GB/T 223.63-2022 English PDF (GB/T223.63-2022)

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GB/T 223.63-2022: Iron, steel and alloy - Determination of manganese content - Sodium (potassium) periodate spectrophotometric method
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 c...