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GB/T 24198-2009 English PDF (GBT24198-2009)
GB/T 24198-2009 English PDF (GBT24198-2009)
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GB/T 24198-2009: Ferronickel -- Determination of nickel, silicon, phosphorus, manganese, cobalt, chromium, and copper contents -- Wavelength dispersive X-ray fluorescence spectrometry (Routine method)
GB/T 24198-2009
GB
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
H 11
Ferronickel - Determination of nickel silicon phosphorus
manganese cobalt chromium and copper contents -
Wavelength dispersive X-ray fluorescence spectrometry
(Routine method)
ISSUED ON. JULY 8, 2009
IMPLEMENTED ON. APRIL 1, 2010
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration Committee.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle... 5
4 Reagents and materials ... 5
5 Instrument and equipment ... 6
6 Sampling and sample preparation ... 7
7 Instrument preparation ... 7
8 Analysis steps ... 7
9 Calculation of results ... 11
10 Precision ... 11
11 Test report ... 12
Annex A (Normative) Instrument precision test ... 14
Annex B (Normative) Sample analysis value acceptance flow chart ... 15
Foreword
Annex A and Annex B of this Standard are normative.
This Standard was proposed by China Iron and Steel Industry Association.
This Standard shall be under the jurisdiction of National Technical Committee
on Pig Iron and Ferroalloy of Standardization Administration of China.
Main drafting organization of this Standard. Jiuquan Iron and Steel (Group)
Co., Ltd.
Main drafters of this Standard. Zhu Weihua, Sun Yuguang, Wang Hao, Fu
Baorong.
Ferronickel - Determination of nickel silicon phosphorus
manganese cobalt chromium and copper contents -
Wavelength dispersive X-ray fluorescence spectrometry
(Routine method)
WARNING -- Personnel using this Standard should have formal
laboratory work experience. This Standard does not indicate all
possible security issues. It is the responsibility of the user to take
appropriate safety and health measures and to ensure compliance with
the conditions set forth in the relevant national regulations.
1 Scope
This Standard specifies the determination of nickel silicon phosphorus
manganese cobalt chromium and copper contents by wavelength dispersive
X-ray fluorescence spectrometry.
It is applicable to the determination of electric furnace, induction furnace,
converter and other as-cast conditions or nickel rolling. The range of each
element is shown in Table 1.
Table 1 -- Elements and measurement range
Element for analysis Measurement range (mass fraction) / %
Ni 12.0 ~ 60.0
Si 0.10 ~ 2.0
P 0.01 ~ 0.15
Mn 0.05 ~ 0.50
Co 0.30 ~ 1.00
Cr 0.05 ~ 1.00
Cu 0.05 ~ 1.5
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 who reach an agreement based on this
Standard are encouraged to study if the latest versions of these documents
are applicable. For undated references, the latest edition of the referenced
6 Sampling and sample preparation
Refer to the provisions of GB/T 20066 and GB/T 4010.
The size of the sample shall depend on the geometry of the sample box. The
analytical surface shall be able to cover all the sample box mask, while
ensuring the sample thickness of at least 5 mm.
The sample surface shall be ground into a smooth analytical surface. When
grinding with a belt or grinding wheel, it shall choose the appropriate abrasive
to prevent abrasive contamination; the abrasive grain size shall be at least 60
#.
If the specimen is exposed to air for more than one day, the surface must be
re-ground before measurement.
7 Instrument preparation
7.1 Instrument working environment
The instrument working environment shall comply with GB/T 16597.
7.2 Instrument working conditions
The X-ray spectrometer shall optimize the operating conditions according to
the requirements of the instrument manufacturer before the measurement,
and preheat for at least 1 h before the measurement or until the instrument is
stable.
8 Analysis steps
8.1 Measurement conditions
Select the appropriate measurement conditions, according to the type of
equipment used, the type of sample, elements for analysis, coexisting
elements and their content range.
(1) The counting time of elements for analysis shall depend on the
amount of the quantified element and the analytical precision, 5 s ~ 60 s
in general.
(2) The count rate generally does not exceed the maximum count of the
counter used.
