GB/T 5686.4-2022 PDF English
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Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal - Determination of phosphorus content - Molybdenum blue spectrophotometric method and bismuth phosphomolybdate blue spectrophotometric method
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| GB/T 5686.4-2008 | English | 125 |
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Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal -- Determination of phosphorus content -- Molybdenum blue photometric method and alkali content titrimetric method
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| GB/T 5686.4-1998 | English | 239 |
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Methods for chemical analysis of silicomanganese --The phosphomolybdenum blue phtometric method for the determination of phosphorus content
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| GB/T 5686.4-1985 | English | RFQ |
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Methods for chemical analysis of silicomanganese alloy--The molybdenum blue photometric method for the determination of phosphorus content
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GB/T 5686.4-2022: Ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal - Determination of phosphorus content - Molybdenum blue spectrophotometric method and bismuth phosphomolybdate blue spectrophotometric method
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
CCS H 11
Replacing GB/T 5686.4-2008
Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing
Ferromanganese and Manganese Metal - Determination of
Phosphorus Content - Molybdenum Blue Spectrophotometric
Method and Bismuth Phosphomolybdate Blue Spectrophotometric
Method
Issued on. OCTOBER 12, 2022
Implemented on. FEBRUARY 1, 2023
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
Introduction... 5
1 Scope... 7
2 Normative References... 7
3 Terms and Definitions... 8
4 Method 1.Molybdenum Blue Spectrophotometric Method... 8
5 Method 2.Bismuth Phosphomolybdate Blue Spectrophotometric Method... 13
6 Test Report... 20
Appendix A (normative) Flow Chart of Specimen Analysis Result Acceptance
Procedure... 21
Foreword
This document was drafted in accordance with the rules provided in GB/T 1.1-2020 Directives
for Standardization - Part 1.Rules for the Structure and Drafting of Standardizing Documents.
This is Part 4 of GB/T 5686.GB/T 5686 has issued the following parts.
---Part 1.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Manganese Content - Potentiometric Method,
Titrimetric Method after Ammonium Nitrate Oxidation and Titrimetric Method after
Perchloric Acid Oxidation;
---Part 2.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Silicon Content - Molybdenum Blue
Spectrophotometric Method, Silicon Potassium Fluoride Titrimetric Method and
Perchloric Acid Dehydration Gravimetric Method;
---Part 4.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Phosphorus Content - Molybdenum Blue
Spectrophotometric Method and Bismuth Phosphomolybdate Blue Spectrophotometric
Method;
---Part 5.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Carbon Content - The Infrared Absorption
Method, the Gasometric Method, the Gravimetric and the Coulometric Method;
---Part 7.Ferromanganese, Ferromanganese-silicon, Nitrogen-bearing Ferromanganese
and Manganese Metal - Determination of Sulfur Content - Infrared Absorption Method
and Combustion-neutralization Method.
This document serves as a replacement for GB/T 5686.4-2008 Ferromanganese,
Ferromanganese-silicon, Nitrogen-bearing Ferromanganese and Manganese Metal -
Determination of Phosphorus Content - Molybdenum Blue Photometric Method and Alkali
Content Titrimetric Method. In comparison with GB/T 5686.4-2008, apart from structural
adjustments and editorial modifications, the main technical changes are as follows.
a) The scope of application is modified (see Chapter 1; Chapter 1 of Version 2008);
b) The operation of arsenic volatilization by molybdenum blue spectrophotometric
method is modified (see 4.5.4.1.2.3; 3.5.3.1.2.3 of Version 2008);
c) The original Method 2 is deleted. alkali content titrimetric method (see Chapter 4 of
Version 2008);
d) Method 2 is added. bismuth phosphomolybdate blue spectrophotometric method (see
Chapter 5).
Please be noted that certain content of this document may involve patents. The institution
issuing this document does not undertake the responsibility of identifying these patents.
This document was proposed by China Iron and Steel Association.
