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GB/T 223.59-2008 English PDF (GBT223.59-2008)

GB/T 223.59-2008 English PDF (GBT223.59-2008)

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GB/T 223.59-2008: Iron, steel and alloy -- Determination of phosphorus content -- Bismuth phosphomolybdate blue spectrophotometric method and antimony phosphomolybdate blue spectrophotometric method

This Part of GB/T 223 specifies the determination of phosphorus content with bismuth phosphomolybdate blue spectrophotometric method and antimony phosphomolybdate blue spectrophotometric method.
GB/T 223.59-2008
GB
NATIONAL STANDARD OF
THE PEOPLE 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 and Steel Co., Ltd and Central Iron and 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 150??g of titanium, 10 mg of manganese, 2 mg of cobalt, 5 mg of copper, 0.5 mg of vanadium, 10 mg of nickel, 500??g of chromium (III), 50??g of cerium, 5 mg of zirconium, 5??g of niobium and 10??g 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, ?? is about 1.15 g/mL.
3.2.2 Perchloric acid, ?? is about 1.67 g/mL.
3.2.3 Hydrochloric acid, ?? is about 1.19 g/mL.
3.2.4 Nitric acid, ?? is about 1.42 g/mL.
3.2.5 Hydrobromic acid, ?? is about 1.49 g/mL.
3.2.6 Sulfuric acid, ?? 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 ??g/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 ??g of phosphorus per mL.
3.2.15.2 Phosphorus standard solution, 5.0 ??g/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 ??g of phosphorus per mL.
3.3 Instruments
Spectroph...

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