Search result: GB/T 21114-2019 (GB/T 21114-2007 Older version)
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Refractories - Chemical analysis by X-ray fluorescence (XRF) - Fused cast-bead method
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GB/T 21114-2019
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| GB/T 21114-2007 | English | 360 |
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Chemical analysis of refractory products by XRF -- Fused cast bead method
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| Standard ID | GB/T 21114-2019 (GB/T21114-2019) | | Description (Translated English) | Refractories -- Chemical analysis by X-ray fluorescence (XRF) -- Fused cast-bead method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | Q40 | | Classification of International Standard | 81.080 | | Word Count Estimation | 74,726 | | Date of Issue | 2019-06-04 | | Date of Implementation | 2020-05-01 | | Older Standard (superseded by this standard) | GB/T 21114-2007 | | Quoted Standard | GB/T 3286.8; GB/T 4513.2; GB/T 6005; GB/T 6900; GB/T 10325; GB/T 15000.7; GB/T 17617 | | Adopted Standard | ISO 12677-2011, MOD | | Drafting Organization | Baoshan Iron and Steel Co., Ltd., Sinosteel Group Luoyang Refractory Research Institute Co., Ltd., Jiangsu Province Ceramic Refractory Product Quality Supervision and Inspection Center, Zhejiang Zili High Temperature Technology Co., Ltd., Zhejiang Zili New Materials Co., Ltd. | | Administrative Organization | National Technical Committee for Standardization of Refractories (SAC/TC 193) | | Proposing organization | National Technical Committee for Standardization of Refractories (SAC/TC 193) | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | | Summary | This standard specifies the chemical analysis methods for refractory materials and ceramics composed of oxides. The samples are prepared by the method of fused and cast glass sheets, and the X-ray fluorescence spectrum (hereinafter referred to as XRF) is determined. This standard applies to the types of materials listed in Chapter 3, and other types of refractory materials can be used for reference. |
GB/T 21114-2019
Refractories - Chemical analysis by X-ray fluorescence (XRF) - Fused cast-bead method
ICS 81.080
Q40
National Standards of People's Republic of China
Replace GB/T 21114-2007
Refractory X-ray fluorescence spectrochemical analysis
Cast glass method
[ISO 12677.2011, Chemicalanalysisofrefractoryproductsby
X-rayfluorescence (XRF)-Fusedcast-beadmethod, MOD]
Published on.2019-06-04
2020-05-01 implementation
State market supervision and administration
China National Standardization Administration issued
Content
Foreword I
1 range 1
2 Normative references 1
3 material type 1
4 Principle 2
5 device 2
6 sample preparation 3
7 Determination of ignition loss (and/or dry) 3
8 flux 3
9 melt casting procedure 4
10 calibration 6
11 correction 13
12 Reproducibility and repeatability 15
13 Accuracy measured with certified standard samples 16
14 Definition of detection limits 17
15 Test report 17
Appendix A (Normative) Calibration Range and Detection Limit 19
Appendix B (Normative) Correction of Tungsten Carbide Grinding Medium
Appendix C (informative) Flux and dilution ratio 26
Appendix D (Normative Appendix) Example of Certified Standard Sample (CRM) for Verification of Synthetic Calibration 27
Appendix E (Normative Appendix) Example of Series Standard Sample (SeRM) 33
Appendix F (Normative Appendix) Theoretical Calculation Equation 39
Appendix G (Normative) Certified Standard Sample (CRM) 40
Appendix H (Normative) Correction method for compensating for coexistence component interference when calibrating with SeRM 43
Appendix I (Normative) Standard deviations obtained using certified standard samples 64
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 21114-2007 "Refractory X-ray fluorescence spectrochemical analysis of molten cast glass sheet method", and
Compared with GB/T 21114-2007, the main technical changes are as follows.
--- Revised scope (see Chapter 1, Chapter 1 of the.2007 edition);
--- Revised the canonical reference document (see Chapter 2, Chapter 2 of the.2007 edition);
--- Added the relevant content of the mechanical mixer (see 5.8);
--- The amount of impurity 3D/R in the flux was changed to D/3R (see 8.1.9, 8.1.9 of the.2007 edition);
---Form m (1
) changed to m (
100-wL
) (see 9.1.3, version 9.2.3 of.2007);
--- Added provisions for the addition of other components to the calibration sample (see 10.2.1);
--- Increased the calibration range and detection limit of the phosphorus pentoxide component (see Table A.1, Table A.2);
--- Added some standard samples (see Table D.8, Table D.17 in Appendix D);
--- Added Table I.16, Table I.17, Table I.18 (see Appendix I).