This document shall be under the jurisdiction of National Technical Committee 318 on Pig Irons
and Ferroalloys of Standardization Administration of China (SAC/TC 318).
The drafting organizations of this document. Sichuan CHUANTOU EMEI Ferroalloy (Group)
Co., Ltd.; Xiangxi Autonomous Prefecture Fengda Alloy Technology Co., Ltd.; Anhui Chang
Jiang Iron & Steel Co., Ltd.; Jitie Ferroalloy Co., Ltd.; Hebei Jinxi International Trade Co., Ltd.;
CITIC Jinzhou Metal Co., Ltd.; China Metallurgical Information and Standardization Institute.
The main drafters of this document. Fang Yan, Liu Huili, Tang Huaying, Wang Guoning, Chen
Rong, Yang Jiadong, Li Jinglin, Lv Xuemei, Liu Bing, Wang Min, Ye Xiaoshuang, Wu Yinjun,
Lu Chunsheng, Zhang Chen.
The issuing of the previous versions.
---Firstly issued in 1985 as GB/T 5686.4-1985;
---During the first revision in 1998, the content of GB 5686.3-1988 Methods for Chemical
Analysis of Silicomanganese Alloy - The Neutralization Titration Method for the
Determination of Phosphorus Content was incorporated;
---During the second revision in 2008, the contents of GB/T 7730.3-1997 Methods for
Chemical Analysis of Ferromanganese - The Determination of Phosphorus Content and
GB/T 8654.5-1988 Methods for Chemical Analysis of Manganese Metal - The
Molybdenum Blue Photometric Method for the Determination of Phosphorus Content
were incorporated (the previous versions of GB/T 7730.3-1997 are as follows. GB/T
7730.3-1987 Methods for Chemical Analysis of Ferromanganese and Blast Furnace
Ferromanganese - The Alkalimetric Method for the Determination of Phosphorus
Content and GB/T 7730.4-1987 Methods for Chemical Analysis of Ferromanganese
and Blast Furnace Ferromanganese - The Reduced Molybdophosphoric Acid
Spectrophotometric Method for the Determination of Phosphorus Content);
---This is the third revision.
1 Scope
This document describes the determination of phosphorus content in ferromanganese,
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal, using
molybdenum blue spectrophotometric method and bismuth phosphomolybdate blue
spectrophotometric method.
This document is applicable to the determination of phosphorus content in ferromanganese,
ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese metal. The
determination range (mass fraction) is 0.0030% ~ 0.650%. Method 1.molybdenum blue
spectrophotometric method, which is applicable to the determination of phosphorus content in
ferromanganese, ferromanganese-silicon, nitrogen-bearing ferromanganese and manganese
metal, with a determination range (mass fraction) of 0.0030% ~ 0.450%; Method 2.bismuth
phosphomolybdate blue spectrophotometric method, which is applicable to the determination
of phosphorus content in ferromanganese, ferromanganese-silicon, nitrogen-bearing
ferromanganese and manganese metal, with a determination range (mass fraction) of 0.0030%
~ 0.650%.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 4010 Ferroalloys Sampling and Preparation of Samples for Chemical Analysis
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 12806 Laboratory Glassware - One-mark Volumetric Flasks
GB/T 12807 Laboratory Glassware - Graduated Pipettes
GB/T 12808 Laboratory Glassware - One Mark Pipettes
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Method 1.Molybdenum Blue Spectrophotometric Method
4.1 Principle
The test portion is decomposed by nitric acid and hydrofluoric acid. Add perchloric acid to
evaporate it, until emitting smoke, thereby oxidizing phosphorus into orthophosphoric acid.
Add sodium bisulfite to reduce iron, etc., add ammonium molybdate and hydrazine sulfate to
generate phosphomolybdenum blue. At a wavelength of 825 nm, use a spectrophotometer to
measure its absorbance, and calculate the mass fraction of phosphorus.
