GB/T 223.63-2022_English: PDF (GB/T223.63-2022)
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Iron, steel and alloy - Determination of manganese content - Sodium (potassium) periodate spectrophotometric method
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GB/T 223.63-2022
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| GB/T 223.63-1988 | English | 85 |
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Methods for chemical analysis of iron, steel and alloy - The sodium (potassium) periodate photometric method for the determination of manganese content
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GB/T 223.63-1988
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| Standard ID | GB/T 223.63-2022 (GB/T223.63-2022) | | Description (Translated English) | Iron, steel and alloy - Determination of manganese content - Sodium (potassium) periodate spectrophotometric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.080.01 | | Date of Issue | 2022-07-11 | | Date of Implementation | 2023-02-01 | | Older Standard (superseded by this standard) | GB/T 223.63-1988 | | Standard ID | GB/T 223.63-1988 (GB/T223.63-1988) | | Description (Translated English) | Methods for chemical analysis of iron, steel and alloy - The sodium (potassium) periodate photometric method for the determination of manganese content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.08 | | Word Count Estimation | 4,444 | | Date of Issue | 1988/2/5 | | Date of Implementation | 1989/2/1 | | Older Standard (superseded by this standard) | GB 223.4-1981 | | Drafting Organization | Ministry of Metallurgical Industry | | Administrative Organization | Ministry of Metallurgical Industry | | Issuing agency(ies) | National Bureau of Standards | | Summary | This standard applies to pig iron, iron, carbon steel, alloy steel, high temperature alloys, precision determination of the amount of manganese alloys. Measuring range: 0. 010% to 2. 00%. |
GB/T 223.63-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.080.01
CCS H 11
Replacing GB/T 223.63-1988
Iron, Steel and Alloy - Determination of Manganese Content
- Sodium (potassium) Periodate Spectrophotometric Method
(ISO 629:1982, Steel and Cast Iron - Determination of Manganese Content -
Spectrophotometric Method, NEQ)
ISSUED ON: JULY 11, 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 ... 6
2 Normative References ... 6
3 Terms and Definitions ... 7
4 Principle ... 7
5 Reagents or Materials ... 7
6 Instruments and Equipment ... 9
7 Sample ... 9
8 Test Procedures ... 9
9 Processing of Test Data ... 12
10 Precision ... 12
11 Test Report ... 13
Appendix A (informative) Constituent Documents of GB/T 223 ... 14
Appendix B (informative) Relevant Information of Precision Test ... 20
Iron, Steel and Alloy - Determination of Manganese Content
- Sodium (potassium) Periodate Spectrophotometric Method
WARNING---the personnel using this document shall have practical experience in formal
laboratory work. This document does not point out all possible safety issues. It is the user’s
responsibility to take appropriate safety and health measures and ensure the compliance
with the conditions stipulated in the relevant national laws and regulations.
1 Scope
This document specifies the method for the determination of manganese content in iron, steel
and alloy by the sodium (potassium) periodate spectrophotometric method.
This document is applicable to the determination of manganese content in iron, steel, high-
temperature alloy and precision alloy. The range of determination is: 0.001% ~ 4.00%.
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 6379.1 Accuracy (trueness and precision) of Measurement Methods and Results - Part 1:
General Principles and Definitions
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 7729 Chemical Analysis of Metallurgical Products - General Rule for Spectrophotometric
Methods
GB/T 12805 Laboratory Glassware - Burettes
GB/T 12806 Laboratory Glassware - One-mark Volumetric Flasks
GB/T 12808 Laboratory Glassware - One-mark Pipettes
GB/T 20066 Sample and Iron - Sampling and Preparation of Samples for the Determination of
Chemical Composition
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Principle
After the specimen is dissolved in acid, in sulfuric acid and phosphoric acid medium, use
sodium (potassium) periodate to oxidize manganese to heptavalent; at a wavelength of 530 nm,
use a spectrophotometer to measure the absorbance.
5 Reagents or Materials
Unless it is otherwise specified, only reagents confirmed to be analytically pure, as well as
distilled water or deionized water (or water of equivalent purity) are used in the analysis.
