Iron ores—Determination of calcium,silicon,manganese,titanium,phosphorus magnesium,aluminium and barium content—Wavelength dispersive X-ray fluorescence spectrometric method
ICS 73.060.10
D 31
National Standard of the People's Republic of China
GB/T 6730.62-2005
Iron ores - Determination of calcium, silicon, manganese, titanium, phosphorus, magnesium, aluminium and barium content - Wavelength dispersive X-ray fluorescence spectrometric method
鐵礦石 鈣、硅、鎂、鈦、磷、錳、鋁和鋇
含量的測定 波長色散X射線熒光光譜法
(English Translation)
Issue date: 2005-07-21 Implementation date: 2006-01-01
Issued by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
the Standardization Administration of the People's Republic of China
Foreword
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard is developed with reference to ISO 9516:1992 Iron ores - Determination of silicon, calcium, manganese, aluminium, titanium, magnesium, phosphorus, sulfur and potassium - Wavelength dispersive X-ray fluorescence spectrometric method.
With respect to ISO 9516:1992, the main differences are as follows:
a) In the "Scope" of ISO 9516:1992, nine elements are determined (Fe is the reference). In this standard, eight elements are determined, with sulfur and potassium removed, and barium added;
b) In ISO 9516:1992, α coefficient method is used. In this standard, the self-consistent correction coefficient method is used for determining the correction coefficient;
c) In ISO 9516:1992, specimen pretreatment is not included. In this standard, the loss on ignition of the specimen is accurately measured, and the ignited specimen is used for preparing the fuse specimen;
d) In Clause 7 of this standard "Preparation of fuse specimen", in order to make the composition of the specimen the same as that of the standard S specimen, the content of potassium shall be supplemented.
Annex A, Annex B and Annex C to this standard are normative, while Annex D is informative.
This standard was proposed by China Iron and Steel Association.
This standard is under the jurisdiction of China Metallurgical industrial Information and Standardization Institute.
Iron ores - Determination of calcium, silicon, manganese, titanium, phosphorus, magnesium, aluminium and barium content - Wavelength dispersive X-ray fluorescence spectrometric method
Warning – Persons using this standard shall be familiar with normal laboratory practice. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies a method for determining the content of calcium, silicon, manganese, titanium, phosphorus, magnesium, aluminium and barium in iron ores by wavelength dispersive X-ray fluorescence spectrometer.
This standard is applicable to the determination of the content of the eight elements listed in Table 1 in iron ores and artificial rich ores. See Table 1 for the determination range (mass fraction) of each element.
Table 1 Determination range of each element
Element Determination range (mass fraction)/%
Ca 0.02~15.00
Si 0.08~15.00
Mg 0.15~5.00
Ti 0.004~8.00
P 0.005~5.00
Mn 0.009~3.00
Al 0.02~5.00
Ba 0.02~3.00
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments (excluding corrections) to, or revisions, of any of these publications do not apply. However, parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition applies.
GB/T 6379 Precision of test methods; Determination of repeatability and reproducibility for a standard test method by interlaboratory tests (GB/T 6379-1986, neq ISO 5725:1986)
GB/T 6730.1 Methods for chemical analysis of iron ores - Preparation of predried test samples for chemical analysis (GB/T 6730.1-1986, eqv ISO 7764:1985)
GB/T 10322.1 Iron ores - Sampling and sample preparation procedures (GB/T 10322.1-2000, idt ISO 3082:1998)
JJG 810-1993 Wavelength dispersive X-Ray fluorescence spectrometers
3 Principle
Prepare the specimen into borate glass fuse specimen, and determine the X-ray fluorescence intensity of the elements to be determined. The background is determined at the analytical spectral line of the blank fuse specimen and subtracted as the specimen background. The calibration fuse specimen is synthesized by pure chemical reagent, and the inter-element matrix effect is corrected by self-consistent correction principle.
4 Reagents and materials
Unless otherwise specified, only approved analytical reagents shall be used for analysis.
4.1 Ferric oxide (Fe2O3), guaranteed reagent.
It is ignited at 1,000°C for at least 1 h, and then cooled in a desiccator.