This standard uses the redrafting method to modify the use of ISO 12677.2011 "refractory products X-ray fluorescence spectrochemical analysis (XRF) melting
Cast Glass Method.
The technical differences between this standard and ISO 12677.2011 and their reasons are as follows.
--- Amend the scope of application to "This standard applies to the types of materials listed in Chapter 3, other refractory types can be used for reference",
To adapt to the technical conditions of our country;
---About the normative reference documents, this standard has made technical adjustments to adapt to China's technical conditions, adjustments
The situation is reflected in Chapter 2, “Regulatory Citations”, and the specific adjustments are as follows.
● Add references to GB/T 3286.8, GB/T 4513.2, GB/T 6900, GB/T 10325, GB/T 15000.7,
GB/T 17617;
● Replace ISO 565 with GB/T 6005 modified to international standards;
● Remove ISO Guide 35.2006, ISO 26845;
--- Will be applied to laboratory samples in paragraph 1 of Chapter 6, and "Note 1. Large sampling is outside the scope of this method, but
Found in ISO 26845. "Change to "collect laboratory samples according to GB/T 10325, GB/T 17617 and GB/T 4513.2",
To adapt to the technical conditions of our country;
--- Revised the chapter number of Chapter 9 to adapt to the technical conditions of our country;
--- Supplemented in 10.2.1. high-purity reagent ammonium dihydrogen phosphate and potassium dihydrogen phosphate for convenient use;
---In Table A, Table A.1, Table A.2 adds the calibration range and detection limit of the phosphorus pentoxide component for ease of use;
--- Added the relevant content of domestic standard samples in Appendix D for ease of use;
--- Added the contents of the domestic standard series of refractory materials in Appendix E for ease of use;
--- According to the results of the joint test, the allowable difference of iron oxide in Appendix G has been appropriately modified to adapt to the technical conditions of China;
--- Appendix I added the use of domestic series of standard sample melt repeatability results for ease of use.
This standard has made the following editorial changes.
--- Modified the standard name;
--- Increased in 10.4.2.2 "Note. Other calibration equations can also be used";
--- Added some flux and melt ratio content in Appendix C;
--- Add in Appendix F "Base correction alpha coefficient can be calculated according to the software provided by the manufacturer";
--- Add in Appendix H "can use the calibration method provided by the manufacturer";
--- Removed references.
Please note that some of the contents of this document may involve patents. The issuing organization of this document is not responsible for identifying these patents.
This standard is proposed and managed by the National Technical Committee for Refractory Standardization (SAC/TC193).
This standard was drafted. Baoshan Iron and Steel Co., Ltd., Sinosteel Luoyang Refractory Materials Research Institute, Jiangsu Ceramics
Fire Materials Product Quality Supervision and Inspection Center, Zhejiang Zili High Temperature Technology Co., Ltd., Zhejiang Zi Li New Materials Co., Ltd.
The main drafters of this standard. Lu Xiaoming, Li Heshan, Zhang Xiang, Zhang Yi, Cao Haijie, Zhu Huiliang, Yu Yan, Zhu Dongdong, Xu Xiaoying, Ma Xufeng,
Gao Jianrong, Dai Qianyun, Chen Qin, Chen Yaosheng.
The previous versions of the standards replaced by this standard are.
---GB/T 21114-2007.
Refractory X-ray fluorescence spectrochemical analysis
Cast glass method
1 Scope
This standard specifies the chemical analysis method of refractory materials and ceramics composed of oxides.
Light spectrum (hereinafter referred to as XRF) was measured.
This standard applies to the types of materials listed in Chapter 3. Other refractory types can be used as reference.
Note 1. When the content of certain elements in the sample exceeds a certain amount, such as tin, copper, zinc and chromium, melting will be difficult, in which case refer to the corresponding literature.
Note 2. For all components with a mass fraction greater than 99% (dry basis), if all the trace components present and the ignition loss have been determined, the difference is obtained by subtraction.