5.1 Hydrofluoric Acid
ρ is about 1.15 g/mL.
5.2 Hydrochloric Acid
ρ is about 1.19 g/mL.
5.3 Nitric Acid
ρ is about 1.42 g/mL.
5.4 Nitric Acid, 1 + 4
Dilute with nitric acid (5.3).
5.5 Sulfuric Acid, 1 + 1
Dilute with sulfuric acid with ρ about 1.84 g/mL.
5.6 Perchloric Acid, 1 + 499
Dilute with perchloric acid with ρ about 1.67 g/mL.
5.7 Phosphoric Acid - Perchloric Acid Mixed Acid
Mix three portions of phosphoric acid (ρ about 1.69 g/mL) and one portion of perchloric acid
(ρ about 1.67 g/mL).
5.8 Sodium (potassium) Periodate Solution, 50 g/L
Weigh-take 5 g of sodium periodate or potassium periodate and place in a 250 mL beaker; add
60 mL of water and 20 mL of nitric acid (see 5.3), warm to dissolve it, then, cool it. Use water
to dilute to 100 mL and mix it well.
5.9 Sodium Nitrite Solution, 10 g/L
Weigh-take 1 g of sodium nitrite, place in a 250 mL beaker, add 60 mL of water to dissolve it,
then, use water to dilute to 100 mL and mix it well.
5.10 Manganese Standard Solution
5.10.1 Manganese standard solution, 500 g/mL
Weigh-take 1.4383 g of potassium permanganate (mass fraction not less than 99.9%) and place
in a 600 mL beaker; add 300 mL of water to dissolve it, add 10 mL of sulfuric acid (see 5.5)
and dropwise add hydrogen peroxide (ρ about 1.10 g/mL), until the red color just disappears;
heat to boil for 5 min ~ 10 min, then, cool it. Transfer it to a 1,000 mL volumetric flask; use
water to dilute to the mark and mix it well.
Alternatively, weigh-take 0.5000 g of electrolytic manganese (mass fraction not less than 99.9%)
[electrolytic manganese needs to be cleaned in sulfuric acid (5 + 95) in advance, and after
manganese oxide on the surface is cleaned, take it out, immediately use distilled water to
repeatedly wash it, then, wash it in absolute ethanol for 4 ~ 5 times, take it out and dry it in a
desiccator before use] and place in a 250 mL beaker; add 20 mL of nitric acid (1 + 3), heat to
dissolve it and boil to drive out nitrogen oxides; remove and cool it to room temperature. Then,
transfer to a 1,000 mL volumetric flask, use water to dilute to the mark and mix it well.
1 mL of this standard solution contains 500 g of manganese.
5.10.2 Manganese standard solution, 100 g/mL
Weigh-take 20.0 mL of manganese standard solution (see 5.10.1) and place in a 100 mL
volumetric flask; use water to dilute to the mark and mix it well.
1 mL of this standard solution contains 100 g of manganese.
5.10.3 Manganese standard solution, 20 g/mL
Weigh-take 20.0 mL of manganese standard solution (see 5.10.2) and place in a 100 mL
volumetric flask; use water to dilute to the mark and mix it well.
1 mL of this standard solution contains 20 g of manganese.
5.11 Water without Reducing Substances
Heat distilled water or deionized water to boil, use 10 mL of sulfuric acid (1 + 3) to acidify each
liter; add a few granules of sodium (potassium) periodate and continue to boil for 1 min ~ 2
min, cool it before use.
reaction stops. Add 1 mL ~ 2 mL of hydrochloric acid (see 5.2), and continue heating,
until it is completely decomposed.
---For high-nickel-chromium specimens, add 10 mL of (3 + 1), (6 + 1) or (10 + 1) mixed
acid of hydrochloric acid (see 5.2) and nitric acid (see 5.3), heat at low temperature to
dissolve it.
NOTE: when the amount of specimen is 2 g, depending on the situation, the amount of acid can be
increased, so that the specimen can be completely dissolved.
