GB/T 223.59-2008 (GB/T223.59-2008, GBT 223.59-2008, GBT223.59-2008) & related versions
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Iron, steel and alloy -- Determination of phosphorus content -- Bismuth phosphomolybdate blue spectrophotometric method and antimony phosphomolybdate blue spectrophotometric method
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GB/T 223.59-2008
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GBT 223.59-2008
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| GB/T 223.59-1987 | English | 199 |
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Methods for chemical analysis of iron, steel and alloy--The reduced molybdoantimonyl phosphoric acid photometric method for the determination of phosphorus content
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GB/T 223.59-1987
| Obsolete |
GBT 223.59-1987
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GB/T 223.59-2008
GB
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.080.01
H 11
Replacing GB/T 223.59-1987
Iron, steel and alloy - Determination of phosphorus content -
Bismuth phosphomolybdate blue spectrophotometric
method and antimony phosphomolybdate blue
spectrophotometric method
ISSUED ON. AUGUST 19, 2008
IMPLEMENTED ON. APRIL 1, 2009
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration Committee.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method I. Bismuth Phosphomolybdate Blue Spectrophotometric Method .. 5
4 Method II. Antimony Phosphomolybdate Blue Spectrophotometric Method10
5 Test report ... 14
Annex A (Informative) Source data of common precision test ... 16
Foreword
This Part of GB/T 223 replaces "Methods for Chemical Analysis of Iron, Steel
and Alloy-The Reduced Molybdoantimonyl Phosphoric Acid Photometric
Method for the Determination of Phosphorus Content" (GB/T 223.59-1987).
In this revision, this Part has been renamed as "Iron, Steel and
Alloy-Determination of Phosphorus Content-Bismuth Phosphomolybdate
Blue Spectrophotometric Method and Antimony Phosphomolybdate Blue
Spectrophotometric Method"; it includes two analysis methods. bismuth
phosphomolybdate blue spectrophotometric method (Method I) and antimony
phosphomolybdate blue spectrophotometric method ((Method II)).
Method I is a new method.
While compared with GB/T 223.59-1987, Method II in this Part mainly has the
following revisions in terms of technical contents.
- added the description content for reagents and water in the analysis,
and revised the expression method for solution concentration;
- revised the expression for weighing specimen quantity;
- revised the expression of quantity in result calculation formulae and
quantity units in formulae;
- specified the explanation for precision function formula.
Appendix A of this Part is informative.
This Part was proposed by China Iron and Steel Association.
This Part shall be under the jurisdiction of National Technical Committee on
Iron and Steel of Standardization Administration of China.
The drafting organizations of this Part. Maanshan Iron & Steel Co., Ltd and
Central Iron & Steel Research Institute.
Main drafters of this Part. Cheng Jianping, Long Rucheng, Cui Qiuhong, Xu
Fenlan and Hua Jing.
Versions of standard substituted by this Standard are.
- Method IV in GB/T 223.3-1981;
- GB/T 223.59-1987.
Iron, steel and alloy - Determination of phosphorus content -
Bismuth phosphomolybdate blue spectrophotometric
method and antimony phosphomolybdate blue
spectrophotometric method
WARNING. The personnel using this Part shall have practical
experiences in regular laboratory work. This Part does not point out all
the possible safety problems. Users have the responsibility to take
appropriate safety and health measures, and ensure meeting the
conditions specified in relevant regulations of the State.
1 Scope
This Part of GB/T 223 specifies the determination of phosphorus content with
bismuth phosphomolybdate blue spectrophotometric method and antimony
phosphomolybdate blue spectrophotometric method.
This Part is applicable to the determination of phosphorus content in pig iron,
cast iron, iron powder, carbon steel, low alloy steel and alloy steel and is not
applicable to niobium and wolfram steel. The determination scope of Method I
is 0.005% ~0.300% mass fraction while the determination scope of Method II
is 0.01% ~0.06% mass fraction.