Values can also be verified by direct measurements.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
Methods for chemical analysis of limestone and dolphins - Part 8
GB/T 4513.2 Unshaped refractories - Part 2. Sampling (GB/T 4513.2-2017, ISO 1927-2.2012, IDT)
Basic dimensions of GB/T 6005 test sieve wire mesh, perforated plate and electroformed sheet mesh (GB/T 6005-
2008, ISO 565.1990, MOD)
GB/T 6900 Aluminum-silicon refractory chemical analysis method
GB/T 10325 Shaped Refractory Products Acceptance Sampling Inspection Rules (GB/T 10325-2012, ISO 5022.1979, NEQ)
GB/T 15000.7 Standard Sample Working Guidelines (7) General Requirements for Standard Sample Producer Capabilities (GB/T 15000.7-2012,
ISO Guide 34.2009, IDT)
GB/T 17617 Refractory raw materials sampling inspection rules (GB/T 17617-2018, ISO 8656-1. 1988, MOD)
3 material type
The various types of refractory materials analyzed using this standard are listed below. Appendix I lists the repeatability and reproducibility of some materials.
The data can be used as a reference for the first time using this standard.
a) High aluminum (the mass fraction of Al2O3 is greater than 45%)
b) Aluminosilicate (Al2O3 mass fraction is 7%~45%)
c) siliceous (mass fraction of SiO2 is greater than 93%)
d) zircon
e) Zirconia and zirconate
f) Magnesium
g) Magnesium aluminum spinel (~70/30)
h) Dolomite
i) Limestone
j) Magnesium oxide/chromium oxide
......
GB/T 21114–2007
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 81.080
Q 40
Chemical analysis of refractory products by XRF -
fused cast bead method
(ISO 12677. 2003, MOD)
ISSUED ON. SEPTEMBER 01, 2007
IMPLEMENTED ON. FEBRUARY 01, 2008
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine of the People’s Republic of China;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Types of materials ... 5
4 Principle ... 6
5 Sample preparation ... 6
6 Apparatus ... 7
7 Loss on ignition (and/or drying) ... 8
8 Flux ... 8
9 Fusion casting procedures ... 10
10 Calibration ... 13
11 Corrections ... 23
12 Reproducibility and repeatability ... 26
13 Accuracy as measured using certified reference materials ... 28
14 Definitions of limits of detection ... 29
15 Test report ... 30
Annex A (Normative) Calibration range and required detection limits ... 31
Annex B (Normative) Corrections for tungsten carbide grinding media ... 39
Annex C (Informative) Fluxes/flux ratios ... 40
Annex D (Normative) Examples of CRM to be used to check synthetic
calibrations ... 42
Annex E (Normative) Examples of SeRM ... 50
Annex F (Normative) Equation for theoretical calculations ... 59
Annex G (Normative) Certified reference materials (CRMs)... 60
Annex H (Normative) Method of interference correction used to compensate
for the effects of co-existing components when using SeRM for calibration
... 64
Annex I (Informative) Standard deviations achieved with certified reference
materials ... 94
Foreword
This Standard modifies and adopts ISO IM77.2003 Chemical Analysis of Refractory Products
by XRF - Fused Cast Bead Method (English version). The relevant technical differences
between this Standard and ISO 12677.. 2003 are marked with single vertical line at the page
margin of the involved clause. The main revised contents are as follows.
a) Change the quoted standard to Chinese standards that are equivalent to ISO standards;
b) Replace “Massive sampling does not belong to the scope of this method.” in the first
paragraph of Chapter 5 to be “The laboratory sample shall be collected in accordance
with GB/T 10325 and GB/T 17617”.
c) Add “high purity reagents ammonium dihydrogen phosphate and potassium dihydrogen
phosphate ” to 10.2.1;
d) Add “Note. other calibration equation can be also used” to 10.4.2.2;
e) Add part of solvent and dilution ratio contents to Annex C;
f) In Annex C, for ease of understanding, add “Note. the number behind the material is the
sequence number of the listed material type in Chapter 3, for example, 1 is high
aluminum Al2O3>45%, 2 is alumina-silica Al2O3 7%~45%, ..., 17 is magnesium
silicate” corresponding to the contents of Chapter 3.
g) In Annex D, add the contents of standard samples for the domestic refractory products;
h) In Annex E, add the contents of series standard samples for the domestic refractory
products;
i) In Annex F, add “the matrix correction coefficient a can be calculated according to the
software provided by the instrument supplier”;
j) Appropriately modify the permissible error of ferric oxide in Annex G according to the
joint test results;
k) In Annex H, add “Note. the correction method provided by the manufacturer can be
used”;
l) In Annex I, add the application of fusion representation results for the domestic series
standard samples;
m) Change the notes under the titles in 12. 9 and Annex A into the paragraphs according to
our expression habit;
n) Delete the references.
