.10);
b) When the titanium mass fraction is >0.010%~0.50%. pipette 0mL, 2.00mL, 4.00mL, 8.00mL, 12.00mL,
16.00 mL titanium standard solution A (4.2.12) was put into a set of 100 mL volumetric flasks, and 25.0 mL aluminum solution
Liquid (4.2.10).
4.5.4.2 Add 25mL sulfuric acid (4.2.5), add water to about 80mL, add 2 drops of copper sulfate solution (4.2.7), 2mL ascorbic acid solution
(4.2.8), mix well; then add 10mL diantipyrimethane solution (4.2.9), after the solution is cooled to room temperature, dilute to the mark with water, mix
uniform. Leave it for 30 minutes.
4.5.4.3 Move part of the series of standard solutions (4.5.4.1) into the absorption tank, and use the reagent blank solution (without the titanium standard solution) as a reference.
Measure the absorbance at 400.0nm with a spectrophotometer, and draw the working curve with the amount of titanium as the abscissa and absorbance as the ordinate.
4.6 Test data processing
The titanium content is calculated as the mass fraction wTi of titanium and calculated according to formula (1).
The calculation result retains two significant digits, and the numerical rounding is performed in accordance with 3.2 and 3.3 of GB/T 8170-2008.
4.7 Precision
4.7.1 Repeatability
The measured value of two independent test results obtained under repeatability conditions, within the average range given below, 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 within the linear range according to the data in Table 2.
Obtained by interpolation or extension method.
4.7.2 Reproducibility
The measured values of two independent test results obtained under reproducibility conditions are within the average range given below. These two test results
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 3.
Obtained by interpolation or extension.
5 Hydrogen peroxide spectrophotometry
5.1 Method summary
The sample is dissolved in sodium hydroxide solution, neutralized to acidity with a mixed acid of sulfuric acid and nitric acid, and hydrogen peroxide is added to make it color, and then the spectrophotometer
At a wavelength of 410.0nm, measure the absorbance of the solution to determine the titanium content.
5.2 Reagents
Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis.
5.2.1 Sodium hydroxide solution (400g/L), stored in a polyethylene bottle.
5.2.2 Nitric acid (11).
5.2.3 Sulfuric acid (1 1).
5.2.4 Hydrogen peroxide (1 9).
5.2.5 Mixed acid. add 160mL sulfuric acid (11) and 340mL nitric acid (ρ=1.42g/mL) to 500mL water.
5.2.6 Titanium standard solution B. Weigh 0.1000g metallic titanium (wTi≥99.9%) into a 300mL beaker, add 50mL sulfuric acid (5.2.3)
And 10mL of hydrochloric acid (1 1) after heating to decompose, then add 1mL of nitric acid (5.2.2), heating until the titanium is completely dissolved, and continue to heat to evaporate
Remove the white smoke, cool it, carefully add about 10mL of water, dissolve the soluble salts, cool to room temperature, transfer it to a 1000mL volumetric flask, and add water
Dilute to the mark and mix well. 1mL of this solution contains 0.1mg of titanium.
5.3 Apparatus
Spectrophotometer.
5.4 Sample
Process the sample into chips with a thickness not exceeding 1 mm.
5.5 Analysis steps
5.5.1 Sample
According to Table 4, weigh the corresponding mass (m2) of the sample (5.4), accurate to 0.0001g.
5.5.2 Parallel test
Do two tests in parallel and take the average value.
5.5.3 Determination
5.5.3.1 Place the sample (5.5.1) in a 300mL beaker, cover with a watch glass, add 10mL sodium hydroxide solution (5.2.1), wait for a violent reaction
After stopping, heat to completely dissolve. After cooling, rinse the watch glass and the wall of the cup with a small amount of water, add 50mL mixed acid (5.2.5) while stirring, add
Heat to dissolve salts, boil to drive off nitrogen oxides, and cool to room temperature. Transfer to a.200mL volumetric flask, dilute to the mark with water, and mix.
5.5.3.2 Pipette two portions of test solution (5.5.3.1) according to Table 4, put them in a 50mL volumetric flask, add 15mL mixed acid (5.2.5), one of them
Add 5 mL of hydrogen peroxide (5.2.4) in one portion, and no hydrogen peroxide (5.2.4) in the other portion. This solution is a compensation solution; dilute to the mark with water and mix.
uniform. Take water as a reference, use an absorption cell of appropriate specifications, measure the absorbance at 410.0nm in a spectrophotometer, and subtract the absorbance of the compensation solution
Afterwards, check the corresponding amount of titanium (m3) from the working curve.
5.5.4 Drawing of working curve
Pipette 0mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL, 12.00mL titanium standard solution B
(5.2.6), put them in 8 50mL volumetric flasks, respectively add 15mL mixed acid (5.2.5), 5mL hydrogen peroxide (5.2.4), and water
Dilute to the mark and mix well. Pipette a series of standard solutions into the absorption cell, and measure it at the wavelength of 410.0nm in the spectrophotometer, using water as the reference.
Absorbance. Use the amount of titanium as the abscissa and subtract the absorbance of the reagent blank solution as the ordinate to draw a working curve.
5.6 Test data processing
The titanium content is calculated as the mass fraction wTi of titanium and calculated according to formula (2).
5.7 Precision
5.7.1 Repeatability
The measured value of two independent test results obtained under repeatability conditions, within the average range given below, these two test results
The absolute difference of r 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 5.
Obtained by interpolation or extension.
5.7.2 Reproducibility
The measured values of two independent test results obtained under reproducibility conditions are within the average range given below. These two test results
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 6.
Obtained by interpolation or extension.
6 Test report
The test report should include the following.
a) The number, name and method used in this section;
b) All necessary information about identification of samples, laboratory, analysis date, report date, etc.;
c) Express the test results in an appropriate form;
d) Abnormal phenomena during the test;
e) Signatures of review and approval personnel.
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