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GB/T 4702.18-2020: Chromium metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophotometry method
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Chromium metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophotometry method
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GB/T 4702.18-2020
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Basic data | Standard ID | GB/T 4702.18-2020 (GB/T4702.18-2020) | | Description (Translated English) | Chromium metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophotometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.100 | | Word Count Estimation | 10,129 | | Date of Issue | 2020-03-06 | | Date of Implementation | 2020-07-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 4702.18-2020: Chromium metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophotometry method
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Chromium metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophotometry method
ICS 77.100
H11
National Standards of People's Republic of China
Determination of metal chromium and vanadium content
Tantalum Reagent Trichloromethane Extraction Spectrophotometry
2020-03-06 released
2020-07-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 4702 is divided into the following parts.
---GB/T 4702.1 Determination of metal chromium and chromium content by ferrous ammonium sulfate titration method;
---GB/T 4702.2 Determination of metal chromium and silicon content perchloric acid gravimetric method;
---GB/T 4702.3 Determination of metallic chromium phosphorus-Bismuth phosphorus molybdenum blue spectrophotometric method;
---GB/T 4702.4 Determination of metallic ferrochromium content by EDTA titration method and flame atomic absorption spectrometry;
---GB/T 4702.5 Determination of metal chromium and aluminum content-Ethylenediaminetetraacetic acid disodium titration method and flame atomic absorption spectrometry;
---GB/T 4702.6 Determination of metallic ferrochrome, aluminum, silicon and copper content by inductively coupled plasma atomic emission spectrometry;
---GB/T 4702.7 Determination of metal chromium nitrogen content-Distillation separation-Nessler reagent spectrophotometry;
---GB/T 4702.8 Method for chemical analysis of chromium metal, distillation-molybdenum blue spectrophotometric method for the determination of arsenic content;
---GB/T 4702.9 Method for chemical analysis of chromium metal, crystal violet spectrophotometric method for the determination of antimony content;
---GB/T 4702.10 Method for chemical analysis of chromium metal. Copper reagent spectrophotometric method for the determination of copper content;
---GB/T 4702.11 Method for chemical analysis of chromium metal; Alizarin violet spectrophotometric method for the determination of tin content;
---GB/T 4702.14 Method for chemical analysis of chromium metal, infrared absorption method for the determination of carbon content;
---GB/T 4702.15 Determination of metal chromium, lead, tin, bismuth, antimony and arsenic content by plasma mass spectrometry;
---GB/T 4702.16 Determination of metal chromium and sulfur content infrared absorption method and combustion neutralization titration method;
---GB/T 4702.17 Determination of metal chromium oxygen, nitrogen and hydrogen content inert gas melting infrared absorption method and thermal conductivity method;
---GB/T 4702.18 Determination of metal chromium and vanadium content-tantalum reagent chloroform extraction spectrophotometric method.
This part is Part 18 of GB/T 4702.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part was proposed by the China Iron and Steel Association.
This part is under the jurisdiction of the National Pig Iron and Ferroalloy Standardization Technical Committee (SAC/TC318).
Drafting organizations of this section. CITIC Jinzhou Metal Co., Ltd., Qingdao Bozheng Inspection Technology Co., Ltd., Maanshan Iron and Steel Co., Ltd.
Company, Anhui Changjiang Iron and Steel Co., Ltd., Jiangsu Shagang Iron and Steel Research Institute Co., Ltd., Anshan Iron and Steel Co., Ltd., Qingdao Siwen Branch
Measurement Technology Co., Ltd., Metallurgical Industry Information Standard Research Institute.
The main drafters of this section. Wang Liang, Wu Yinjun, Zhang Jijun, Song Zufeng, Chen Rong, Li Yaguang, Zhang Ke, Zhang Jie, Fan Yu, Lu Chunsheng.
Determination of metal chromium and vanadium content
Tantalum Reagent Trichloromethane Extraction Spectrophotometry
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 4702 specifies the tantalum reagent trichloromethane extraction spectrophotometric method for the determination of vanadium content.
This section applies to the determination of vanadium content in metallic chromium, the measurement range (mass fraction). 0.010% ~ 0.500%.
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 4010 Collection and preparation of samples for chemical analysis of ferroalloys
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 7729 General Rules of Spectrophotometry for Chemical Analysis of Metallurgical Products
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
GB/T 12806 Laboratory glassware single mark volumetric flask
GB/T 12808 Single-marked pipette for laboratory glassware
3 Principle
The sample is decomposed with sulfuric acid and perchloric acid. Perchloric acid oxidizes the chromium to hexavalent. The hexavalent chromium and hydrochloric acid form a chromium chloride red-brown smoke which is volatilized.
go with. In hydrochloric acid medium, the purple-red complex formed by pentavalent vanadium and tantalum reagent is extracted by chloroform, and measured at 530nm by spectrophotometer.
