GB/T 223.64-2008 English PDF (GB/T223.64-2008)

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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 than 0.02 μg/mL in a solution similar to the matrix of the final sample solution.
5.1.3 Calibration curve linearity (see Appendix A.3)
When measured in the same manner, the slope of the upper 20% of the calibration curve (expressed as the change in absorbance) is proportional to the lower 20% conc.
The slope of the degree of the ratio of the value should not be less than 0.7.
For instruments calibrated automatically with two or more standard samples, the absorbance readings obtained should be used prior to analysis to
Find the linear calibration curve.
5.1.4 characteristic concentration (see Appendix A.4)
In solutions consistent with the final sample solution matrix, the characteristic concentration of manganese should be less than 0.1 μg/mL.
5.2 Auxiliary devices
It is recommended to use tape recorders or digital reading devices to evaluate the indicators in 5.1.1 to 5.1.3 and make further measurements.
The scale can be magnified until the observed noise is greater than the reading error, and absorbance below 0.1 is recommended. If you have to use the scale to put
Large, but can not read the magnification, available in the following ways to get the magnification. respectively, with and without the use of scale amplification
The appropriate amount of solution absorbance, calculate the ratio of the signal measured.
6 sample preparation
Prepare samples according to ISO 377-2 or appropriate national standards.
7 Analysis steps
WARNING. In the presence of ammonia, nitrous acid fumes, or organic matter, it may cause an explosion when exposed to perchloric acid fumes. All evaporations must be made at a suitable time
Perchloric acid fume hood.
Make sure to flush the sprinkler system and drain system after using perchloric acid.
GB/T 223.64-2008/ISO 10700..1994
7.1 Sample volume
Weigh about 1.0g sample, accurate to 0.001g.
7.2 blank test
Follow the same procedure with a blank test run, using the same amount of reagent and the amount of pure iron (4.1) used
the same.
7.3 Determination
7.3.1 Preparation of test solution
The sample (7.1) placed in 250mL beaker, add 20mL hydrochloric acid (4.2), cover the watch glass, low temperature heating dissolved until the reaction was stopped.
Add 5mL nitric acid (4.4) boil 1min, drive away the nitrogen oxides, add 15mL perchloric acid (4.5), without covering the surface of the dish heated at high temperature until
smoke. Then cover the watch glass to continue heating, heating temperature should make perchloric acid smoke in the beaker wall to maintain a steady reflux, continue heating until
Perchloric acid smoke can not be seen in the beaker.
Hydrochloric acid and nitric acid is not easy to dissolve the sample, add 15mL perchloric acid before the addition of 2mL hydrofluoric acid (4.3), continue with the above operation
get on.
7.3.2 solution treatment
7.3.2.1 Manganese content (mass fraction) below 0.10%
Cooling, adding 25mL of water, slightly soluble salts, cooled again, quantitatively transferred to 250mL single standard line volumetric flask, diluted with water until engraved
Degree, mix well. Filter with medium speed filter paper, filter out the residue or precipitate, after discarding the first part, the filtrate collected in a clean dry beaker.
This filtrate is the determination of manganese content (mass fraction) below 0.10% of the test solution.
7.3.2.2 Manganese content (mass fraction) 0.10% ~ 0.40%
Pipette 50.0mL filtrate (7.3.2.1) in.200mL single-labeled volumetric flask, diluted with water to the mark, and mix.
7.3.2.3 Manganese content (mass fraction) at 0.40% ~ 2.0%
Pipette 10.0mL filtrate (7.3.2.1) in.200mL single-labeled volumetric flask, diluted with water to the mark, and mix.
7.3.3 Preparation of calibration solution
7.3.3.1 Manganese content (mass fraction) below 0.10%
40.0mL bottom solution (4.6) were added to eight 100mL single-labeled volumetric flask, with a burette or pipette according to Table 1 was added to the phase
The volume of manganese standard solution (4.7.2), diluted with water to the mark, mix well.
Table 1 manganese content below 0.10% of the calibration solution
Manganese standard solution (4.7.2) Volume/mL Manganese mass/mg Equivalent to the manganese content (mass fraction) /%
0a
0.4
2.0
4.0
8.0
12.0
16.0
20.0
0.008
0.04
0.08
0.16
0.24
0.32
0.40
0.002
0.010
0.020
0.040
0.060
0.080
0.100
a Zero calibration solution.
7.3.3.2 Manganese content (mass fraction) is 0.10% ~ 0.40%
The 10.0mL bottom solution (4.6) were added to six 100mL single-labeled volumetric flask, with a burette or pipette according to Table 2 added phase
The volume of manganese standard solution (4.7.2), diluted with water to the mark, mix well.
GB/T 223.64-2008/ISO 10700..1994
Table 2 manganese content of 0.10% ~ 0.40% of the calibration solution
Manganese standard solution (4.7.2) Volume/mL Mass of manganese/mg Equivalent to manganese in sample /%
0a
4.0
8.0
12.0
16.0
20.0
0.08
0.16
0.24
0.32
0.40
0.080
0.16
0.24
0.32
0.40
a Zero calibration solution.
7.3.3.3 Manganese content (mass fraction) is 0.40% ~ 2.0%
The 2.0mL bottom solution (4.6) were added to six 100mL single-labeled volumetric flask, with a burette or pipette according to Table 3 added phase
The volume of manganese standard solution (4.7.2), diluted with water to the mark, mix well.
Table 3 manganese content of 0.40% ~ 2.0% calibration solution
Manganese standard solution (4.7.2) Volume/mL Mass of manganese/mg Equivalent to manganese in sample /%
0a
4.0
8.0
12.0
16.0
20.0
0.08
0.16
0.24
0.32
0.40
0.40
0.80
1.20
1.60
2.00
a Zero calibration solution.
7.3.4 Atomic absorption spectrometer adjustment
The adjustment of the instrument is shown in Table 4.
Table 4 Instrument Adjustment
Feature characteristics
Type of lamp
wavelength
flame
Lamp current
bandwidth
Manganese hollow cathode lamp
279.5 nm
Air-acetylene lean flame with maximum manganese response
Follow the manufacturer's recommendations
Follow the manufacturer's recommendations
Warning. In strict accordance with the manufacturer's recommendations, in particular, should pay attention to the following safety points.
犪) acetylene is explosive, should always pay attention to use;
犫) Wear colored glasses to protect the operator's eyes from UV radiation damage;
犮) The burner should be kept clean and free from salt. Plugging of the burner may result in tempering;
7.3.5 ...