Add 10 mL of phosphoric acid - perchloric acid mixed acid (see 5.7) [when the amount of
specimen is 2.0 g, add 15 mL of phosphoric acid - perchloric acid mixed acid (see 5.7); when
using 15 mL of phosphoric acid - perchloric acid mixed acid (see 5.7) to dissolve high-tungsten
specimens, it is not necessary to add], heat and evaporate it, until perchloric acid fumes are
emitted for 2 min ~ 5 min (for specimens with high chromium content, the chromium needs to
be oxidized); slightly cool and add water to dissolve salts. If necessary, remove graphitic carbon
by filtration and use hot perchloric acid (see 5.6) to wash it.
---When the manganese content is not greater than 2.00%, add 10 mL of sulfuric acid (see
5.5) and use water to dilute to about 40 mL.
---When the manganese content is greater than 2.00%, add 10 mL of sulfuric acid (see 5.5)
and use water to dilute to about 40 mL; cool to room temperature, then, transfer to a
100 mL volumetric flask; use water to dilute to the mark and mix it well. Transfer-take
50.0 mL of test solution in a 150 mL conical flask, additionally add 5 mL of sulfuric
acid (see 5.5).
8.2.2 Color development
In the test solution prepared in 8.2.1, add 10 mL of sodium (potassium) periodate solution (see
5.8), heat to boil and maintain it for 2 min ~ 3 min (to prevent the test solution from splashing
out); cool to room temperature and transfer to a 100 mL volumetric flask; use water without
reducing substances (see 5.11) to dilute it to the mark and mix it well.
8.2.3 Preparation of reference solution
Transfer-take about 25 mL of chromogenic solution (see 8.2.2) to a 100 mL conical flask; while
shaking it, dropwise add sodium nitrite solution (see 5.9), until the purple color just fades (see
NOTE). Use this solution as the reference solution.
NOTE: when the cobalt-containing specimen is faded with sodium nitrite solution, the reddish
color of cobalt will not fade, and it can be handled in accordance with the following method:
constantly shake the volumetric flask, slowly and dropwise add sodium nitrite solution (see
5.9), if the reddish color of the specimen remains unchanged, put the solution in an
absorption vessel and measure its absorbance; add sodium nitrite solution (see 5.9) to the
remaining test solution, then, measure the absorbance again, until there is no change in the
absorbance.
9 Processing of Test Data
Utilize the calibration curve (see 8.2.5.2) to convert the absorbance to the mass of manganese
in the corresponding test solution, expressed in g.
The manganese content (wMn), which is expressed in mass fraction (%), shall be calculated in
accordance with Formula (1):
Where,
m1---the mass of manganese obtained from the calibration curve, expressed in (g);
m---the amount of specimen, expressed in (g);
V---the total volume of the test solution, expressed in (mL);
V1---the volume of the divided test solution, expressed in (mL).
10 Precision
The precision test in this document was performed by 10 laboratories on 10 levels of manganese
content. Each laboratory determines each level of manganese content twice under the
repeatability conditions specified in GB/T 6379.1.
See Table B.1 of Appendix B for the specimens used. See Table B.2 of Appendix B for the
original data of the precision test.
In accordance with GB/T 6379.2, conduct statistical analysis on the obtained results. The results
suggest that there is a logarithmic relation between the manganese content and the repeatability
limit (r) and reproducibility limit (R) of the test results, which are summarized in Table 3.
The repeatability limit (r) and reproducibility limit (R) are obtained through the equation
provided in Table 3.
Under repeatability conditions, the absolute difference of the obtained two independent
......
GB 223.63-1988
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
UDC 669.14/.15. 543.06
H 11
GB 223.63-88
Replacing GB 223.4-81 Method III
Methods for Chemical Analysis of Iron, Steel and Alloy -
The Sodium (Potassium) Periodate Photometric Method
for the Determination of Manganese Content
ISSUED ON. FEBRUARY 05, 1988
IMPLEMENTED ON. FEBRUARY 01, 1989
Issued by. National Bureau of Standards;
Approved by. Ministry of Metallurgical Industry of PRC, January 18, 1988.