The amount of absorbance.
4 Reagents and materials
Unless otherwise specified, only confirmed analytical reagents are used in the analysis, and the water used meets the requirements of GB/T 6682.
Distilled water or water of equivalent purity.
4.1 Sulfuric acid, 1 1.
4.2 Perchloric acid, ρ is about 1.70g/mL.
4.3 Hydrochloric acid, ρ is about 1.19g/mL.
4.4 Hydrochloric acid, 1 1.
4.5 Potassium permanganate, 2.5g/L.
4.6 Tantalum reagent-chloroform solution. 0.2%. Weigh 0.20g of tantalum reagent, dissolve it in 100mL of chloroform solution, mix well, and store in brown
Color bottle.
4.7 Vanadium standard stock solution, 1000μg/mL. Weigh 1.7852g high-purity vanadium pentoxide (purity greater than 99.99%, pre-baked at 110 ℃
1h, and cool to room temperature in a desiccator) In a 250mL beaker, moisten with water, add 30mL hydrochloric acid (4.3), heat to decompose, remove the cold
After reaching room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. This solution 1mL contains 1000μg vanadium.
4.8 Vanadium standard solution, 10μg/mL. Pipette 5.00mL vanadium standard stock solution (4.7) into a 500mL volumetric flask, dilute with water to
Degree, mix well. 1mL of this solution contains 10μg of vanadium.
5 Instruments
5.1 The volumetric flask and pipette used should meet the requirements of GB/T 12806 and GB/T 12808.
5.2 The spectrophotometer should meet the requirements of GB/T 7729.
6 Sampling and sample preparation
Take samples according to GB/T 4010, and the samples should pass through a 1.68mm mesh.
7 Analysis steps
7.1 Number of determinations
The same sample shall be measured independently at least twice.
7.2 Sample
Weigh the sample according to Table 1, accurate to 0.0001g.
7.3 Blank test
Carry out a blank test with the sample.
7.4 Preparation and determination of sample solution
7.4.1 Preparation of sample solution
Place the sample (see 7.2) in a 400mL beaker, add 10mL-20mL water, add 10mL sulfuric acid (4.1), add 20mL perchloric acid
(4.2), decompose the sample by heating until the test solution is orange-yellow, add hydrochloric acid (4.3) slowly and repeatedly until no yellow smoke appears. Continue heating until sulfur
After sour fume, remove it and cool it slightly, add 40mL~50mL water, heat to dissolve the salt, remove it, and cool to room temperature. Transfer to a 100mL volumetric flask,
Dilute to a constant volume and mix well.
7.4.2 Color development and measurement
7.4.2.1 Divide the test solution according to Table 1 into a 125mL separatory funnel, add 1 drop of potassium permanganate (4.5), let stand for 30s, and add 25mL hydrochloric acid
(4.4), add 10mL of tantalum reagent-chloroform solution (4.6), shake immediately for 60s, and let stand for 10min.
7.4.2.2 Use a 1cm cuvette, take the blank test solution (see 7.3) as a reference, and measure the absorbance at 530nm on a spectrophotometer. From
On the calibration curve, find out the quality of the corresponding vanadium.
7.5 Drawing the calibration curve
Pipette six blank test solutions (the same volume as the sample solution), place them in a set of 125mL separatory funnels, add 0mL, 0.50mL,
1.00mL, 2.00mL, 3.50mL, 5.00mL vanadium standard solution (see 4.8), the following steps are carried out according to 7.4.2.
Take the mass of vanadium (μg) as the abscissa and absorbance as the ordinate to draw a calibration curve.
8 Analysis results
The analysis results are rounded off according to GB/T 8170, and two significant digits are retained.
9 tolerance
The difference between the analysis results should not be greater than the allowable difference listed in Table 2.
The difference between the two independent analysis results of the same sample is not greater than the allowable error in the laboratory, and the arithmetic mean is taken as the analysis result. in case
If the difference between the two independent analysis results is greater than the allowable error in the laboratory, follow the flow chart of the test sample analysis value acceptance procedure in Appendix A
To deal with.
10 Test report
The test report should include the following.
a) The name and address of the testing laboratory;
b) Date of release of test report;
c) The number of this part of the standard;
d) The necessary detailed description of the sample itself;
e) Analysis results;
f) The name and result of the standard sample;
g) Any abnormal characteristics in the measurement process and possible analysis results of the sample or standard sample not specified in this section
Any operation that has an impact.
Appendix A
(Normative appendix)
Flowchart of the procedure for receiving the analysis value of the test sample
The flow chart of the procedure for receiving the analysis value of the test sample is shown in Figure A.1.
Figure A.1 Flow chart of the procedure for receiving the analysis value of the test sample
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