GB/T 24585-2009 English PDF (GB/T24585-2009)

GB/T 24585-2009: Ferronickel - Determination of Phosphorus, Manganese, Chromium, Copper, Cobalt and Silicon Contents - Inductively Coupled Plasma Atomic Emission Spectrometric Method
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GB/T 24585-2009
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
H 11
Ferronickel – Determination of Phosphorus,
Manganese, Chromium, Copper, Cobalt
and Silicon Contents – Inductively Coupled
Plasma Atomic Emission Spectrometric Method
ISSUED ON: OCTOBER 30, 2009
IMPLEMENTED ON: MAY 01, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Principle ... 5
4 Reagents ... 5
5 Instrument ... 7
6 Sampling and Sample Preparation ... 9
7 Analysis Procedures ... 9
8 Calculation of Results ... 11
9 Precision ... 13
10 Expression of Analysis Results ... 13
11 Test Report ... 14
Appendix A (Normative) Performance Test for the Detection Limit (DL) and the
Background Equivalent Concentration (BEC) of the Inductively Coupled
Plasma Spectrometer ... 15
Appendix B (Normative) Standardization of Calibration Curve (Drift Correction)
... 18
Ferronickel – Determination of Phosphorus,
Manganese, Chromium, Copper, Cobalt
and Silicon Contents – Inductively Coupled
Plasma Atomic Emission Spectrometric Method
Warning: The personnel using this Standard shall have practical experience
working in the formal laboratory. This Standard does not point out all possible
safety issues. The user is responsible for taking appropriate safety and health
measures and ensuring compliance with the conditions stipulated by relevant
national laws and regulations.
1 Scope
This Standard specifies the use of inductively coupled plasma atomic emission
spectrometric method (ICP-AES) to determine the contents of phosphorus,
manganese, chromium, cobalt, copper and silicon.
This Standard is applicable to the determination of phosphorus, manganese,
chromium, cobalt, copper and silicon contents in ferronickel. The content ranges of the
determined elements are shown in Table 1.
The silicon measured by this method is acid-soluble silicon.
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
4.4 Nitric acid, ρ is about 1.42g/mL.
4.5 Nitric acid, 1+1.
4.6 Perchloric acid, ρ is about 1.61g/mL.
4.7 Hydrofluoric acid, ρ is about 1.14g/mL.
4.8 Standard stock solution
4.8.1 Phosphorus standard solution, 1000μg/mL
Take 4.3936g of reference dipotassium hydrogen phosphate dried at 105°C ~ 110°C;
dissolve it in an appropriate amount of water; transfer it into a 1000 mL volumetric flask;
dilute to the mark with water; and mix evenly. 1mL of this solution contains 1000μg of
phosphorus.
4.8.2 Manganese standard solution, 1000μg/mL
Take 1.0000g of electrolytic manganese (content is greater than 99.95%) in a 250mL
beaker; add 30mL of nitric acid (4.5); cover with a watch glass; heat to dissolve; boil to
expel the nitrogen oxides completely; cool to room temperature; and transfer it into the
1000mL volumetric flask; dilute to the mark with water and mix well. 1mL of this solution
contains 1000μg of manganese.
4.8.3 Chromium standard solution, 1000μg/mL
Take 2.8290g of benchmark potassium dichromate (content is greater than 99.95%)
that has been dried at 150°C ± 5°C in advance; and cooled to room temperature in a
250 mL beaker; dissolved in water; then transferred to a 1000 mL volumetric flask; and
diluted with water to the mark, mix evenly. 1 mL of this solution contains 1000μg of
chromium.
4.8.4 Cobalt standard solution, 1000μg/mL
Take 1.0000g of high-purity cobalt powder (content is greater than 99.9%) in a 600mL
beaker; then add 40mL of nitric acid (4.5); cover with a watch glass; heat it to
completely dissolve it; slightly boil to discharge nitrogen oxides; cool to room
temperature; transfer to a 1000 mL volumetric flask containing 160 mL of nitric acid
(4.5); dilute to the mark with water; and mix evenly. 1mL of this solution contains
1000μg of cobalt.
4.8.5 Copper standard solution, 1000μg/mL
Take 1.0000g of pure copper (content is greater than 99.9%) into a 300mL beaker; add
30mL of nitric acid (4.5); cover with a watch glass; heat at low temperature to
decompose it; cool to room temperature; and transfer it into a 1000ml volumetric flask;
The linearity of the calibration curve is checked by calculating the correlation coefficient,
which must be greater than 0.999.
