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GB/T 223.14-2000 PDF in English


GB/T 223.14-2000 (GB/T223.14-2000, GBT 223.14-2000, GBT223.14-2000)
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GB/T 223.14-2000: PDF in English (GBT 223.14-2000)

GB/T 223.14-2000
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 11
Replacing GB/T 223.14-1989
Methods for Chemical Analysis of Iron, Steel and Alloy -
The N-benzoy-N-phenylhydroxylamine Extraction Photometric
Method for the Determination of Vanadium Content
ISSUED ON. APRIL 11, 2000
IMPLEMENTED ON. NOVEMBER 1, 2000
Issued by. Quality and Technology Supervision Bureau of the People’s
Republic of China
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 References ... 4 
3 Method Summary ... 4 
4 Reagents and Materials ... 5 
5 Instruments and Equipment ... 6 
6 Sampling and Sample Preparation ... 6 
7 Analytical Procedures ... 6 
8 Analytical Result and Expression ... 8 
9 Precision ... 8 
10 Test Report ... 9 
Foreword
This Standard is a revised edition of GB/T 223.14-1989 Methods for Chemical Analysis
of Iron, Steel and Alloy - The N-benzoy-N-phenylhydroxylamine Extraction Photometric
Method for the Determination of Vanadium Content.
In this revised edition, the following chapters and content are added to this Standard.
“Foreword”, “2 References”, “5 Instruments and Equipment”, “6 Sampling and Sample
Preparation” and “10 Test Report”. Furthermore, the following provisions are modified.
---The previous 1 is modified into 1 (the title and content of the chapter are
modified);
---The previous 2 is modified into 3 (extraction acidity is modified);
---The previous 3 is modified into 4 (the title of the chapter is modified; explanatory
content is added);
---The previous 4.1 is modified into 7.1 (the expression of sample weighing-taking
is modified);
---The previous 5 is modified into 8 (the result calculation formula and the
description of formula content are modified).
GB/T 223 is under the general title of Methods for Chemical Analysis of Iron, Steel and
Alloy. It includes several independent parts. This Standard is Part 14.
Since the date of implementation, this Standard shall be served as a replacement of
GB 223.14-1989 Methods for Chemical Analysis of Iron, Steel and Alloy - The N-
benzoy-N-phenylhydroxylamine Extraction Photometric Method for the Determination
of Vanadium Content.
This Standard was proposed by the State Bureau of Metallurgical Industry.
This Standard shall be under the jurisdiction of National Technical Committee on Steel
of Standardization Administration of China.
The responsible drafting organization of this standard. Beijing Central Iron & Steel
Research Institute.
The participating drafting organization of this standard. Beiman Special Steel Co., Ltd.
The main drafters of this Standard. Tianling, Jiang Chunhui, Cui Qiuhong, Fujie.
This Standard was initially issued in 1982. The first revised edition of this Standard
was issued in March 1989.
Methods for Chemical Analysis of Iron, Steel and Alloy
The N-benzoy-N-phenylhydroxylamine Extraction Photometric
Method for the Determination of Vanadium Content
1 Scope
This Standard specifies the N-benzoy-N-phenylhydroxylamine extraction photometric
method for the determination of vanadium content.
This Standard is applicable to the determination of vanadium content in iron, steel and
alloy under the range of 0.0050% (m/m) ~ 0.50% (m/m).
2 References
Provisions that are included in the following standards constitute the provisions of this
Standard through the reference in this Standard. When this Standard was published,
all the announced versions were valid. All the standards will be revised. Parties that
adopt this Standard shall discuss the possibility of adopting the latest versions of the
following standards.
GB/T 222-1984 Method of Sampling Steel for Determination of Chemical
Composition and Permissible Variations for Product Analysis
GB/T 6379-1986 Precision of Test Methods Determination of Repeatability and
Reproducibility for a Standard Test Method by Interlaboratory Tests
3 Method Summary
After dissolving test piece with acid, in the medium of sulfuric acid-phosphoric acid,
use potassium permanganate to oxidize vanadium and pentavalent at room
temperature. Add tantalum reagent-trichloromethane solution; extract the complex of
vanadium into trichloromethane. Then, measure the absorbance at the wavelength of
530 nm.
Interference determination of color developing solution that contains over 1 mg of
molybdenum and titanium. when hydrochloric acid concentration in the extract rises to
6 mol/L, the permissible amount of molybdenum can be raised to 2.5 mg. Use sulfuric
acid-hydrogen peroxide solution to rinse the organic phase, then, the permissible
amount of titanium can be increased to 5 mg.
8 mL of sulfuric acid (4.5) and 8 mL of phosphoric acid (4.7); continue to heat it up,
evaporate it, till it emits smoke. At this moment, if there is carbide that is not damaged,
add drops of nitric acid (4.4), then, re-evaporate it, till it emits smoke. Repeat this step
till carbide is completely damaged. Wait till it is slightly cooled down, then, add 50 mL
of water; heat it up to dissolve salt, then, cool it down to room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the constant volume, then, mix it
up. When there is precipitation, start dry filtration.
7.3.2 Oxidization of vanadium
7.3.2.1 Transfer-take 10.00 mL of test solution (7.3.1), place it in a 60 mL separating
funnel. Add 1 mL of copper solution (4.8); shake it while adding drops of potassium
permanganate solution (4.9), till it manifests steady red; maintain for 2 ~ 3 min.
7.3.2.2 Add 2 mL of uric acid solution (4.10); shake it continuously while adding drops
of sodium nitrite solution (4.11) [in terms of sample that contains over 1 mg of chromium,
add 5 drops of sodium arsenite solution (4.12) to restore surplus potassium
permanganate before adding drops of sodium nitrite solution, till the pink color
completely vanishes].
7.3.3 Color development, extraction
7.3.3.1 General sample
Add 10.00 mL of tantalum reagent-trichloromethane solution (4.13), then, add 15 mL
of hydrochloric acid (4.3); immediately start oscillation for 1 min; place it evenly for
stratification.
7.3.3.2 Molybdenum-containing sample
When the transferred test solution contains 1 ~ 5 mg of molybdenum, add 10.00 mL of
tantalum reagent-trichloromethane solution (4.13), then, add 10 mL of hydrochloric
acid (4.2). Immediately start oscillation for 1 min; place it statically for stratification.
7.3.3.3 Titanium-containing sample
When the transferred test solution contains 1 ~ 5 mg of titanium, add 10.00 mL of
tantalum reagent-trichloromethane solution (4.13), then, add 15 mL of hydrochloric
acid (4.3). Immediately start oscillation for 1 min; place it statically for stratification.
Then, transfer organic phase into another 60 mL separating funnel. Add 10 mL of
sulfuric acid-hydrogen peroxide lotion (4.14); start rinsing and oscillation for 30 s; place
it statically for stratification.
7.3.4 Measurement of absorbance
7.3.4.1 Use filter paper or absorbent cotton to dry-filter the lower layer of organic phase
solution (7.3.3) in a 1 cm (or an appropriate size) absorption vessel. Take
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.