4.2.8 Hydrazine sulfate solution, 1.5 g/L.
4.2.9 Color development solution. When in use, transfer-take 25 mL of ammonium molybdate
solution (see 4.2.7) and 10 mL of hydrazine sulfate solution (see 4.2.8), add 65 mL of water and
mix it well.
4.3 Instruments
In the analysis, only common laboratory instruments are used. The one-mark volumetric flasks,
graduated pipettes and one-mark pipettes used shall comply with the requirements of GB/T
12806, GB/T 12807 and GB/T 12808, respectively.
4.4 Sampling and Sample Preparation
In accordance with the provisions of GB/T 4010, conduct sampling and sample preparation.
The specimens shall all pass the 0.125 mm sieve mesh.
4.5 Analytical Steps
4.5.1 Number of determinations
For the same specimen, conduct at least 2 independent determinations.
4.5.2 Amount of test portion
4.5.3 Blank test
Along with the test portion, carry out a blank test.
4.5.4 Determination
4.5.4.1 Decomposition of test portion
4.5.4.2 Color development and determination
4.5.4.2.1 Slightly cool, remove the watch glass, add about 30 mL of warm water, heat and boil
to dissolve the soluble salts. Remove it, dropwise add sodium bisulfite solution (see 4.2.6) to
decompose manganese dioxide, etc. Use a medium-speed filter paper to filter it into a 250 mL
volumetric flask. Use warm water to wash it, until there is no acidity, cool to room temperature,
use water to dilute to the scale and mix it well.
4.5.5 Drawing of calibration curve
4.5.5.1 Drawing of calibration curve of manganese metal with low phosphorus content
(mass fraction 0.0030% ~ 0.020%)
4.5.5.1.1 Transfer-take 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL and 12.00 mL
of phosphorus standard solution (see 4.2.11) and place them into a set of 100 mL beakers.
Respectively add 5 mL of perchloric acid (see 4.2.5), heat and evaporate them, until emitting
perchloric acid smoke. Remove them and follow 4.5.4.2 for the subsequent operations.
4.5.5.3 Drawing of calibration curve of ferromanganese, ferromanganese-silicon,
nitrogen-bearing ferromanganese
4.5.5.3.1 Transfer-take 0 mL, 1.00 mL, 3.00 mL, 5.00 mL, 7.00 mL and 9.00 mL of phosphorus
standard solution (see 4.2.10) and place them into a set of 100 mL beakers. Respectively add 5
mL of perchloric acid (see 4.2.5), heat and evaporate them, until emitting perchloric acid smoke.
Remove them and follow 4.5.4.2 for the subsequent operations.
4.6 Calculation of Analysis Results
In accordance with Formula (1), calculate the phosphorus content wP in the specimen, expressed
in mass fraction (%).
4.7 Allowable Difference
The difference in the intra-laboratory and inter-laboratory analysis results shall be not greater
than the allowable difference listed in Table 2.Otherwise, the number of additional
measurements and the analysis results shall be determined as specified in Appendix A.
5 Method 2.Bismuth Phosphomolybdate Blue Spectrophotometric Method
5.1 Principle
The test portion is decomposed by nitric acid and hydrofluoric acid. Add perchloric acid to
evaporate it, until emitting smoke, thereby oxidizing phosphorus into orthophosphoric acid. In
sulfuric acid medium,
5.2 Reagents and Materials
Unless otherwise specified, only reagents that are confirmed to be analytically pure are used in
the analysis. The test water is distilled water or water with an equivalent purity of Grade-3 or
above that complies with the provisions of GB/T 6682.
5.2.7 Sodium hydroxide solution, 250 g/L. Stored in plastic bottles.
5.2.8 Sodium thiosulfate solution, 10 g/L.
Weigh-take 1.0 g of sodium thiosulfate and 2.0 g of anhydrous sodium sulfite, dissolve it in 100
mL of water, and mix it well. Prepare it right before use.