(3) The choice of light pipe voltage and current shall take into account the
where,
wi - reference value of i, an element for analysis in certified reference material
(CRM) or reference material (RM), in mass fraction, in %;
dj - comprehensive absorption correction coefficient;
αj - theoretical α coefficient;
lj - spectral overlap correction factor;
wj - content of coexisting element in certified reference material (CRM) or
reference material (RM), in mass fraction, in %;
Ii - X-ray fluorescence intensity of i, an element for analysis;
a, b, c - calibration curve constants.
8.2.2 Confirmation of calibration curve accuracy
According to the selected analysis conditions, use X-ray fluorescence
spectrometer to measure certified reference material (CRM) or reference
material (RM) of similar sample smelting process and of similar chemical
composition. There shall be no statistically significant difference between the
analyzed value of the element for analysis and the certified value or standard
value Ac. Determine whether there are significant differences according to
equation (3).
For reference material (RM) that only has one laboratory set value, it shall
use equation (3) to determine whether there is significant difference.
where,
µc - final analysis of the elements to be tested in certified reference material
(CRM) or reference material (RM);
σL - standard deviation between the laboratories determined by the joint test;
Il - initial strength of low content of standardized sample;
α, β - drift correction factor.
8.3.2 Standardization confirmation
For drifted and calibrated reference material for analysis (CRM or RM), the
confirmed analysis value shall comply with the provisions of 8.2.2 or within
the laboratory accreditation range.
8.3.3 Measurement of unknown sample
Use X-ray fluorescence spectrometer to measure the fluorescence intensity
of the analytical elements in the unknown sample, according to the working
conditions selected at 8.1. Each sample shall be measured at least 2 times.
9 Calculation of results
Calculate the contents of elements for analysis from the calibration curve,
according to the fluorescence intensity measurement of unknown sample, by
equation (8) or equation (9).
where,
wi - content of i, an element for analysis in the unknown sample, in mass
fraction, numerical value in %;
wj - content of j, a coexistence element in the unknown sample, in mass
fraction, numerical value in %;
Ii - X-ray fluorescence intensity of i, an element for analysis;
lj - spectral overlap correction factor;
αj - theoretical α coefficient;
dj - comprehensive absorption correction coefficient;
a, b, c - calibration curve constants of elements for analysis.
10 Precision
The precision of this Standard is the result of a common test conducted in 12
Get QUOTATION in 1-minute: Click GB/T 24198-2009
Historical versions: GB/T 24198-2009
Preview True-PDF (Reload/Scroll if blank)
GB/T 24198-2009: Ferronickel -- Determination of nickel, silicon, phosphorus, manganese, cobalt, chromium, and copper contents -- Wavelength dispersive X-ray fluorescence spectrometry (Routine method)
GB/T 24198-2009
GB
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.100
H 11
Ferronickel - Determination of nickel silicon phosphorus
manganese cobalt chromium and copper contents -
Wavelength dispersive X-ray fluorescence spectrometry
(Routine method)
ISSUED ON. JULY 8, 2009
IMPLEMENTED ON. APRIL 1, 2010
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration Committee.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle... 5
4 Reagents and materials ... 5
5 Instrument and equipment ... 6
6 Sampling and sample preparation ... 7
7 Instrument preparation ... 7
8 Analysis steps ... 7
9 Calculation of results ... 11
10 Precision ... 11
11 Test report ... 12
Annex A (Normative) Instrument precision test ... 14
Annex B (Normative) Sample analysis value acceptance flow chart ... 15
Foreword
Annex A and Annex B of this Standard are normative.
This Standard was proposed by China Iron and Steel Industry Association.
This Standard shall be under the jurisdiction of National Technical Committee
on Pig Iron and Ferroalloy of Standardization Administration of China.
Main drafting organization of this Standard. Jiuquan Iron and Steel (Group)
Co., Ltd.
Main drafters of this Standard. Zhu Weihua, Sun Yuguang, Wang Hao, Fu
Baorong.
Ferronickel - Determination of nickel silicon phosphorus
manganese cobalt chromium and copper contents -
Wavelength dispersive X-ray fluorescence spectrometry
(Routine method)
WARNING -- Personnel using this Standard should have formal
laboratory work experience. This Standard does not indicate all
possible security issues. It is the responsibility of the user to take
appropriate safety and health measures and to ensure compliance with
the conditions set forth in the relevant national regulations.
1 Scope
This Standard specifies the determination of nickel silicon phosphorus
manganese cobalt chromium and copper contents by wavelength dispersive
X-ray fluorescence spectrometry.
