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GB/T 4698.10-2020: Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 10: Determination of chromium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry (with vanadium)
Status: Valid GB/T 4698.10: Evolution and historical versions
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| GB/T 4698.10-2020 | English | 189 |
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Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 10: Determination of chromium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry (with vanadium)
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GB/T 4698.10-2020
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| GB/T 4698.10-1996 | English | 239 |
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Sponge titanium, titanium and titanium alloys. Determination of chromium content in thepresence of Vanadium. Ammonium ferrous sulfate titration method
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GB/T 4698.10-1996
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| GB/T 4698.10-1984 | English | RFQ |
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Methods for chemical analysis of titanium and titanium alloys--The ammonium ferrous sulfate volumetric method for the determination of chromium content in the presence of vanadium
| Obsolete |
GB/T 4698.10-1984
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PDF similar to GB/T 4698.10-2020
Basic data | Standard ID | GB/T 4698.10-2020 (GB/T4698.10-2020) | | Description (Translated English) | Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 10: Determination of chromium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry (with vanadium) | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.50 | | Word Count Estimation | 10,127 | | 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 4698.10-2020: Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 10: Determination of chromium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry (with vanadium)
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Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 10.Determination of chromium content - Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry (with vanadium)
ICS 77.120.50
H14
National Standards of People's Republic of China
Replace GB/T 4698.10-1996
Sponge titanium, titanium and titanium alloy chemical analysis methods
Part 10.Determination of Chromium Content
Ferrous ammonium sulfate titration and inductively coupled plasma
Atomic emission spectrometry (with vanadium)
2020-03-06 released
2021-02-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 4698 "Methods for Chemical Analysis of Sponge Titanium, Titanium and Titanium Alloys" is divided into the following parts.
---Part 1.Determination of copper content by flame atomic absorption spectrometry;
---Part 2.Determination of iron content 1,10-phenanthroline spectrophotometry, flame atomic absorption spectrometry and inductively coupled plasma
Bulk atomic emission spectroscopy;
---Part 3.Determination of silicon content molybdenum blue spectrophotometry;
---Part 4.Determination of manganese content, periodate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 5.Determination of molybdenum content, thiocyanate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 6.Determination of Boron Content Curcumin Spectrophotometry;
---Part 7.Determination of Oxygen and Nitrogen Inert Gas Melting-Infrared Absorption/Thermal Conductivity Method and Distillation Separation-Nessler Reagent Spectroscopy
Degree method;
---Part 8.Determination of aluminum content by alkali separation-EDTA complexometric titration and inductively coupled plasma atomic emission spectrometry;
---Part 9.Determination of tin content by potassium iodate titration and inductively coupled plasma atomic emission spectrometry;
---Part 10.Determination of chromium content by ferrous ammonium sulfate titration and inductively coupled plasma atomic emission spectrometry (including vanadium);
---Part 11.Determination of chromium content by ferrous ammonium sulfate titration and inductively coupled plasma atomic emission spectrometry (without vanadium);
---Part 12.Determination of vanadium content by ferrous ammonium sulfate titration and inductively coupled plasma atomic emission spectrometry;
---Part 13.Determination of the amount of zirconium inductively coupled plasma atomic emission spectrometry;
---Part 14.Determination of carbon content high frequency combustion-infrared absorption method;
---Part 15.Determination of the amount of hydrogen inert gas melting infrared absorption method/thermal conductivity method;
---Part 17.Determination of magnesium content by flame atomic absorption spectrometry;
---Part 18.Determination of tin content by flame atomic absorption spectrometry;
---Part 19.Determination of Molybdenum Content Thiocyanate Differential Spectrophotometry;
---Part 21.Determination of manganese, chromium, nickel, aluminum, molybdenum, tin, vanadium, yttrium, copper, and zirconium by atomic emission spectrometry;
---Part 22.Determination of the amount of niobium 5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 23.Determination of palladium content, stannous chloride-potassium iodide spectrophotometry and inductively coupled plasma atomic emission spectrometry;
---Part 24.Determination of Nickel Content Dimethylglyoxime Spectrophotometry and Inductively Coupled Plasma Atomic Emission Spectrometry;
---Part 25.Determination of chlorine content, silver chloride spectrophotometric method;
---Part 26.Determination of alloying elements and impurity elements inductively coupled plasma atomic emission spectrometry;
---Part 27.Determination of the amount of neodymium inductively coupled plasma atomic emission spectrometry;
---Part 28.Determination of ruthenium content by inductively coupled plasma atomic emission spectrometry;
--- Part 29.Determination of tungsten and tantalum content inductively coupled plasma atomic emission spectrometry.
