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GB/T 4702.18-2020Chromiun metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophtometry method (English PDF)

金属铬 钒含量的测定 钽试剂三氯甲烷萃取分光光度法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

March 6, 2020

Implementation date

July 1, 2020

Scope

GB/T 4702.18-2020 is the English-translated version of 金属铬 钒含量的测定 钽试剂三氯甲烷萃取分光光度法.

GB/T 4702.18-2020 is the Chinese standard "Chromiun metal - Determination of vanadium content - Tantalum reagent trichloromethane extraction spectrophtometry method".

Its scope clause reads: 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%. Its clauses include principle; reagents and materials; instruments; sampling and sample preparation; analysis steps; analysis results; tolerance; test report.

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Document preview — GB/T 4702.18-2020

National Standard of the People's Republic of China

ICS
77.100
Classification
H 11

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • 1 Scope
  • 2 Normative references
  • 3 Principle
  • 4 Reagents and materials
  • 5 Instruments
  • 6 Sampling and sample preparation
  • 7 Analysis steps
  • 8 Analysis results
  • 9 tolerance
  • 10 Test report

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, rho is about 1.70g/mL.

4.3

Hydrochloric acid, rho 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 °C

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 […]

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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