GB/T 223.54-2022_English: PDF (GB/T223.54-2022)
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Iron, steel and alloy - Determination of nickel content - Flame atomic absorption spectrometric method
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GB/T 223.54-2022
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GB/T 223.54-1987 | English | 75 |
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Methods for chemical analysis of iron, steel and alloy - The flame atomic absorption spectrophotometric method for the determination of nickel content
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GB/T 223.54-1987
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Standard ID | GB/T 223.54-2022 (GB/T223.54-2022) | Description (Translated English) | Iron, steel and alloy - Determination of nickel content - Flame atomic absorption spectrometric 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International Standard | 77.080.01 | Date of Issue | 2022-07-11 | Date of Implementation | 2023-02-01 | Older Standard (superseded by this standard) | GB/T 223.54-1987 | Standard ID | GB/T 223.54-1987 (GB/T223.54-1987) | Description (Translated English) | Methods for chemical analysis of iron, steel and alloy - The flame atomic absorption spectrophotometric method for the determination of nickel content | Sector / Industry | National Standard (Recommended) | Classification of Chinese Standard | H11 | Classification of International Standard | 77.08 | Word Count Estimation | 3,366 | Date of Issue | 1987/5/12 | Date of Implementation | 1988/3/1 | Drafting Organization | Ministry of Metallurgical Industry | Administrative Organization | Ministry of Metallurgical Industry | Issuing agency(ies) | Ministry of Metallurgical Industry | Summary | This standard applies to iron, carbon steel, low alloy nickel content. Measurement range: 0. 005 to 0. 50%. |
GB/T 223.54-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.080.01
CCS H 11
Replacing GB/T 223.54-1987
Iron, Steel and Alloy - Determination of Nickel Content -
Flame Atomic Absorption Spectrometric Method
(ISO 4940-1985, Steel and Cast Iron - Determination of Nickel Content - Flame
Atomic Absorption Spectrometric Method, MOD)
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 ... 6
1 Scope ... 7
2 Normative References ... 7
3 Terms and Definitions ... 8
4 Principle ... 8
5 Reagents or Materials ... 8
6 Instruments and Equipment ... 9
7 Sample ... 11
8 Test Procedures ... 11
9 Result Expression ... 16
10 Test Report ... 17
Appendix A (informative) Constituent Documents of GB/T 223 ... 18
Appendix B (normative) Measurement Steps of Instrument Indicators ... 24
Appendix C (informative) Additional Information of Precision Test ... 27
Appendix D (informative) Graphical Representation of Precision Data ... 29
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 document is Part 54 of GB/T 223. The parts of GB/T 223 that have been issued are shown
in Appendix A.
This document serves as a replacement of GB/T 223.54-1987 Methods for Chemical Analysis
of Iron, Steel and Alloy - The Flame Atomic Absorption Spectrophotometric Method for the
Determination of Nickel Content. In comparison with GB/T 223.54-1987, apart from structural
adjustments and editorial modifications, the main technical changes are as follows:
---The scope of determination is modified (see Chapter 1; the Scope of Version 1987);
---Normative References is added (see Chapter 2);
---The amount of specimen is modified (see 8.1; 4.1 of Version 1987);
---The amount of acid used when the specimen is decomposed is reduced (see 8.3.1; 4.3.1
of Version 1987);
---The preparation of the calibration solution is modified (see 8.3.2; 4.4 of Version 1987);
---The stipulations on the determination of wavelength by the atomic absorption
spectrometer are modified (see 8.3.3 and 8.3.4; 4.4.3 of Version 1987);
---The adjustment of the atomic absorption spectrometer is added (see 8.3.3);
---The optimization of the atomic absorption device is added (see 8.3.4);
---Spectral measurement is added (see 8.3.5);
---The drawing of calibration curve is added (see 8.4);
---The calculation formula of nickel content is modified (see 9.1; Chapter 5 of Version
1987);
---The precision requirements of the method are modified (see 9.2; Chapter 6 of Version
1987);
---Appendix B is added.
This document modifies and adopts ISO 4940-1985 Steel and Cast Iron - Determination of
Nickel Content - Flame Atomic Absorption Spectrometric Method.