5.2.9 Bismuth nitrate solution, 30 g/L.
Weigh-take 30 g of bismuth nitrate [Bi(NO3)3 5H2O] and dissolve it in 100 mL of nitric acid
(see 5.2.1). After it is completely dissolved, add 900 mL of water and 4 g of urea, and mix it
well.
5.2.14 Phosphorus standard solution, 100 g/mL.
5.2.16 Phosphorus standard solution, 2.5 g/mL.
Weigh-take 25.00 mL of phosphorus standard solution (see 5.2.14) into a 1,000 mL volumetric
flask. Use water to dilute to the scale and mix it well. 1 mL of this solution contains 2.5 g of
phosphorus.
5.2.17 Phenolphthalein solution, 1 g/L.
Weigh-take 0.1 g of phenolphthalein into a 150 mL beaker and add 50 mL of ethanol (950 g/L)
to dissolve it. Add water to dilute to 100 mL and mix it well.
5.3 Instruments
In the analysis, only common laboratory instruments are used. The one-mark volumetric flasks,
graduated pipettes and one-mark pipettes used shall respectively comply with the requirements
of GB/T 12806, GB/T 12807 and GB/T 12808.
5.4 Sampling and Sample Preparation
In accordance with the provisions of GB/T 4010, conduct sampling and sample preparation.
The specimens shall all pass the 0.125 mm sieve mesh.
5.5 Analytical Steps
5.5.1 Number of determinations
For the same specimen, conduct at least 2 independent determinations.
5.5.2 Amount of test portion
In accordance with Table 3, weigh-take the specimens, accurate to 0.0001 g.
Table 3 -- Amount of Test Portion and Recommended Thickness of Cuvette
5.5.3 Blank test
Along with the test portion, carry out a blank test.
5.5.4 Determination
5.5.4.1 Decomposition of test portion
5.5.5 Drawing of Calibration Curve
5.5.5.1 Drawing of calibration curve of manganese metal with low phosphorus content
(mass fraction 0.0030% ~ 0.020%)
5.5.5.2.1 Transfer-take 0 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL and 6.00 mL of
phosphorus standard solution (see 5.2.15) and place them into a set of 50 mL beakers.
Respectively transfer 1.00 mL of ferric ammonium sulfate solution (see 5.2.13) into them, add
5.00 mL of sulfuric acid (see 5.2.4), use water to adjust the volume to about 20 mL, add 5 mL
of sodium thiosulfate solution (see 5.2.8), mix them well, then, add 5 mL of bismuth nitrate
solution (see 5.2.9), use water to purge the wall of the beakers,
5.5.5.3 Drawing of calibration curve of ferromanganese, ferromanganese-silicon,
nitrogen-bearing ferromanganese
5.5.5.3.1 Transfer-take 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL and 10.00 mL of phosphorus
standard solution (see 5.2.15) and place them into a set of 50 mL beakers. Respectively transfer
1.5 mL of ferric ammonium sulfate solution (see 5.2.13) into them, add 5.00 mL of sulfuric acid
(see 5.2.4), use water to adjust the volume to about 20 mL, add 5 mL of sodium thiosulfate
solution (see 5.2.8), mix them well, then, add 5 mL of bismuth nitrate solution (see 5.2.9), use
water to purge the wall of the beakers, and shake them well. Add 5 mL of ammonium molybdate
solution (see 5.2.10), use water to purge the wall of the beakers, and shake them well; add 5 mL
of ascorbic acid solution (see 5.2.11) and mix them well; use water to dilute them to the scale
and mix them well. Let them stand for 15 minutes.
5.5.5.3.2 Transfer the test solutions (see 5.5.5.3.1) into 0.5 cm cuvettes. At a wavelength of 700
nm, use water as a reference to zero the spectrophotometer, and measure their absorbance.
6 Test Report
The test report shall include the following content.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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