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Iron, steel and alloy -- Determination of sulfur content -- Gravimetric method
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| GB/T 223.72-1991 | English | 199 |
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Methods for chemical analysis of iron, steel and alloy--The alumina chromatographic separation-barium sulfate gravimetric method for the deteremination of sulphur content
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Basic data
| Standard ID | GB/T 223.72-2008 (GB/T223.72-2008) |
| Description (Translated English) | Iron, steel and alloy -- Determination of sulfur content -- Gravimetric method |
| Sector / Industry | National Standard (Recommended) |
| Classification of Chinese Standard | H11 |
| Classification of International Standard | 77.080.01 |
| Word Count Estimation | 14,180 |
| Date of Issue | 2008-05-13 |
| Date of Implementation | 2008-11-01 |
| Older Standard (superseded by this standard) | GB/T 223.72-1991 |
| Quoted Standard | GB/T 6379.1; GB/T 6379.2; GB/T 20066; ISO 565; ISO 3696; ISO 5725-3 |
| Regulation (derived from) | National Standard Approval Announcement 2008 No.8 (Total No.121) |
| Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China |
| Summary | This standard specifies the determination of sulfur in steel by gravimetric method. This method is particularly suitable as a standard reference sample value method used. This section applies to a method for the determination of the mass fraction of 0. 003% to 0. 35 % sulfur content, This section applies to the second method for the determination of the mass fraction of 0. 003% to 0. 20 % sulfur content. |
GB/T 223.72-2008: Iron, steel and alloy -- Determination of sulfur content -- Gravimetric method
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H 11
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
Replacing GB/T 223.72-1991
Iron, Steel and Alloy - Determination of
Sulfur Content - Gravimetric Method
Issued on: MAY 13, 2008
Implemented on: NOVEMBER 1, 2008
Jointly issued by. General Administration of Quality Supervision, Inspection
and Quarantine (GAQSIQ);
Standardization Administration (SAC) of the People’s
Republic of China.
GB
3. No action is required - Full-copy of this standard will be automatically &
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Foreword
In this revision, this part of GB/T 223 is changed to "Iron steel and alloy - Determination of
sulfur content - Gravimetric method" and has two analysis methods.
——Method 1. gravimetric method;
——Method 2. aluminum oxide chromatographic separation - barium sulfate gravimetric
method.
Method 1 in this Part is identical to ISO 4934. 2003(E).
To be convenient for use, the following editing revisions are made in this part.
——"This international standard" is changed into "this Part";
——The comma "," acting as decimal point was replaced by the decimal point ".";
——The foreword of the international standard is canceled;
——In "normative reference", the international documents or specific chapter/article are
consistent with domestic documents and replaced with the domestic documents.
This part replaces GB/T 333.72-1991 "Methods for chemical analysis of iron, steel and
alloy - The alumina chromatographic separation - barium sulfate gravimetric method for the
determination of sulphur content".
Compared with GB/T 223.72-1991. method 1 of this Part has the following revisions.
——In sample dissolution, the conical flask containing test portion and agent is connected
with a condenser, to control the dissolving speed of the sample better and avoid the sample
dissolving too fast; a small amount of sulfur is oxidized to generate sulfate radical and escapes
by the way of hydrogen sulfide.
——For precipitant adding, firstly add an approximate ammount of BaCl2 required
depositing all -24SO , stand for 1h, and add about 25 mg of BaCl2; control the S content in the
test portion within 1.5~5.5 mg and exceed precipitant BaCl2 about (0.7~3) times; but in GB/T
223.72-1991. add 500 mg of BaCl2 at a time and exceed precipitant BaCl2 about (15 ~ 30)
times.
Compared with GB/T 223.72-1991. method 2 of this Part has the following revisions.
——The description content for reagents and water in the analysis is added, and the
expression method for solution concentration is revised;
——The expression of quantity in result calculation formulae and quantity units in
formulae is revised;
——The explanation for precision function formula is specified.
Appendix A and Appendix B of this part are informative.
This Part was proposed by China Iron and Steel Association.
This Part is under the jurisdiction of the National Technical Committee on Iron and Steel of
Standardization Administration of China.
Chief Drafting Organization. China Iron & Steel Research Institute Group
Chief drafting staffs. Fan Xiaoyun, Ke Ruihua, Fan Chunqi
All previously replaced editions hereof are as.
——GB/T 223.72-1981. GB/T 223.73-1991.
Table of Contents
1 Scope ... 1
2 Normative References ... 1
3 Method 1. Gravimetric method ... 2
4 Method 2. Aluminum Oxide Chromatographic Separation - Barium Sulfate Gravimetric
Method ... 9
5 Test Report ... 14
Annex A (Informative) Additional Information on International Cooperative Tests ... 15
Annex B (Informative) Graphical Representation of Precision Data... 16
Iron Steel and Alloy -
Determination of Sulfur Content - Gravimetric Method
Warning. Staffs using this part shall have normal practical experience in the laboratory.
Potential safety problems are not indicated totally in this part, therefore the staffs using this part
are responsible for taking safe and health measures properly, as well as ensuring to conform the
defined terms in national relevant regulations.