In comparison with ISO 4940-1985, this document makes the following structural adjustments:
---The Chapter “Terms and Definitions” is added (see Chapter 3);
---Chapter 4 corresponds to Chapter 3 of ISO 4940-1985;
---Chapter 5 corresponds to Chapter 4 of ISO 4940-1985, in which, 5.1 ~ 5.3, and 5.6
respectively correspond to 4.1 ~ 4.3 and 4.4 of ISO 4940-1985, 5.4 corresponds to 7.3.2
of ISO 4940-1985, and 5.5 is added;
---Chapter 6 corresponds to Chapter 5 of ISO 4940-1985;
---Chapter 7 corresponds to Chapter 6 of ISO 4940-1985;
---Chapter 8 corresponds to Chapter 7 of ISO 4940-1985;
---Chapter 9 corresponds to Chapter 8 of ISO 4940-1985;
---Chapter 10 corresponds to Chapter 9 of ISO 4940-1985;
---Appendix A and Appendix B are added, Appendix C corresponds to Appendix A of ISO
4940-1985, and Appendix D corresponds to Appendix B of ISO 4940-1985.
The technical differences between this document and ISO 4940-1985 are marked with a vertical
single line () in the outer margin of the clauses involved. These technical differences and the
reasons for these differences are as follows:
---The scope of determination is expanded (see Chapter 1), so as to enhance the
applicability of this document;
---Normative References is modified (see Chapter 2), so as to adapt to the technical
documents of China;
---Iron solutions of two concentrations are used (see 5.4 and 5.5), so as to adapt to the
requirements of different amounts of specimen;
---The detection limit (see 6.1.3) is modified, so as to be compatible with the determination
range of this document;
---The amount of specimen is modified (see 8.1), so as to simplify the operating process;
---The amount of acid used when the specimen is decomposed is reduced (see 8.3.1), so as
to satisfy the demands of environmental protection;
---The preparation of the calibration solution is modified (see 8.3.2.3), so as to satisfy the
demands of the expansion of the detection range;
---The description of instrument optimization in the high concentration section is added
(see 8.3.4), so as to satisfy the accuracy requirements for the measurement;
Iron, Steel and Alloy - Determination of Nickel Content -
Flame Atomic Absorption Spectrometric 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 nickel content in steel and cast
iron by the flame atomic absorption spectrometric method.
This document is applicable to the determination of nickel content with a mass fraction of
0.002% ~ 5.0%.
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 6379.1-2004, ISO 5725-1:1994, IDT)
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 6379.2-2004, ISO 5725-2:1994, IDT)
GB/T 12805 Laboratory Glassware - Burettes (GB/T 12805-2011, ISO 385:2005, NEQ)
GB/T 12806 Laboratory Glassware - One-mark Volumetric Flasks (GB/T 12806-2011, ISO
1042:1998, NEQ)
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 (GB/T 20066-2006, ISO 14284:1996, IDT)
min, so that the white perchloric acid fumes maintain a steady reflux on the wall of the beaker.
Cool it, add 100 mL of water, and heat to dissolve the salts. After cooling, transfer it to a 250
mL one-mark volumetric flask, use water to dilute to the mark and mix it well.
5.5 Iron Solution, 8 mg/mL
Weigh-take 2 g 0.01 g of pure iron (see 5.1), put it into an 800 mL beaker, add 100 mL of
hydrochloric acid - nitric acid mixed acid (see 5.2) and use a watch glass to cover it; heat it,
until it is completely dissolved. Then, add 80 mL of perchloric acid (ρ about 1.67 g/mL),
evaporate it, until white perchloric acid fumes are emitted. Let it continue to emit fumes for 1
min, so that the white perchloric acid fumes maintain a steady reflux on the wall of the beaker.
Cool it, add 100 mL of water, and heat to dissolve the salts. After cooling, transfer it to a 250
mL one-mark volumetric flask, use water to dilute to the mark and mix it well.
5.6 Nickel Standard Solution
5.6.1 Nickel stock solution, 1,000 g/mL
Weigh-take 0.5000 g of pure nickel (with a mass fraction not less than 99.9%), accurate to
0.0001 g, place it in a 250 mL beaker, add 25 mL of nitric acid (ρ about 1.42 g/mL, diluted to 1
+ 1). After heating to dissolve it, boil it to remove nitrogen oxides. After cooling to room
temperature, transfer it to a 500 mL one-mark volumetric flask, use water to dilute to the mark
and mix it well.
1 mL of this stock solution contains 1,000 g of nickel.
5.6.2 Nickel standard solution, 40 g/mL
Weigh-take 10.0 mL of the nickel stock solution (5.6.1) and put it in a 250 mL one-mark
volumetric flask. Use water to dilute to the mark and mix it well.
1 mL of this standard solution contains 40 g of nickel.
Prepare it right before use.
