GB/T 6730.63-2024 PDF English
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Iron ores - Determination of aluminum, calcium, magnesium, manganese, phosphorus, silicon and titanium content - Inductively coupled plasma atomic emission spectrometric method
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| GB/T 6730.63-2006 | English | 230 |
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Iron ores -- Determination of aluminum calcium magnesium manganese phosphorus silicon and titanium content -- Inductively coupled plasma atomic emission spectrometric method
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GB/T 6730.63-2024: PDF in English (GBT 6730.63-2024) GB/T 6730.63-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.10
CCS D 31
Replacing GB/T 6730.63-2006
Iron ores - Determination of aluminum, calcium,
magnesium, manganese, phosphorus, silicon and titanium
content - Inductively coupled plasma atomic emission
spectrometric method
(ISO 11535:2006, Iron ores - Determination of various elements - Inductively coupled
plasma atomic emission spectrometric method, MOD)
ISSUED ON: MAY 28, 2024
IMPLEMENTED ON: DECEMBER 01, 2024
Issued by: State Administration for Market Regulation;
National Standardization Administration.
Table of Contents
Foreword ... 3
Introduction ... 6
1 Scope ... 7
2 Normative references ... 7
3 Terms and definitions ... 8
4 Principle ... 8
5 Reagents and materials ... 8
6 Instruments and equipment ... 11
7 Sampling and specimen preparation ... 12
8 Analytical procedures ... 12
9 Calculation of results ... 15
10 Test report ... 21
Appendix A (Informative) Components of GB/T 6730 ... 22
Appendix B (Informative) Comparison of structure numbers of this document with ISO
11535:2006 ... 27
Appendix C (Informative) Recommended solution concentrations for calibration curves
... 28
Appendix D (Normative) Performance test of plasma spectrometer ... 29
Appendix E (Informative) Derivation of repeatability and allowable deviation equations
... 32
Appendix F (Normative) Acceptance procedure for specimen analysis result ... 33
Iron ores - Determination of aluminum, calcium,
magnesium, manganese, phosphorus, silicon and titanium
content - Inductively coupled plasma atomic emission
spectrometric method
Warning - Personnel using this document shall have formal laboratory work
experience. This document does not point out all possible safety issues. Users are
responsible for taking appropriate safety and health measures and ensuring that
the conditions stipulated by relevant national laws and regulations are met.
1 Scope
This document specifies the determination of aluminum, calcium, magnesium,
manganese, phosphorus, silicon, titanium content by inductively coupled plasma
emission spectrometry.
This document is applicable to the determination of the following elements in natural
iron ore, iron concentrate, sintered ore, pelletized ore. The determination range is as
shown in Table 1.
2 Normative references
The contents of the following documents constitute the essential terms of this document
through normative references in the text. Among them, for dated references, only the
version corresponding to that date applies to this document; for undated references, the
5.5 Hydrochloric acid, 1 + 1.
5.6 Standard storage solution
5.6.1 Phosphorus standard storage solution, 1000 μg/mL.
Weigh 4.3936 g of standard potassium dihydrogen phosphate, which was dried at
110 °C into a 400 mL beaker. Add 200 mL of water. Transfer to a 1000 mL volumetric
flask after complete dissolution. Use water to dilute it to the mark. Mix well.
5.6.2 Manganese standard stock solution, 1000 μg/mL.
Weigh 1.0000 g of metallic manganese [w (Mn) > 99.9% (mass fraction)] with surface
oxide removed into a 250 mL beaker. Add 20 mL of hydrochloric acid (5.5). Heat until
completely dissolved. Cool to room temperature. Transfer to a 1000 mL volumetric
flask. Use water to dilute it to the mark. Mix well.
5.6.3 Magnesium standard stock solution, 1000 μg/mL.
Weigh 1.6582 g of magnesium oxide [w (MgO) > 99.9% (mass fraction)], that has been
calcined at 850 °C for 30 min and cooled to room temperature, in a desiccator. Place it
in a 250 mL beaker. Add 20 mL of hydrochloric acid (5.5). Heat to dissolve completely.
Cool to room temperature. Transfer to a 1000 mL volumetric flask. Use water to dilute
it to the mark. Mix well.
5.6.4 Silicon standard stock solution, 1000 μg/mL.
Weigh 2.1393 g of silicon dioxide [w (SiO2) > 99.9% (mass fraction)], that has been
calcined at 1000 °C for 45 min and cooled to room temperature, in a desiccator. Place
it in a platinum crucible with 5 g of anhydrous sodium carbonate. Mix well. Melt in a
high-temperature furnace at 1000 °C for 15 min. Use 100 mL of warm water to heat
and dissolve the molten material in a polytetrafluoroethylene beaker. Cool to room
temperature. Transfer to a 1000 mL volumetric flask. Use water to dilute it to the mark.
Mix well. Store in a polyethylene bottle.
5.6.5 Aluminum standard storage solution, 1000 μg/mL.
Weigh 1.0000 g of metallic aluminum [w (Al) > 99.99% (mass fraction)]. Place it in a
250 mL polytetrafluoroethylene beaker. Add 25 mL of sodium hydroxide solution (200
g/L). Heat and dissolve completely. Neutralize with hydrochloric acid (5.5) and add 20
mL in excess. Boil until the solution is clear. Cool to room temperature. Transfer to a
1000 mL volumetric flask. Use water to dilute it to the mark. Mix well.