In addition, editorially modify the places that need to be corrected in ISO 12677.2003; and
add the footnotes at the corresponding places.
Annexes A, B, D, E, F, G and H of this Standard are normative; Annexes C and I are
Chemical analysis of refractory products by XRF –
fused cast bead method
1 Scope
This Standard specifies a method for chemical analysis of refractory products and materials,
and technical ceramics composed of oxides, including the determination of oxide at levels
between 0.01% and 99% by means of the XRF fused cast bead method.
NOTE. Constituents at concentrations greater than 99% (on a dried basis) should be reported on by
difference, provided that all likely minor constituents and any loss on ignition have been determined. These
figures should also be checked by direct determination.
2 Normative references
The articles contained in the following documents have become part of this Standard when
they are quoted herein. For the dated documents so quoted, all the modifications (excluding
corrections) or revisions made thereafter shall not be applicable to this Standard. For the
undated documents so quoted, the latest editions shall be applicable to this Standard.
GB/T 3286 Methods for chemical analysis of limestone and dolomite
GB/T 6005 Test sieves - Metal wire cloth perforated metal plate and electroformed sheet
- Nominal sizes of openings (GB/T 6005-1997, eqv ISO 565. 1990)
GB/T 6900 Chemical analysis of alumina-silica refractories
GB/T 8170 Rules of rounding off for numerical values & expression and judgement of
limiting values
GB/T 10325 Shaped refractory products - Rule of acceptance, sampling and inspection
GB/T 15000.7-2001 Directives for the work of reference materials(7) - General
requirements for the competence of reference material producers (ISO Guide 34.2000,
IDT)
GB/T 17617 Refractory products - Sampling of raw materials and unshaped products
ISO/IEC Directives (1992) - Part 2. Methodology for the development of International
Standards - Annex B Mention of reference materials
3 Types of materials
1) High alumina (Al2O3)≥45%;
2) Alumino-silicate (Al2O3) 7% to 45%;
3) Silica (SiO2)≥93%;
4) Zircon;
5) Zirconia and zirconates;
6) Magnesia;
7) Magnesia/alumina spinel (~ 70/30);
8) Dolomite;
9) Limestone;
10) Magnesia/chromic oxide;
11) Chrome ore;
12) Chrome alumina;
13) Alumina/magnesia spinel (~ 70/30);
14) Zirconia-alumina-silica cast material (AZS);
15) Calcium silicates;
16) Calcium aluminates;
17) Magnesium silicates.
A list of elemental ranges and required detection limits are given in Annex A. Some of the
above material types can be accommodated on to common calibrations (see 10.3.4).
4 Principle
The powdered sample is fused with a suitable flux to destroy its mineralogical and particulate
composition. The resultant melt is casted into the shape of a glass bead which is then
introduced into an XRF spectrometer. The intensities of the fluorescent X-rays of the required
elements in the bead are measured and the chemical composition of the sample is analysed
by reference to previously determined calibration graphs or equations and applying
corrections for inter-element effects. The calibration equations and inter-element corrections
are established from beads produced using pure reagents and/or series reference materials
(SeRMs), prepared in the same way as the samples.
Because of the universality of the fused cast bead technique, various fluxes and modes of
calibration are permitted, providing they have been demonstrated to be able to meet certain
criteria of reproducibility, sensitivity and accuracy. Provided that a laboratory's own methods
conform to all the various criteria set down, they will be accepted as conforming to this
Standard.
5 Sample preparation
Bulk sampling a laboratory sample according to GB/T 10325 and GB/T 17617.
It is permissible to apply the sample grinding methods cited in conventional chemical methods
for the classes of materials covered. In addition, the use of tungsten carbide is permitted and
is the preferred method, provided that the appropriate corrections for tungsten carbide (and
its binder if necessary) are applied to loss on ignition and analysis figures.
Corrections for tungsten carbide (and ...
......
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