This part is Part 10 of GB/T 4698.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part replaces GB/T 4698.10-1996 "Methods for Chemical Analysis of Sponge Titanium, Titanium and Titanium Alloys for the Determination of Chromium by Ferrous Ammonium Sulfate Titration"
Quantity (with vanadium)". Compared with GB/T 4698.10-1996, the main technical changes in this part are as follows except for editorial changes.
---Modified the measurement range, changed the measurement range from "0.30%~12.00%" to "The measurement range of method one is 0.30%~
The determination range of 15.00% and Method 2 is 0.010%~15.00%" (see Chapter 1, Chapter 1 of the.1996 edition);
---Added the arbitration analysis method (see Chapter 2);
--- Added precision clause (see 2.6 and 3.7);
---Inductively coupled plasma atomic emission spectrometry has been added (see Chapter 3);
---Added the test report (see Chapter 4).
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. Xi'an Hantang Analysis and Testing Co., Ltd., Guangdong Industrial Analysis and Testing Center, Western Metal Materials Co., Ltd.
Company, Baoti Group Co., Ltd., Chinalco Shenyang Nonferrous Metal Processing Co., Ltd., Shenzhen Zhongjin Lingnan Nonferrous Metal Co., Ltd., China
Standard (Beijing) Inspection and Certification Co., Ltd., Youyan Yijin New Materials Co., Ltd.
The main drafters of this section. Wang Jinlei, Liu Leilei, Sun Baolian, Zhu Li, Rowling, Wang Fang, Wang Jin, Xiong Xiaoyan, Li Juan, Kong Lingchen, Sun Aiping,
Hao Siwen, Chen Yuxia, Zuo Hongyi, Zhang Lijiu, Sun Haifeng, Li Manzhi, Liu Chaofang, Wang Weihua.
The previous versions of the standards replaced by this part are as follows.
---GB/T 4698.10-1984, GB/T 4698.10-1996.
Sponge titanium, titanium and titanium alloy chemical analysis methods
Part 10.Determination of Chromium Content
Ferrous ammonium sulfate titration and inductively coupled plasma
Atomic emission spectrometry (with vanadium)
1 Scope
This part of GB/T 4698 specifies the method for determining the amount of chromium (including vanadium) in sponge titanium, titanium and titanium alloys.
This section applies to the determination of chromium in sponge titanium, titanium and titanium alloys (the main component of titanium alloys contains vanadium). Method one measurement range
Circumference. 0.30%~15.00%; Method 2 measurement range. 0.010%~15.00%. When the scope of determination overlaps, method one in this section is arbitration
method.
2 Method-Ferrous ammonium sulfate titration method
2.1 Principle
The sample is dissolved in sulfuric acid, and in a sulfuric acid medium at room temperature, the vanadium is oxidized to a high price with potassium permanganate, and the standard drop of ferrous ammonium sulfate is used.
Titrate vanadium with a constant solution.
Under heating conditions, using silver nitrate as a catalyst, ammonium persulfate is used to simultaneously oxidize vanadium and chromium to high prices, and then use ferrous ammonium sulfate standard
The titration solution titrates vanadium and chromium.
The difference between the volume of the titrant consumed in the two titrations is the volume of the titrant required for the titration of chromium, from which the amount of chromium is obtained.
2.2 Reagents
Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis.
2.2.1 Nitric acid (ρ=1.42g/L).
2.2.2 Sulfuric acid (1 1).
2.2.3 Potassium permanganate solution (5g/L).
2.2.4 Urea solution (100g/L).
2.2.5 Sodium nitrite solution (10g/L).
2.2.6 Silver nitrate solution (10g/L).
2.2.7 Ammonium persulfate solution (250g/L), prepared immediately after use.
2.2.8 Sodium chloride solution (100g/L).
2.2.9 Chromium standard solution. weigh 2.8290g of potassium dichromate (reference reagent) dried at 105°C for 1h and cooled to room temperature in 500mL
In the beaker, add about 100mL of water to dissolve it, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. This solution 1mL contains
1.0mg chromium.