6 Instruments and Equipment
6.1 Atomic Absorption Spectrometer
6.1.1 General requirements
Configure a nickel hollow cathode lamp; the supply air and acetylene shall be sufficiently pure,
and free of water, oil and nickel, so as to provide a stable and clear lean-burn flame.
After the atomic absorption spectrometer used is optimized in accordance with 8.3.4, the
detection limit and characteristic concentration shall be consistent with the parameters provided
by the instrument manufacturer and satisfy the indicators in 6.1.2 ~ 6.1.4; the instrument shall
also reach the additional performance requirements provided in 6.1.5.
To establish a standard method for flame atomic absorption spectrometry, the working group
shall determine the value of the instrument indicators in accordance with the inter-laboratory
measurement results.
6.1.2 Lowest precision (in accordance with B.1 of Appendix B)
Use the calibration solution of the highest concentration, measure the absorbance for 10 times
and calculate its standard deviation. The standard deviation shall not exceed 1.0% of the mean
absorbance.
Use the calibration solution of the lowest concentration (not the zero-concentration calibration
solution), measure the absorbance for 10 times and calculate its standard deviation. This
standard deviation shall not exceed 0.5% of the mean absorbance of the calibration solution of
the highest concentration.
6.1.3 Detection limit (in accordance with B.2)
The detection limit is defined as the concentration corresponding to 4.65 times the standard
deviation of the 10 absorbance measurements of the analytical element in solution at a
concentration level slightly above the zero-calibration solution.
In a solution similar to the final specimen solution matrix, the detection limit of nickel shall be
less than 0.06 g/mL.
6.1.4 Linearity of calibration curve (in accordance with B.3)
When using the same method for the determination, the ratio of the slope value of the upper
20% concentration range of the calibration curve (expressed as a change in absorbance) to the
slope value of the lower 20% concentration range (expressed as a change in absorbance) shall
not be less than 0.7.
For instruments that are automatically calibrated with 2 or more standard samples, before the
analysis, the obtained absorbance readings shall be used to establish a calibration curve whose
linearity satisfies the above-mentioned requirements.
6.1.5 Characteristic concentration (in accordance with B.4)
In a solution consistent with the matrix of the final specimen solution, for a wavelength of 232.0
nm, the characteristic concentration of nickel shall be less than 0.10 g/mL; for a wavelength
of 352.5 nm, the characteristic concentration of nickel shall be less than 0.60 g/mL.
6.2 Auxiliary Device
It is recommended to use a suitable recorder or digital reading device to evaluate the indicators
in 6.1.2 ~ 6.1.4 and to conduct the subsequent measurements.
In accordance with the expected nickel content, in the order of increasing concentration,
successively spray the corresponding series of calibration solutions (see 8.3.2.1, 8.3.2.2 or
8.3.2.3) into the flame; measure the absorbance of each calibration solution for 2 ~ 3 times to
obtain the average absorbance of each calibration solution. It shall be noted that a constant
sample injection rate shall be maintained during the determination of the calibration solution.
After each measurement, water shall be sprayed to clean the burner.
Under the same conditions, successively measure the absorbance of the blank test solution and
the test solution at least twice to obtain the average absorbance of the blank test solution and
the test solution.
During the determination of batches of specimens, at regular intervals, the calibration solution
of intermediate concentration shall be sprayed into for inspection. If the results show loss of
absorbance or precision due to clogging, the burner shall be cleaned.
Make sure to thoroughly rinse the atomizing system and drain system after using perchloric
acid.
8.4 Drawing of Calibration Curve
For each measurement series and range of nickel content to be measured, a new calibration
curve shall be drawn.
Before drawing the curve, the concentration of the zero-calibration solution of the calibration
curve shall be determined. If the zero-calibration solution has significant absorption, then, in
accordance with Formula (1), calculate the nickel concentration (ρNi,z) in the zero-calibration
solution:
Where,
ρNi,z---the nickel concentration after adding the first calibration solution, expressed in (g/mL);
AZ---the absorbance of the zero-calibration solution;
ANi,C1---the absorbance of the first calibration solution.
Add the calibrated nickel concentration (ρNi,z) in the zero-calibration solution to the
concentration of each calibration solution, and make the calibration curve pass through the
origin of coordinates.
Take the average absorbance value of each calibration solution to draw against the nickel
content (g/mL) to establish a calibration curve.
Alternatively, the instrument data processing software that comes with the instrument may also
be used to subtract the absorbance of the zero-calibration solution from the absorbance of each
......