Table of Contents
1 Method Summary ... 3
2 Reagents ... 3
3 Analysis Procedures ... 4
4 Calculation of Analysis Results ... 6
5 Precision ... 6
Appendix A Original Data on Precision Test (Supplement) ... 8
Additional information... 8
Methods for Chemical Analysis of Iron, Steel and Alloy -
The Sodium (Potassium) Periodate Photometric Method
for the Determination of Manganese Content
This Standard is applicable to the determination of manganese content in pig iron, iron
powder, carbon steel, alloy steel, high-temperature alloy, precision alloy. The
measuring range is 0.010% ~ 2.00%.
This Standard complies with GB 1467-78 Method for Chemical Analysis of Metallurgy
Product – General Rules and Regulations.
This Standard complies with GB 7729-87 Chemical Analysis of Metallurgical Products
– General Rule for Spectrophotometric Methods.
1 Method Summary
After the specimen is dissolved in the acid, use sodium (potassium) periodate to
oxidize the manganese in the sulfuric acid or phosphoric acid medium into heptavalent;
then measure its absorbance.
2 Reagents
2.1 Hydrofluoric acid (ρ 1.15g/ml).
2.2 Hydrochloric acid (ρ 1.19g/ml).
2.3 Nitric acid (ρ 1.42g/ml).
2.4 Nitric acid (1+4).
2.5 Nitric acid (2+98).
2.6 Sulfuric acid (1+1).
2.7 Mixed acid of phosphoric acid – perchloric acid. evenly mix 3 pieces of
phosphoric acid (ρ 1.69g/ml) and 1 piece of perchloric acid (ρ 1.67g/ml).
2.8 Sodium (potassium) periodate solution (5%). take 5g of sodium (potassium)
periodate; place into 250ml beaker; add 60ml of water, 20ml of nitric acid (2.3); after
warmly dissolving, cool off. Use water to dilute to 100ml; mix evenly.
2.9 Sodium nitrite solution (1%).
2.10 Standard manganese solution
2.10.1 Take 1.4383g of reference potassium permanganate; place into 600ml beaker;
add 300ml of water to dissolve; add 10ml of sulfuric acid (2.6), titrate hydrogen
peroxide (ρ 1.10g/ml) till the red just fades; heating and boiling for 5~10min; cool off.
Transfer into 1000ml volumetric flask; use water to dilute to the scale; mix evenly. 1ml
of such solution contains 500µg of manganese.
It can also take 0.5000g of electrolytic manganese (99.9% above) [the electrolytic
manganese shall be pre-cleaned in sulfuric acid (5+95), after the manganese oxide on
the surface is removed, take out; immediately use distilled water to wash repeatedly;
then place into anhydrous ethanol to wash for 4~5 times; take out to place into the
dryer; it can be used after drying], place into 250ml beaker; add 20ml nitric acid (1+3);
heat and dissolve; boiling to expel the nitrogen oxide; take off, cool off to the room
temperature; transfer into 1000ml volumetric flask; use water to dilute to the scale, mix
evenly. 1ml of such solution contains 500µg of manganese.
2.10.2 Take 20.00ml of standard manganese solution (2.10.1); place into 100ml
volumetric flask; use water to dilute to the scale, mix evenly. 1ml of such solution
contains 100µg of manganese.
2.11 Water containing no reduction material. heat and boil the deionized (distilled)
water; each liter shall be acidized by 10ml of sulfuric acid (1+3); add several particles
of sodium (potassium) periodate; continue to boil for several minutes; it can be used
after cooling off.
3 Analysis Procedures
3.1 Specimen quantity
Take specimen as per Table 1.
Table 1
3.2 Determination
3.2.1 Place the specimen (3.1) into 150ml conical flask; add 15ml of nitric acid (2.4)
[high-silicon specimen shall be added 3~4 drops of hydrofluoric acid (2.1); pig-iron
specimen shall be dissolved by nitric acid (1+4); and titrate 3~4 drops of hydrofluoric
acid (2.1); after the specimen is dissolved; take off to cool; use the rapid filter paper to
filter it into another 150ml conical flask; use hot nitric acid (2.5) to wash the original
conical flask and filter paper for 4 times; high-nickel-chromium specimen shall be
dissolved by appropriate proportion of mixed acid between hydrochloric acid (2.2) and
nitric acid (2.3); for high-tungsten specimen (5% above) or hard-to-dissolve specimen,
add 15ml of mixed acid of phosphoric acid-perchloric acid (2.7) to dissolve], heat at
low temperature and dissolve.