6 Sampling and Sample Preparation
It shall be performed according to the provisions of GB/T 4010 and GB/T 20066.
7 Analysis Procedures
7.1 Amount of testing material
Take 0.50g of testing material, accurate to 0.0001g.
7.2 Blank test
Do a blank test with the testing material. The blank test shall use pure nickel (4.1) and
pure iron (4.2) equivalent to the amount of nickel and iron in the testing material to
replace the testing material.
7.3 Determination
7.3.1 Preparation of testing material solution
7.3.1.1 Place the testing material (7.1) in a 150mL conical flask; add 25mL of water,
10mL of nitric acid (4.4) and 4mL of hydrochloric acid (4.3); and keep the dissolved
volume of 40mL~50mL. Heat at low temperature to completely dissolve; cool to room
temperature; transfer to a 100mL volumetric flask; dilute with water to the mark; mix
evenly.
7.3.1.2 For testing materials with high carbon and high silicon that are difficult to
dissolve, place the testing material (7.1) in a polytetrafluoroethylene beaker; and add
10 mL of nitric acid (4.4), 4mL of hydrochloric acid (4.3) and 5mL of hydrofluoric acid
(4.7). Heat at low temperature until the violent reaction stops; add 5mL of perchloric
acid (4.6); continue to heat and smoke until reach the flowing wet salt; cool off slightly.
Add 10 mL of nitric acid (4.4) and 4 mL of hydrochloric acid (4.3); dissolve the salts;
cool to room temperature; transfer to a 100 mL volumetric flask; dilute to the mark with
water; and mix evenly. This solution measures elements other than silicon.
7.3.1.3 Filter all solutions with medium-speed filter paper; discard the first 2mL ~ 3mL
solution.
7.3.2 Preparation of calibration curve solution
Replace the testing material with pure nickel (4.1) and pure iron (4.2) equivalent to the
7.4.2.2 Measurement of test solution
After the calibration solution is measured, measure the test solution immediately; and
inhale the deionized water between each measurement. The measurement of the
certified standard sample solution is inserted in the interval. The test solution shall be
repeated for at least 2 times.
7.5 Correction of interference line in analysis line
First check the spectral interference of each coexisting element on the analysis line of
the measured element. In the case of spectral interference, calculate the spectral
interference correction coefficient according to 8.2, that is, the equivalent mass fraction
of the measured element when the mass fraction of coexisting elements is 1%.
7.6 Drawing of calibration curve
Do the linear regression with the net intensity as the Y-axis and the concentration of
the measured element (µg/mL) as the X-axis. The calculation of the correlation
coefficient shall meet the requirements of 5.1.6.
8 Calculation of Results
8.1 According to the calibration curve (7.6), the spectral intensity of the test solution is
calculated to the concentration of the corresponding element to be measured,
expressed in µg/mL.
The content of the measured element is calculated in terms of mass fraction wM; and
the value is expressed in %; it shall be calculated according to Formula (1):
Where:
m – mass of testing material, in g;
ρ1 – concentration of analysis element in the test solution, in µg/mL;
ρ0 – concentration of analysis element in the blank test solution, in µg/mL;
V – final volume of correction and test solution, in mL.
NOTE 1: If spectral interference is found, it shall be corrected in accordance with the provisions
of 8.2.
NOTE 2: If the analysis of the specimen is performed immediately after the calibration curve
Appendix A
(Normative)
Performance Test for the Detection Limit (DL) and the Background
Equivalent Concentration (BEC) of the Inductively Coupled Plasma
Spectrometer
A.1 Objective
The objective of the performance test given in this appendix is to use different types of
instruments to properly determine the performance of detection limit (DL) and the
background equivalent concentration (BEC) of the plasma spectrometer; allowing
different instruments to use different operating conditions, but the plasma spectrometer
may eventually produce consistent results.
The elements to be tested are shown in Table 3.
A.2 Definition
This Standard applies the following definitions.
A.2.1 Detection limit (DL): when the element produces a minimum concentration signal,
it may be considered to exceed any false background signal with a certain level; on
the other hand, the element concentration produces a signal that is 3 times the
standard deviation of the background level value.