4.2 Silicon dioxide (SiO2), guaranteed reagent.
It is heated to 1,000°C, ignited for at least 1 h, and then cooled in a desiccator.
4.3 Calcium carbonate (CaCO3), guaranteed reagent.
It is dried at 105°C for 1 h and then cooled in a desiccator.
4.4 Magnesium oxide (MgO), guaranteed reagent.
It is ignited at 1,000°C for 1 h, then cooled in a desiccator, and weigh immediately after being cooled down.
4.5 Aluminium oxide (Al2O3), guaranteed reagent, α-type.
It is ignited at 1,000°C for at least 2 h (if the aluminium oxide is not α-type, it shall be heated to 1,250 °C to convert to α-type) and then cooled in a desiccator.
4.6 Titanium dioxide (TiO2), guaranteed reagent.
It is ignited at 1,000°C for at least 1 h and then cooled in a desiccator.
4.7 Manganese oxide (Mn3O4), guaranteed reagent.
Manganese dioxide (MnO2) is ignited in a platinum crucible at 1,000°C for 24 h and then cooled. The resulting lump material is crushed into a fine powder, sintered at 550°C for 1 h and then cooled in a desiccator.
4.8 Potassium dihydrogen phosphate (KH2PO4), guaranteed reagent.
It is dried at 105°C for 1 h and then cooled in a desiccator.
4.9 Barium carbonate (BaCO3), guaranteed reagent.
It is dried at 105°C for 1 h and then cooled in a desiccator.
4.10 Potassium carbonate (K2CO3), guaranteed reagent.
It is dried at 105°C for 1 h and then cooled in a desiccator.
4.11 Sodium nitrate (NaNO3)
It is dried at 105°C for 1 h and then cooled in a desiccator.
4.12 Ammonium iodide (NH4I)
It does not require drying but shall be stored in a desiccator.
4.13 Desiccant
It shall be freshly regenerated, self-indicating silica gel.
4.14 Flux
The guaranteed reagent anhydrous lithium tetraborate (Li2B4O7), shall be ignited at 500°C for 4 h, then cooled in a desiccator and stored.
4.15 Synthetic calibration specimen (S)
Weigh the reagents by the proportion listed in Table 2, accurately to 0.0002 g, mix the reagents thoroughly in a large plastic container, break all agglomerates, then move into an agate mortar, grind and mix well. Transfer the powder to a platinum dish, put it in an electric furnace at room temperature, and slowly raise the furnace temperature to 950°C in not less than 1 h. Keep it at this temperature for 20 min, then take it out, cool it in a desiccator filled with silica gel, grind and mix well repeatedly, and then store it in a sealed container. Prepare two separate synthetic calibration specimens (on different days). The amount of reagents specified in Table 2 is for reference only, which can be more or less, but the proportion of each component must be kept unchanged.
Table 2 Composition of synthetic calibration specimen
Oxide Oxide content (mass fraction)/% Reagent amount/g Quoted clause/subclause
Fe2O3 67.00 67.000 0 (Fe2O3) 4.1
SiO2 10.00 10.000 0(SiO2) 4.2
CaO 6.50 11.600 9(CaCO3) 4.3
MgO 5.00 5.000 0 (MgO) 4.4
Al2O3 5.00 5.000 0 (Al2O3) 4.5
TiO2 1.50 1.500 0 (TiO2) 4.6
Mn3O4 2.00 2.000 0 (Mn3O4) 4.7
P2O3 2.00 3.835 1 (KH2PO4) 4.8
BaO 1.00 1.287 (BaCO3) 4.9
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Apparatuses
6 Sampling and specimen
7 Preparation of fuse specimen
8 Analytical conditions and analytical procedures
9 Calculation of results
10 Test report
Annex A (Normative) Flow chart of specimen analytical value acceptance procedure
Annex B (Normative) Calculation of inter-element correction coefficient and unknown specimen content
Annex C (Normative) Standard deviation for specimen preparation
Annex D (Informative) Source program of "self-consistent calibration program"
