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GB/T 223.64-2008 English PDF (GBT223.64-2008)

GB/T 223.64-2008 English PDF (GBT223.64-2008)

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GB/T 223.64-2008: Iron, steel and alloy -- Determination of manganese content -- Flame atomic absorption spectrometric method
GB/T 223.64-2008
Iron, steel and alloy. Determination of manganese content. Flame atomic absorption spectrometric method
ICS 77.080.01
H11
National Standards of People's Republic of China
GB/T 223.64-2008/ISO 10700..1994
Replacing GB/T 223.64-1988
Steel and alloy - Determination of manganese content
Flame atomic absorption spectrometry
(ISO 10700..1994, IDT)
2008-05-13 released
2008-11-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
This part of GB/T 223 is equivalent to ISO 10700..1994 "Determination of manganese content of steel flame atomic absorption spectrometry."
For ease of use, this section made the following editorial changes.
a) Replace the word "international standard" with "this part";
b) Use "." instead of "," as the decimal point
c) Delete the preface to the International Standard.
This section instead of GB/T 223.64-1988, compared with the main changes made to the following.
--- Determination range from 0.1% ~ 2.0% adjusted to 0.002% ~ 2.0%;
--- The amount of sample is adjusted from 0.5000g to 1.0g;
--- Sample processing according to different samples by adding different acids into a unified by hydrochloric acid, nitric acid dissolved, perchloric acid smoke;
--- From a unified calibration curve to a piecemeal calibration curve.
This part of the Appendix A normative appendix, Appendix B and Appendix C are informative appendices.
This part is proposed by China Iron and Steel Association.
This part of the National Standardization Technical Committee Iron and Steel centralized.
This section mainly drafted by. Wuhan Iron and Steel (Group) Company.
The main drafters of this section. Li Xiaojie, Shen Ke, Shang Hui, Zhou Daqing.
This part of the standard replaces the previous editions are.
--- GB/T 223.64-1988.
GB/T 223.64-2008/ISO 10700..1994
Steel and alloy - Determination of manganese content
Flame atomic absorption spectrometry
Warning. Personnel using this section should have practical experience in formal laboratory work. This section does not indicate all possible security issues. Make
It is the user's responsibility to take appropriate safety and health measures and to ensure compliance with the requirements of the relevant state laws and regulations.
1 range
This section GB/T 223 specifies the determination of manganese content in steel by flame atomic absorption spectrometry.
This section applies to the mass fraction of 0.002% ~ 2.0% determination of manganese content.
2 Normative references
The following documents contain provisions that, through reference in this section, become the provisions of this part of GB/T 223. Any reference to the date of the citation
All subsequent amendments (not including errata content) or revisions do not apply to this section, however, encouraged to be reached under this section
The parties to the agreement study whether the latest versions of these documents are available. For undated references, the latest version applies to this book
section.
ISO 377-2. 1989 Selection and preparation of test specimens for sample and forged steels - Part 2. Samples for determination of chemical composition
ISO 385-1. 1984 Laboratory glassware burets - Part 1. Basic requirements
Laboratory glassware single standard pipette
ISO 5725. 1986 Precision of measurement methods - Repeatability and reproducibility of standard measurement methods are determined by interlaboratory tests
ISO 1042. 1983 Laboratory glassware single standard line volumetric flask
ISO 3696. 1987 Analysis of laboratory water specifications and test methods
3 principle
Sample with hydrochloric acid and nitric acid decomposition, plus perchloric acid evaporated to take white smoke. The solution is injected into the air - acetylene flame, with a hollow cathode lamp made of manganese
Light source, Atomic absorption spectrometer at 279.5nm, atomic absorption spectrometry.
4 reagent
Unless otherwise indicated in the analysis, only certified analytical reagents and secondary water specified in ISO 3696 are used.
4.1 Pure iron, manganese-free or known residual manganese content.
4.2 Hydrochloric acid, p approximately 1.19 g/mL.
4.3 hydrofluoric acid, p about 1.15 g/mL.
4.4 nitric acid, p about 1.40 g/mL.
4.5 perchloric acid, ρ about 1.54g/mL.
Note 1. Perchloric acid with a density of 1.67 g/mL, 100 mL of perchloric acid with a density of 1.54 g/mL and 79 mL with a density of 1.67 g/mL
Perchloric acid quite.
4.6 The bottom liquid. Weigh 10.00g pure iron (4.1), accurate to 0.01g, placed in a 1000mL beaker, add.200mL hydrochloric acid (4.2),
Cover the beaker with a watch glass and heat at low temperature until the pure iron decomposes, then add 50 mL of nitric acid (4.4) to oxidize. Add 150 mL perchloric acid
(4.5), high temperature heating, until the concentration of white perchloric acid smoke. Continue to smoke 15min, control the temperature of white perchloric acid smoke in the beaker wall shape
Into a stable return. Cool, add 300mL water, low temperature heat to dissolve salts. Quantitatively transferred to 1000mL single standard line volumetric flask, water
Dilute to the mark and mix well. 1mL The bottom liquid contains 0.010g of iron.
GB/T 223.64-2008/ISO 10700..1994
4.7 manganese standard solution
4.7.1 Manganese stock solution, equivalent to 1.00g manganese per liter. Weigh 1.000g pure manganese metal [purity ≥ 99.9% (mass fraction)], accurate to
0.1mg, placed in 250mL beaker, add 40mL hydrochloric acid (4.2), cover the surface of the dish, low temperature heating until the manganese completely decomposed. Cool, will
Quantitative solution into the 1000mL single-standard line volumetric flask, diluted with water to the mark, mix. This standard solution 1mL contains 1.00mg manganese.
4.7.2 manganese standard solution, equivalent to 0.0200g per liter of manganese. Pipette 20.0mL stock solution (4.7.1) in 1000mL single standard line capacity
Bottle, diluted with water to the mark, mix well. Prepared before use. This standard solution 1mL contains 0.0200mg manganese.
5 instruments
All glass feelers shall comply with Class A of ISO 385-1, ISO 648 or ISO 1042.
5.1 Atomic Absorption Spectrometer with Manganese Hollow Cathode Lamps, Supplied Air - The acetylene gas should be pure enough not to contain water, oil, and manganese to mention
For the stable and clear lean flame.
After optimization of the atomic absorption spectrometer according to 7.3.5, the detection limit and characteristic concentration should be consistent with the parameters provided by the instrument manufacturer, and satisfy
Indicators in 5.1.1 to 5.1.3.
The apparatus should also meet the additional performance requirements given in 5.1.4.
5.1.1 Minimum precision (see Appendix A.1)
With the highest concentration of the calibration solution, absorbance measured 10 times, calculate the standard deviation of this standard deviation shall not exceed this solution absorbance level
1.5% of the mean.
Measure the absorbance 10 times with the lowest calibration solution (not a zero calibration solution) and calculate its standard deviation, which should not exceed
The highest concentration of 0.5% of the average absorbance of the calibration solution.
5.1.2 detection limit (see Appendix A.2)
The detection limit is defined as the standard deviation of the 10 absorbance measurements of the analyte element in the solution slightly above the zero calibration solution
2 times.
The detection limit of manganese should be less tha...
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