GB 223.54-87
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
UDC 669.14/.15.543.06
Methods for chemical analysis of iron, steel and alloy -
The flame atomic absorption spectrophotometric
method for the determination of nickel content
APPROVED ON. APRIL 03, 1987
IMPLEMENTED ON. MARCH 01, 1988
Approved by. Ministry of Metallurgical Industry
Table of Contents
1 Method summary ... 3
2 Reagent ... 3
3 Instruments ... 4
4 Analytical procedures ... 5
5 Calculation of analysis results ... 6
6 Precision... 7
Additional information ... 8
Methods for chemical analysis of iron, steel and alloy -
The flame atomic absorption spectrophotometric
method for the determination of copper content
This standard applies to the determination of the amount of nickel in cast iron,
carbon steel, and low alloy steel. Measuring range is 0. 005% ~ 0. 50%.
This standard follows the requirements GB 1467-78 “Method for chemical
analysis of metallurgy product - General rules and regulations”.
1 Method summary
The sample is decomposed with appropriate mixed acid, perchloric acid is
added to evaporate it to produce smoke, AND water is used to dissolve the salt.
The sample solution is sprayed into the air-acetylene flame, and the copper
hollow cathode lamp is used as the light source. The atomic absorption
spectrophotometer is used to measure the absorbance at the wavelength of
232.0nm.
To eliminate matrix effects, when drawing the calibration curve, it shall add the
iron the amount of which is similar to that of the sample solution.
2 Reagent
2.1 Perchloric acid (ρ1.67g/ml).
2.2 Hydrochloric acid-nitric acid mixture. MIX three parts of hydrochloric acid
(ρ1.19g/ml), one part of nitric acid (ρ1.42g/ml), and two parts of water together;
PREPARE it before use.
2.3 Nitric acid-perchloric acid mixture. MIX 100ml of nitric acid (ρ1.42g/ml) with
800 ml of perchloric acid (2.1); USE water to dilute it to 1l; MIX it uniformly.
2.4 Pure iron solution. WEIGH 10g of pure iron (nickel content less than
0.0005%); PLACE it into a 800ml beaker; ADD 100ml of hydrochloric acid-nitric
acid mixture (2.2); HEAT to fully dissolve it; ADD 120ml of perchloric acid (2.1);
EVAPORATE it until the perchloric acid produces white smoke; KEEP 1min;
COOL it down; ADD 100ml of water; HEAT to dissolve the salts; after cooling it
down, TRANSFER it into a 250ml volumetric flask; USE water to dilute it to the
mark; MIX it uniformly.
2.5 Nickel standard solution
2.5.1 WEIGH 1.0000g of metallic nickel (< 99.9%); PLACE it into a 250ml
beaker; ADD 50ml of nitric acid (1 + 1); HEAT to dissolve it; COOL it to room
temperature; TRANSFER it into a 1000ml volumetric flask; USE water to dilute
it to the mark; MIX it uniformly. AND 1ml of this solution contains 1.0mg of
nickel.
2.5.2 PIPETTE 10.00ml of nickel standard solution (2.5.1); PLACE it into a
100ml volumetric flask; USE water to dilute it to the mark; MIX it uniformly.
AND 1ml of this solution contains 100µg of nickel.
3 Instruments
Atomic absorption spectrophotometer, equipped with air-acetylene burner and
copper hollow cathode lamp. Air and acetylene shall be pure enough
(containing no water, oil, or copper) to provide a stable and clear lean flame.
The atomic absorption spectrophotometer used shall reach the following
indicators.
3.1 The minimum precision requirements. The calibration solution of the
highest concentration is used for absorbance measurements for 10 times,
AND the standard deviation shall not exceed 1.0% of the average absorbance.
The calibration solution of the smallest concentration (not zero calibration
solution) is used for absorbance measurements for 10 times, AND its standard
deviation shall not exceed 0.5% of the average absorbance of the calibration
solution of the highest concentration.
3.2 Characteristic concentration. The characteristic concentration of nickel in a
solution having a similar matrix with that of the final measurement sample
solution shall be less than 0.10μg of nickel/ml (at wavelength 232.0nm).
3.3 Detection limit. The detection limit of nickel in a solution having a similar
matrix with that of the final measurement sample solution shall be less than
0.15μg of nickel/ml (at wavelength 232.0nm).
3.4 Linearity of calibration curves. The ratio of the slope of the upper 20%
concentration range of the calibration curve (expressed as the change in
absorbance) to the slope of the lower 20% concentration range shall be not
less than 0.7.
4 Analytical procedures
4.1 Sample amount
WEIGH 1.0000g of sample.