2.2.10 Preparation of ferrous ammonium sulfate standard titration solution [c(Fe2)≈0.025mol/L]. Weigh 10.0g ferrous ammonium sulfate [Fe(SO4)·
(NH4)2SO4·6H2O] was placed in a 500mL beaker, and.200mL sulfuric acid (2.2.2) was added to dissolve it. Transfer into 1000mL capacity
In the bottle, dilute to the mark with water and mix well.
2.2.11 Calibration of ferrous ammonium sulfate standard titration solution. Pipette three 10.00mL chromium standard solutions (2.2.9) into three 500mL cones.
In the flask, add 25mL sulfuric acid (2.2.2), 2 drops of manganese sulfate solution (50g/L), and perform the other operations according to 2.4.4.5~2.4.4.7.parallel
The volume range of the standard titration solution (2.2.10) of ferrous ammonium sulfate consumed for calibration should be no more than 0.10mL, whichever is the average value. According to formula (1)
Calculate the actual concentration of the ferrous ammonium sulfate titration solution (2.2.10).
2.2.12 N-phenylanthranilic acid solution (2g/L). Weigh 0.2g of N-phenylanthranilic acid and dissolve in 100mL sodium carbonate solution.
Solution (2g/L).
2.3 Sample
Follow the published sampling standards for titanium sponge, titanium and titanium alloys.
2.4 Test procedure
2.4.1 Sample
Weigh the sample (2.3) according to Table 1, accurate to 0.0001g.
2.4.2 Parallel test
Do two tests in parallel and take the average value.
2.4.3 Blank test
Do a blank test with the sample.
2.4.4 Determination
2.4.4.1 Place the sample (2.4.1) in a 500mL conical flask, add 25mL sulfuric acid (2.2.2), heat to dissolve the sample, and add nitric acid dropwise
(2.2.1) To the solution purple disappears, heat to remove nitrogen oxides, and cool.
2.4.4.2 Dilute with water to about 100mL, add potassium permanganate solution (2.2.3) dropwise until the solution is stable red, and leave it for 3min.
2.4.4.3 Add 10mL urea solution (2.2.4), add sodium nitrite solution (2.2.5) dropwise under shaking until the red color of the solution disappears, and place
2min.
2.4.4.4 Add 5 drops of N-phenylanthranilic acid solution (2.2.12) and titrate to solution with ferrous ammonium sulfate standard titration solution (2.2.10)
The end point is the change from pink to yellow-green.
2.4.4.5 Dilute the solution (2.4.4.4) with water to.200mL, add 5mL silver nitrate solution (2.2.6), 10mL ammonium persulfate solution
(2.2.7), heat the solution until the red color of permanganic acid appears, and boil until big bubbles appear.
2.4.4.6 Remove, add 5mL sodium chloride solution (2.2.8), heat and boil until the solution red disappears, remove, cool to room temperature with running water.
2.4.4.7 Add 10mL sulfuric acid (2.2.2), 5 drops of N-phenylanthranilic acid solution (2.2.12), and use ferrous ammonium sulfate standard titration solution
(2.2.10) Titration until the solution changes from pink to yellow-green is the end point.
2.5 Test data processing
2.6 Precision
2.6.1 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 case of exceeding the repeatability limit (r) does not exceed 5%. Repeatability limit (r) adopts the line according to the data in Table 2
Obtained by sexual interpolation or extension method.
2.6.2 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 does not exceed 5% in the case of exceeding the reproducibility limit (R). Reproducibility limit (R) is adopted according to the data in Table 3
Obtained by linear interpolation or extension method.
3 Method two inductively coupled plasma atomic emission spectrometry
3.1 Principle
Dissolve the sample with hydrochloric acid and hydrofluoric acid, and add titanium oxide nitrate dropwise. Use inductively coupled plasma atomic emission spectrometry to determine
Calculate the mass concentration of chromium by curve method, and express the measurement result by mass fraction.
3.2 Reagents
Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis.
3.2.1 Hydrochloric acid (ρ=1.18g/mL).
3.2.2 Hydrofluoric acid (ρ=1.15g/mL).
3.2.3 Nitric acid (ρ=1.42g/mL).
3.2.4 Chromium standard storage solution. weigh 2.8290g of potassium dichromate (reference reagent) dried at 105°C for 1h and cooled to room temperature in 500mL
In the beaker, add about 100mL of water to dissolve it, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. This solution 1mL contains
1.0mg chromium.