3.2.2 Add 10ml of mixed acid of phosphoric acid-perchloric acid (2.7) [when high-
tungsten specimen is dissolved by 15ml of mixed acid of phosphoric acid-perchloric
acid (2.7), it shall not be added]; heat, vaporize till perchloric acid (high-chromium
specimen shall be oxidized the chromium) is smoked; cool off slightly; add 10ml of
sulfuric acid (2.6); use water to dilute to about 40ml.
3.2.3 Add 10ml of sodium (potassium) periodate solution (2.8); heat to boil, and keep
for 2~3min (avoid the specimen solution splashing); cool off to the room temperature;
transfer into 100ml volumetric flask; use water containing no reduction material (2.11)
to dilute to the scale, mix evenly.
3.2.4 Transfer partial coloring solution into absorption vessel as per Table 1; titrate
sodium nitrite solution (2.9) to the remained coloring solution as shake it till the purple
red just fades [when use sodium nitrite solution to fade the cobalt-containing specimen,
if the slight-red doesn’t fade, it can be treated by the following method. shake the
volumetric flask continuously; slowly titrate sodium nitrite solution (2.9); if the slight-red
of specimen has no change, place the specimen solution into the absorption vessel;
measure its absorbance; add sodium nitrite solution (2.9) to the remained solution;
measure the absorbance again till the two absorbances have no change; then such
Content Range, %
Specimen quantity, g
Concentration of standard manganese solution, µg/ml
Transferring volume of standard manganese
solution, ml
Absorption vessel, cm
solution can be used as the reference solution], transfer such solution into another
absorption vessel as the reference; measure its absorbance at wavelength of 530nm
on the spectrophotometer.
3.2.5 According to the measured absorbance of specimen solution, then check the
corresponding manganese content from the working curve.
3.3 Draw working curve
Take standard manganese solution as per Table 1; separately place into 150ml conical
flasks; then follow the procedures of 3.2.2~3.2.4; measure its absorbance. Take
manganese content as abscissa, and absorbance as the ordinate to draw working
curve.
4 Calculation of Analysis Results
Calculate the percentage content of manganese as per the following formula.
Where.
m1 – manganese content checked from the working curve, g;
m0 – specimen quantity, g.
5 Precision
The precision in this Standard indicates after testing the same uniform specimens
uniformly distributed in the measuring range of this method according to the analysis
procedures of this method in 10 laboratories in 1987, then summarize the data; and
obtained the repeatability of r and reproducibility of R (see Table 2) through statistical
analysis as per GB 6379-86 Precision of Test Methods; Determination of Repeatability
and Reproducibility for A Standard Test Method by Interlaboratory Tests.
Table 2
Repeatability indicates the maximum difference between two independent test results
Level, % (m/m) Repeatability r Reproducibility R
performed on the same specimen by the same operator, in the same laboratory using
the same instrument under the normal and correct conditions under this method, with
a 95% probability.
Reproducibility indicates the maximum difference between two independent test
results performed on the same specimen by two operators, in different laboratories
under normal and correct conditions of this method, with a 95% probability.
If the difference of two independent test results exceed the corresponding repeatability
and reproducibility; then the two results are dubious.
Appendix A
Original Data on Precision Test
(Supplement)
Additional information.
This Standard shall be under the jurisdiction of Central Iron and Steel Research
Institute, Ministry of Metallurgical industry.
This Standard was responsibly drafted by Central Iron and Steel Research Institute,
Ministry of Metallurgical industry.
This Standard was drafted by Central Iron and Steel Research Institute, Ministry of
Levels
Labs
Metallurgical industry; and Jiangxi Steel Plant.
This Standard’s chief drafter. Ke Ruihua.
This Standard’s level mark. GB 223.63-88 Y
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