A.2.2 Background equivalent concentration (BEC): It produces a net intensity equal to
the background intensity value, which is equivalent to the concentration of the analysis
element; it is a measure of sensitivity to a given wavelength.
A.3 Calibration solution
Three matrix solutions with the content of iron and nickel equivalent to the testing
material matrix, and calibration solutions with the concentration levels of all elements
to be tested are 0×DL (blank), 10×DL, and 1000×DL, shall be prepared.
The DL value of the calibration solution may be the laboratory value or the estimated
value given in Table 3.
A.4 Procedure
This procedure is used for the operation of each test element.
The plasma spectrometer shall be initially adjusted according to the manufacturer’s
GB/T 24585-2009
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
H 11
Ferronickel – Determination of Phosphorus,
Manganese, Chromium, Copper, Cobalt
and Silicon Contents – Inductively Coupled
Plasma Atomic Emission Spectrometric Method
ISSUED ON: OCTOBER 30, 2009
IMPLEMENTED ON: MAY 01, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Principle ... 5
4 Reagents ... 5
5 Instrument ... 7
6 Sampling and Sample Preparation ... 9
7 Analysis Procedures ... 9
8 Calculation of Results ... 11
9 Precision ... 13
10 Expression of Analysis Results ... 13
11 Test Report ... 14
Appendix A (Normative) Performance Test for the Detection Limit (DL) and the
Background Equivalent Concentration (BEC) of the Inductively Coupled
Plasma Spectrometer ... 15
Appendix B (Normative) Standardization of Calibration Curve (Drift Correction)
... 18
Ferronickel – Determination of Phosphorus,
Manganese, Chromium, Copper, Cobalt
and Silicon Contents – Inductively Coupled
Plasma Atomic Emission Spectrometric Method
Warning: The personnel using this Standard shall have practical experience
working in the formal laboratory. This Standard does not point out all possible
safety issues. The user is responsible for taking appropriate safety and health
measures and ensuring compliance with the conditions stipulated by relevant
national laws and regulations.
1 Scope
This Standard specifies the use of inductively coupled plasma atomic emission
spectrometric method (ICP-AES) to determine the contents of phosphorus,
manganese, chromium, cobalt, copper and silicon.
This Standard is applicable to the determination of phosphorus, manganese,
chromium, cobalt, copper and silicon contents in ferronickel. The content ranges of the
determined elements are shown in Table 1.
The silicon measured by this method is acid-soluble silicon.
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
4.4 Nitric acid, ρ is about 1.42g/mL.
4.5 Nitric acid, 1+1.
4.6 Perchloric acid, ρ is about 1.61g/mL.
4.7 Hydrofluoric acid, ρ is about 1.14g/mL.
4.8 Standard stock solution
4.8.1 Phosphorus standard solution, 1000μg/mL
Take 4.3936g of reference dipotassium hydrogen phosphate dried at 105°C ~ 110°C;
dissolve it in an appropriate amount of water; transfer it into a 1000 mL volumetric flask;
dilute to the mark with water; and mix evenly. 1mL of this solution contains 1000μg of
phosphorus.
4.8.2 Manganese standard solution, 1000μg/mL
Take 1.0000g of electrolytic manganese (content is greater than 99.95%) in a 250mL
beaker; add 30mL of nitric acid (4.5); cover with a watch glass; heat to dissolve; boil to
expel the nitrogen oxides completely; cool to room temperature; and transfer it into the
1000mL volumetric flask; dilute to the mark with water and mix well. 1mL of this solution
contains 1000μg of manganese.
4.8.3 Chromium standard solution, 1000μg/mL
Take 2.8290g of benchmark potassium dichromate (content is greater than 99.95%)
that has been dried at 150°C ± 5°C in advance; and cooled to room temperature in a
250 mL beaker; dissolved in water; then transferred to a 1000 mL volumetric flask; and
diluted with water to the mark, mix evenly. 1 mL of this solution contains 1000μg of
chromium.
4.8.4 Cobalt standard solution, 1000μg/mL
Take 1.0000g of high-purity cobalt powder (content is greater than 99.9%) in a 600mL
beaker; then add 40mL of nitric acid (4.5); cover with a watch glass; heat it to
completely dissolve it; slightly boil to discharge nitrogen oxides; cool to room
temperature; transfer to a 1000 mL volumetric flask containing 160 mL of nitric aci...