4.2 Blank test
MAKE blank test together with the sample.
4.3 Determination
4.3.1 PLACE the sample (4.1) into a 400ml beaker; ADD 15ml of nitric
acid-perchloric acid mixture (2.3); COVER the watch glass; HEAT to dissolve it
at low temperature; EVAPORATE it until the perchloric acid produces white
smoke; MAINTAIN it for 1min; COOL it down; ADD 15ml of water; slightly
HEAT it until the salt is dissolved; CCOL it to room temperature; TRANSFER it
into a 100ml volumetric flask; USE water to dilute it to the mark; MIX it
uniformly. If there is precipitation of graphite, silicate, tungstic acid, and so on
from the sample solution, it shall be filtered at dry state.
Note.
1. As for the sample which is hard to be dissolved in nitric acid-perchloric acid
mixture (2.3), it may first use hydrochloric acid-nitric acid (2.2) to dissolve it;
then ADD 12ml of perchloric acid (2.1); EVAPORATE it until the smoke is
produced; MAINTAIN it for 1 min; FOLLOW the corresponding procedures in
4.3.1.
2. If the sample solution containing more than 1.0% of nickel, then it requires
dilution; PIPETTE 20ml of sample solution (4.3.1) and PLACE it into a 100ml
volumetric flask; USE water to dilute it to the mark; MIX it uniformly. USE the
same method to dilute the blank solution.
4.3.2 PLACE the sample solution in the atomic absorption spectrophotometer
at a wavelength of 232.0nm; USE the air-acetylene flame; USE water to adjust
it to zero; MEASURE its absorbance. Combining with the sample solution
absorbance and the absorbance of the blank solution accompanied with the
sample, FIND the concentration of nickel (μg/ml) from the calibration curve.
4.4 Calibration curve drawing
4.4.1 Nickel content less than 0.10%
In eight 100ml volumetric flasks, respectively ADD 25ml of pure iron solution
(2.4), then respectively ADD 0.00, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00, 10.00
nickel standard solution (2.5.1); USE water to dilute it to the mark; MIX it
uniformly.
4.4.2 Nickel content 0.10% ~ 0.50%
In seven 100ml volumetric flasks, respectively ADD 5ml of pure iron solution
(2.4), then respectively ADD 0.00, 1.00, 2.00, 4.00, 6.00, 8.00, 10.00 nickel
standard solution (2.5.1); USE water to dilute it to the mark; MIX it uniformly.
4.4.3 At the atomic absorption spectrophotometer at a wavelength of 232.0 nm,
USE the air-acetylene flame; USE water to adjust zero; MEASURE the
absorbance of the solution (4.4.1) or (4.4.2).
The absorbance of each solution of the calibration curve series minus the
absorbance of the zero concentration solution is the net absorbance of the
nickel calibration curve series solutions. The nickel concentration is used as
the abscissa AND the net absorbance as the ordinate, to draw the calibration
curve.
5 Calculation of analysis results
CALCULATE the percentage of nickel by the following formula.
Where.
c2 - Concentration of nickel in the sample solution as found from the
calibration curve, μg/ml;
c1 - Concentration of nickel in the accompanied sample blank solution as
found from the calibration curve, μg/ml;
f - Dilution factor, f = 1 when the nickel content of the sample is less than or
equal to 0.10%; AND f = 5 if the nickel content of the sample is more than
0.10%;
V - Volume of the test sample solution, ml;
m0 - Sample amount, g.
6 Precision
Precision table
degree, % (m/m) Repeatability, r Reproducibility, R
0.005 ~ 0.50 lgr = -1.5732 + 0.6021lgm lgR = -1.1569 + 0.6799lgm
Repeatability is the maximum difference of two independent test results of the
same sample at the 95% probability level under normal and correct operating
conditions using this method by the same operator in the same laboratory
using the same instrument in a short period of time.
Reproducibility is the maximum difference of the two independent test results
of the same sample at 95% probability level under normal and correct
operating conditions using this method by two operators in different
laboratories.
If the difference between two independent test results exceeds the
corresponding value of repeatability and reproducibility, the two results are
considered suspect.
Additional information
This standard shall be under the jurisdiction of the Ministry of Metallurgical
Industry Research Institute of Iron and Steel Technology.
This standard was responsibly drafted by the Iron and Steel Research Institute
of the Ministry of Metallurgical Industry.
This standard was drafted by the Iron and Steel Research Institute.
The main drafters of this standard. Xie Ronghou, Xing Rugang.
This standard’s level marking. GB 223.54-87 I.
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