1 Scope
This part of GB/T 223 specifies a gravimetric method for the determination of the sulfur
content in steels and iron, excluding steels containing selenium. The method is particularly
suitable as a reference method for the standardization of samples on which certified standard
values are to be established.
Method 1 is applicable to a sulfur content between 0.003 % (mass fraction) and 0.35 %
(mass fraction). Method 2 is applicable to a sulfur content between 0.003 % (mass fraction) and
0.20 % (mass fraction).
2 Normative References
The following referenced documents are indispensable for the application of this document.
For dated references, only the edition cited applies. For undated references, the latest edition of
the referenced document (including any amendments) applies.
GB/T 6379.1 Accuracy (Trueness and Precision) of Measurement Methods and Results-Part 1.
General Principles and Definitions(GB/T 6379.1-2004, ISO 5725-1. 1994, IDT)
GB/T 6379.2 Accuracy (Trueness and Precision) of Measurement Methods and Results - Part
2. Basic Method for the Determination of Repeatability and Reproducibility of a
Standard Measurement Method (GB/T 6379.2-2004, ISO 5725-2. 1994, IDT)
GB/T 20066 Steel and Iron - Sampling and Preparation of Samples for the Determination of
Chemical Composition (GB/T 20066-2006, ISO 14284. 1996, IDT)
ISO 565 Test sieves - Metal wire cloth, perforated metal plate and electroformed sheet -
Nominal sizes of openings
ISO 3696 Water for analytical laboratory use - Specification and test methods
ISO 5725-3 Accuracy (trueness and precision) of measurement methods and results - Part 3.
Intermediate measures of the precision of a standard measurement method
3 Method 1. Gravimetric Method
3.1 Principle
Dissolution of a test portion in dilute nitric acid in the presence of bromine, or in the mixed
acid of nitric acid and hydrochloric acid in the presence of bromine (with the aid of an
appropriate device to prevent sulfur losses). Addition of perchloric acid and evaporation of the
solution until white fumes of perchloric acid are evolved. Filtration of the solution and removal
of the dehydrates of silicon, tungsten, niobium, etc. Addition of a determined quantity of sulfate
ions to aid precipitation. Chromatographic separation of the sulfate ions from the test solution
by adsorption on an alumina column, and elution using an ammonium hydroxide solution.
Precipitation of the sulfate ions as barium sulfate under controlled conditions and filtering,
washing, heating and weighing.
3.2 Reagents and material
During the analysis, use only reagents of recognized analytical grade and only grade 2
water as specified in ISO 3696.
3.2.1 Aluminium oxide (alumina, Al2O3), prepared for chromatography, of particle size
corresponding to a sieve mesh size of 75 (im to 150 (im (supplementary series R 40/3 of ISO
565)
Alumina designated alkaline, neutral or acid may be used.
Place approximately 200 g of the dry alumina in a 400 ml beaker containing 300 ml of
water and place the beaker in a sink. Insert a glass tube having a bore of 5 mm, such that it
extends to the bottom of the beaker and connect the tube to a water supply. Adjust the water
flow so that the suspended fine material overflows the rim of the beaker. Continue this treatment
until all the fine material, which does not settle within 1 min of stopping the water flow, is
removed.
Pour off the supernatant liquid from the coarser material, add the hydrochloric acid (3.2.5)
in an amount sufficient to cover the alumina; stir and allow to stand for not less than 12 h. Pour
off the hydrochloric acid and wash the alumina with water as described in the second paragraph.
For preparation of the column, make a slurry of the washed alumina and the hydrochloric
acid solution (3.2.8).
3.2.2 Bromine (Br2), min 99 % (mass fraction)
3.2.3 Nitric acid (HNO3), ρ = approximately 1.40 g/ml
3.2.4 Nitric acid (HNO3), ρ = approximately 1.40 g/ml, diluted 1 + 1
3.2.5 Hydrochloric acid (HCl), ρ = approximately 1.19 g/ml
3.2.6 Hydrochloric acid (HCl), ρ = approximately 1.19 g/ml, diluted 1 + 1
3.2.7 Hydrochloric acid (HCl), ρ = approximately 1.19 g/ml, diluted 1 + 9
3.2.8 Hydrochloric acid (HCl), ρ = approximately 1.19 g/ml, diluted 1 + 19
3.2.9 Perchloric acid (HClO4), ρ = approximately 1.54 g/ml
Note. If this reagent is shown to have a high sulfate content, this may be removed by passing the
reagent through the adsorption column (3.3.4).
3.2.10 Perchloric acid (HClO4), ρ = approximately 1.54 g/ml, diluted 1 + 49
3.2.11 Acid mixture
Mix hydrochloric acid (4.5) and nitric acid (4.3) in proportions liable to ensure total
solubility of the samples. This mixture should be freshly prepared as required.
Note. Generally, aqua regia can be used. For some samples, the proportion of hydrochloric
acid and nitric acid can be adjusted.
3.2.12 Ammonium hydroxide (NH4OH), ρ = approximately 0.90 g/ml
3.2.13 Ammonium hydroxide (NH4OH), ρ = approximately 0.90 g/ml, dilut...
...