2 Normative references
The following standards contain provisions which, through reference in this
text, constitute provisions of this Part of GB/T 223. For dated reference,
subsequent amendments to (excluding correction to), or revisions of, any of
these publications do not apply. However, the parties whose enter into
agreement according to this Part are encouraged to research whether the
latest editions of these documents are applied or not. For undated references,
the latest edition of the normative document is applicable to this Part.
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)
3 Method I. Bismuth Phosphomolybdate Blue
Spectrophotometric Method
3.1 Principle
After the sample is subject to acid dissolution, perchloric acid smoke is given
out so that all phosphorus is oxidized into orthophosphoric acid and the
carbide is damaged. In sulfuric acid medium, the phosphorus, bismuth and
ammonium molybdate form yellow complex compound; ascorbic acid is used
to reduce bismuth phosphomolybdate yellow into bismuth phosphomolybdate
blue. The absorbance shall be measured at 700nm wave length on
spectrophotometer; the mass fraction of phosphorus shall be calculated out.
If there are 150μg of titanium, 10 mg of manganese, 2 mg of cobalt, 5 mg of
copper, 0.5 mg of vanadium, 10 mg of nickel, 500μg of chromium (III), 50μg of
cerium, 5 mg of zirconium, 5μg of niobium and 10μg of wolfram in color
reagent, the determination will not be affected. Arsenium has severe
interference on the determination and may be removed with hydrobromic acid
where treating samples.
3.2 Reagents and materials
Unless otherwise specified, it can only use approved analytical reagent and
distilled water or water with equivalent purity during the analysis.
3.2.1 Hydrofluoric acid, ρ is about 1.15 g/mL.
3.2.2 Perchloric acid, ρ is about 1.67 g/mL.
3.2.3 Hydrochloric acid, ρ is about 1.19 g/mL.
3.2.4 Nitric acid, ρ is about 1.42 g/mL.
3.2.5 Hydrobromic acid, ρ is about 1.49 g/mL.
3.2.6 Sulfuric acid, ρ is about 1.84 g/mL.
3.2.7 Sulfuric acid, 1+1. Slowly add sulfuric acid (3.2.6) into water while
stirring and diluting into 1+1.
3.2.8 Acid mixture of hydrochloric acid and nitric acid, 2+1. Mix two shares
of hydrochloric acid (3.2.3) and one share of nitric acid (3.2.4) uniformly.
3.2.9 Acid mixture of hydrobromic acid and hydrochloric acid, 1+2. Mix one
share of hydrobromic acid (3.2.5) and two shares of hydrochloric acid (3.2.3)
uniformly.
3.2.10 Ascorbic acid solution, 20 g/L. Weigh 2 g of ascorbic acid, place it
into 100 mL beaker and add 50 mL of water to dissolve and dilute it until 100
mL, then mix uniformly. This solution shall be prepared immediately before
use.
3.2.11 Ammonium molybdate solution, 30 g/L. Weigh 3 g of ammonium
molybdate [(NH4)6Mo7O24·4H2O] dissolve it in water, dilute until 100 mL and
mix uniformly.
3.2.12 Sodium nitrite solution, 100 g/L. Weigh 10g of sodium nitrite, dissolve
in water, dilute until 100 mL and mix uniformly.
3.2.13 Bismuth nitrate solution, 10 g/L. Weigh 10 g of bismuth nitrate
[Bi(NO3)3·5H2O], Place it into 200 mL beaker, add 25 mL of nitric acid (3.2.4) ,
dissolve it in water, boil to remove nitrogen oxide, cool until room temperature,
transfer it into 1000 mL volumetric flask, dilute it with water to the scale and
mix uniformly.
