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GB/T 21114-2007 PDF in English

GB/T 21114-2007 (GB/T21114-2007, GBT 21114-2007, GBT21114-2007)
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GB/T 21114-2007: PDF in English (GBT 21114-2007)

GB/T 21114–2007
ICS 81.080
Q 40
Chemical analysis of refractory products by XRF -
fused cast bead method
(ISO 12677. 2003, MOD)
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
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 
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;
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
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
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,
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
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 ...
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.