It is applicable to the determination of electric furnace, induction furnace,
converter and other as-cast conditions or nickel rolling. The range of each
element is shown in Table 1.
Table 1 -- Elements and measurement range
Element for analysis Measurement range (mass fraction) / %
Ni 12.0 ~ 60.0
Si 0.10 ~ 2.0
P 0.01 ~ 0.15
Mn 0.05 ~ 0.50
Co 0.30 ~ 1.00
Cr 0.05 ~ 1.00
Cu 0.05 ~ 1.5
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 who reach an agreement based on this
Standard are encouraged to study if the latest versions of these documents
are applicable. For undated references, the latest edition of the referenced
6 Sampling and sample preparation
Refer to the provisions of GB/T 20066 and GB/T 4010.
The size of the sample shall depend on the geometry of the sample box. The
analytical surface shall be able to cover all the sample box mask, while
ensuring the sample thickness of at least 5 mm.
The sample surface shall be ground into a smooth analytical surface. When
grinding with a belt or grinding wheel, it shall choose the appropriate abrasive
to prevent abrasive contamination; the abrasive grain size shall be at least 60
#.
If the specimen is exposed to air for more than one day, the surface must be
re-ground before measurement.
7 Instrument preparation
7.1 Instrument working environment
The instrument working environment shall comply with GB/T 16597.
7.2 Instrument working conditions
The X-ray spectrometer shall optimize the operating conditions according to
the requirements of the instrument manufacturer before the measurement,
and preheat for at least 1 h before the measurement or until the instrument is
stable.
8 Analysis steps
8.1 Measurement conditions
Select the appropriate measurement conditions, according to the type of
equipment used, the type of sample, elements for analysis, coexisting
elements and their content range.
(1) The counting time of elements for analysis shall depend on the
amount of the quantified element and the analytical precision, 5 s ~ 60 s
in general.
(2) The count rate generally does not exceed the maximum count of the
counter used.
(3) The choice of light pipe voltage and current shall take into account the
where,
wi - reference value of i, an element for analysis in certified reference material
(CRM) or reference material (RM), in mass fraction, in %;
dj - comprehensive absorption correction coefficient;
αj - theoretical α coefficient;
lj - spectral overlap correction factor;
wj - content of coexisting element in certified reference material (CRM) or
reference material (RM), in mass fraction, in %;
Ii - X-ray fluorescence intensity of i, an element for analysis;
a, b, c - calibration curve constants.
8.2.2 Confirmation of calibration curve accuracy
According to the selected analysis conditions, use X-ray fluorescence
spectrometer to measure certified reference material (CRM) or reference
material (RM) of similar sample smelting process and of similar chemical
composition. There shall be no statistically significant difference between the
analyzed value of the element for analysis and the certified value or standard
value Ac. Determine whether there are significant differences according to
equation (3).
For reference material (RM) that only has one laboratory set value, it shall
use equation (3) to determine whether there is significant difference.
where,
µc - final analysis of the elements to be tested in certified reference material
(CRM) or reference material (RM);
σL - standard deviation between the laboratories determined by the joint test;
Il - initial strength of low content of standardized sample;
α, β - drift correction factor.
8.3.2 Standardization confirmation
For drifted and calibrated reference material for analysis (CRM or RM), the
confirmed analysis value shall comply with the provisions of 8.2.2 or within
the laboratory accreditation range.
8.3.3 Measurement of unknown sample
Use X-ray fluorescence spectrometer to measure the fluorescence intensity
of the analytical elements in the unknown sample, according to the working
conditions selected at 8.1. Each sample shall be measured at least 2 times.
9 Calculation of results
Calculate the contents of elements for analysis from the calibration curve,
according to the fluorescence intensity measurement of unknown sample, by
equation (8) or equation (9).
where,
wi - content of i, an element for analysis in the unknown sample, in mass
fraction, numerical value in %;
wj - content of j, a coexistence element in the unknown sample, in mass
fraction, numerical value in %;
Ii - X-ray fluorescence intensity of i, an element for analysis;
lj - spectral overlap correction factor;
αj - theoretical α coefficient;
dj - comprehensive absorption correction coefficient;
a, b, c - calibration curve constants of elements for analysis.
10 Precision
The precision of this Standard is the result of a common test conducted in 12
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