3.2.14 Iron solution
3.2.14.1 Iron solution A, 5 mg/mL. Weigh 0.5000 g of pure iron (with mass
fraction of phosphorus less than 0.0005%), dissolve it with 10 mL of
hydrochloric acid (3.2.3) before dropwise adding nitric acid (3.2.4) for
oxidation, add 3 mL of perchloric acid (3.2.2) for evaporating until giving out
perchloric acid smoke and continue evaporating till taking on wet salt state,
cool it with 20 mL of sulfuric acid (3.2.7) dissolution salt until room
temperature, transfer into 100 mL volumetric flask, dilute it with water to the
scale and mix uniformly. This solution contains 5 mg of iron per mL.
3.2.14.2 Iron solution B, 1 mg/mL. Weigh 0.1000 g of pure iron (with mass
fraction of phosphorus less than 0.001%), dissolve it with 10 mL of
hydrochloric acid (3.2.3) before dropwise adding nitric acid (3.2.4) for
oxidation, add 3 mL of perchloric acid (3.2.2) for evaporating until giving out
perchloric acid smoke and continue evaporating till taking on wet salt state,
cool it with 20 mL of sulfuric acid (3.2.7) dissolution salt until room
temperature, transfer into 100 mL volumetric flask, dilute it with water to the
scale and mix uniformly. This solution contains 1 mg of iron per mL.
3.2.15 Phosphorus standard solution
3.2.15.1 Phosphorus stock solution, 100 μg/mL. Weigh 0.4393 g of
reference potassium dihydrogen phosphate (KH2PO4) dried in advance at
105°C till constant quantity, dissolve it with right amount of water, add 5 mL of
sulfuric acid (3.2.7), transfer into 1000 mL volumetric flask, dilute it with water
to the scale and mix uniformly. This solution contains 100 μg of phosphorus
per mL.
3.2.15.2 Phosphorus standard solution, 5.0 μg/mL. Take 50.00 mL of
phosphorus stock solution (3.2.15.1), place it into 1000 mL volumetric flask,
dilute it with water to the scale and mix uniformly. This solution contains 5.0
μg of phosphorus per mL.
3.3 Instruments
Spectroph...
......
| Standard ID | GB/T 223.59-2008 (GB/T223.59-2008) | | Description (Translated English) | Iron, steel and alloy - Determination of phosphorus content - Bismuth phosphomolybdate blue spectrophotometric method and antimony phosphomolybdate blue spectrophotometric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.080.01 | | Word Count Estimation | 11,141 | | Date of Issue | 2008-08-19 | | Date of Implementation | 2009-04-01 | | Older Standard (superseded by this standard) | GB/T 223.59-1987 | | Quoted Standard | GB/T 6379.1; GB/T 6379.2; GB/T 20066 | | Drafting Organization | Maanshan Iron & Steel Co., Ltd. | | Administrative Organization | National Steel Standardization Technical Committee | | Regulation (derived from) | National Standard Approval Announcement 2008 No.14 (Total No.127) | | Proposing organization | China Iron and Steel Association | | Issuing agency(ies) | Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China; Standardization Administration of China | | Summary | This standard specifies the use of phosphorus molybdenum blue spectrophotometry bismuth and antimony phosphorus molybdenum blue spectrophotometric determination of phosphorus content. This section applies to pig iron, determination of phosphorus content in alloy steel, iron, iron, carbon steel, low alloy steel. Does not apply to niobium, tungsten steel. A method for the determination of the mass fraction of the range from 0. 005% to 0. 300%, two methods of measuring the mass fraction range of 0. 01% -0. 06 %. | | Standard ID | GB/T 223.59-1987 (GB/T223.59-1987) | | Description (Translated English) | Methods for chemical analysis of iron, steel and alloy--The reduced molybdoantimonyl phosphoric acid photometric method for the determination of phosphorus content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.080 | | Word Count Estimation | 5,558 | | Date of Issue | 1987/5/12 | | Date of Implementation | 1988/3/1 | | Older Standard (superseded by this standard) | GB 223.3-1981 | | Regulation (derived from) | Announcement of Newly Approved National Standards 2008 No. 14 (No. 127 overall) | | Issuing agency(ies) | Ministry of Metallurgical Industry |
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