3.2.5 Chromium standard solution A. Pipette 10.00mL chromium standard stock solution (3.2.4) into a 100mL volumetric flask, add 5mL hydrochloric acid
(3.2.1), dilute to the mark with water, and mix well. This solution 1mL contains 100μg chromium.
3.2.6 Chromium standard solution B. Pipette 10.00mL chromium standard solution A (3.2.5) into a 100mL volumetric flask, add 5mL hydrochloric acid
(3.2.1), dilute to the mark with water, and mix well. This solution 1mL contains 10μg chromium.
3.2.7 Titanium (wTi≥99.95%, wCr< 0.001%).
3.2.8 Argon (volume fraction ≥99.99%).
3.3 Apparatus
3.3.1 Inductively coupled plasma atomic emission spectrometer. equipped with a hydrofluoric acid resistant sampling system, with a resolution of less than 0.006nm (at.200nm).
3.3.2 The recommended wavelength of the chromium element analysis line is 283.56nm.
3.4 Sample
Follow the published sampling standards for titanium sponge, titanium and titanium alloys.
3.5 Test procedure
3.5.1 Sample
Weigh 0.10g sample (3.4), accurate to 0.0001g.
3.5.2 Parallel test
Do two tests in parallel and take the average value.
3.5.3 Blank test
Do a blank test with the sample.
3.5.4 Preparation of test solution
3.5.4.1 Preparation of analysis test solution
Place the sample (3.5.1) in a polytetrafluoroethylene beaker, blow in a small amount of water, add 5 mL of hydrochloric acid (3.2.1), and add 1 mL of hydrofluoric acid
(3.2.2), heat at low temperature until the sample is completely dissolved, then add 0.5mL nitric acid (3.2.3) dropwise until the solution is clear. Remove and cool to room temperature,
Transfer to a 100mL plastic volumetric flask, dilute to the mark with water, and mix.
For samples containing chromium ≥ 8%, it is necessary to separate them for determination. Pipette 10.00mL of the above test solution into a 100mL volumetric flask, add 2mL of salt
Acid (3.2.1), dilute to the mark with water, and mix well.
3.5.4.2 Preparation of standard series solutions
Curve 1 (the mass fraction of chromium is 0.010%~8.00%). Weigh 7 parts of titanium metal (3.2.7) equivalent to the titanium content of the sample (3.5.1)
In a series of 100mL PTFE beakers, dissolve the sample according to 3.5.4.1 along with the sample. After the solution is cooled, transfer 7 100mL plastic
Material in a volumetric flask. Add 0mL, 1.00mL chromium standard solution B (3.2.6), 1.00mL chromium standard solution A (3.2.5), 1.00mL,
2.00mL, 4.00mL, 8.00mL chromium standard stock solution (3.2.4), dilute to the mark with water, and mix.
Curve 2 (the mass fraction of chromium is 8.00%~15.00%). Weigh the metal titanium (3.2.7) with the titanium content of the sample (3.5.1) into one
In a 100mL polytetrafluoroethylene beaker, dissolve, cool and dilute with the sample according to 3.5.4.1.Divide 10.00mL test solution into 6
100mL plastic volumetric flask. Add 0mL, 3.00mL, 6.00mL, 9.00mL chromium standard solution A (3.2.5), 1.20mL,
1.60mL chromium standard stock solution (3.2.4), dilute to the mark with water, and mix.
3.6 Determination
Measure the working curve solution on the inductively coupled plasma emission spectrometer at the recommended wavelength, when the linear correlation coefficient of the working curve
When k≥0.999, measure the emission intensity of the test element in the analysis test solution (3.5.4.1) and the accompanying sample blank solution (3.5.3), from the working curve
Check the mass concentration of chromium.
3.7 Test data processing
The amount of chromium is calculated by the mass fraction wCr of chromium, calculated according to formula (3).
When the result is less than or equal to 0.10%, two significant digits are reserved; when the result is greater than 0.10%, it is reserved to two decimal places.
3.8 Precision
3.8.1 Repeatability
The measured values of two independent test results obtained under repeatability conditions are within the average range given in Table 4, and the 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 4.
Obtained by sexual interpolation or extension method.
3.8.2 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 based on the data in Table 5.
Obtained by sexual interpolation or extension method.
4 Test report
The test report should include the following.
---Test object;
--- Standards used (including release and publication year number);
---Method used;
---result;
--- Anomalies observed;
---Test date.
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