5.6.6 Titanium standard storage solution, 1000 μg/mL.
Weigh 1.0000 g of high-purity titanium metal [w (Ti) > 99.95% (mass fraction)] in a
400 mL beaker. Add 100 mL of sulfuric acid (1 + 9). Cover with a watch glass. Heat to
dissolve. After complete dissolution, add a few drops of hydrogen peroxide to oxidize
and boil to decompose excess hydrogen peroxide. Cool to room temperature. Transfer
to a 1000 mL volumetric flask. Use sulfuric acid (1 + 9) to dilute it to the mark. Mix
well.
5.6.7 Calcium standard storage solution, 1000 μg/mL.
Weigh 2.4972 g of calcium carbonate [w (CaCO3) > 99.99% (mass fraction)], which
was dried to a constant amount at 110 °C, in a 250 mL beaker. Cover with a watch glass.
Slowly add 20 mL of hydrochloric acid (5.5). Heat until complete dissolution. Boil to
drive out carbon dioxide. Cool to room temperature. Transfer to a 1000 mL volumetric
flask. Use water to dilute it to the mark. Mix well.
Note 1: To facilitate the preparation of calibration curve solutions, the 1000 μg/mL standard
stock solutions of aluminum, calcium, magnesium, manganese, phosphorus, silicon, titanium
are diluted to 100 μg/mL standard solutions for preparation.
Note 2: It is allowed to directly use the certified standard solutions of the same acidity medium
as standard stock solutions.
5.7 Calibration and reference solutions
The calibration solution is the solution required for drawing the calibration curve of the
analyzed elements. Its concentration range in the solution is expressed in micrograms
per milliliter, which depends on the performance parameters and linear sensitivity of
the instrument. At least 10 solutions are required to cover the measurement range (mass
fraction) shown in Table 1. For specimens with a narrow measurement range (mass
fraction), the calibration solution shall include the effective area. If the element
concentration in the solution exceeds 5000 × the detection limit (DL), an additional
calibration curve must be drawn to include this range.
In the case of nonlinearity, use the sub-sensitive line or use appropriately diluted
specimen solution and calibration solution.
Note: For the recommended spectral lines shown in Table 2, the calibration solution prepared
according to the recommended method in Appendix C is consistent with the performance test
value.
In order to meet the requirement of similarity between the specimen and the calibration
solution, the calibration solution must be added with the corresponding amount of iron,
flux, acid. For each calibration solution, follow the steps recommended in 8.4.1; use the
iron oxide (5.1) equivalent to the amount of iron in the specimen to replace the sample.
Before the final dilution to 200 mL, add the standard solution and hydrochloric acid
(5.5) required for the concentration of the calibration solution, to obtain a relatively
consistent final acid concentration (40 mL 1+1 diluted hydrochloric acid).
In order to meet the consistency of the test, the same bottle of reagent shall be used
For each operation, a certified reference material/sample of the same type of ore shall
be analyzed in parallel with the specimen under the same conditions and a blank test
shall be performed. The pre-dried specimen of the certified reference material/sample
shall be prepared as specified in 7.2.
For the blank test, the same amount of iron oxide (5.1) as the specimen shall be used
instead of the specimen.
The certified reference material/sample and the sample should be of the same type; the
properties of the two substances shall be sufficiently similar to ensure that no significant
changes occur during the analysis. When a certified reference material/sample is not
available, other standard samples may be used.
When analyzing several specimens at the same time, if the analysis steps are the same
and the reagents used are from the same reagent bottle, a blank test can be performed.
When analyzing several ore specimens of the same type at the same time, a certified
standard substance/sample can be used.
8.4 Determination
8.4.1 Specimen decomposition
Pre-place 0.80 g of sodium carbonate (5.2) in a platinum or suitable platinum alloy
crucible (6.3). Place the specimen (8.2) in the crucible. Use a platinum wire or stainless
steel wire to mix thoroughly. Add 0.40 g of sodium tetraborate (5.3) and mix again. Pre-
melt the mixture to make it uniform.
Pre-melting can be performed using a gas torch or a high-temperature furnace with a
metal holder for manual stirring. First, make the crucible temperature reach 350 °C ~
400 °C (slightly dark red flame color); heat the mixture for 2 min ~ 3 min. Pre-melt
until there is no bubbling. Perform high-temperature melting within 5 min. Raise the
temperature of the high-temperature furnace to 800 °C ~ 900 °C, until the mixture is
completely melted.
After pre-melting, place the crucible in a high-temperature furnace at 1020 °C and melt
for 15 minutes. Take out the crucible and gently rotate it to solidify the melt. Cool it.
Put the stirring magnet (6.7) into the crucible. Place the crucible in a 250 mL beaker.
Add 40 mL of hydrochloric acid (5.5) and 30 mL of water (add appropriate amount of
water for high-silicon specimens) into the crucible. Cover with a watch glass. Heat
while stirring on a magnetic stirrer hot plate. Keep the temperature of the leaching
solution at about 70 °C, until the melt is completely dissolved. Take out the crucible
and the stirring magnet. Rinse it clean with water. After the solution cools, immediately
pipette it to a 200 mL single-scale volumetric flask. Use water to dilute to the mark.
Mix well.
Note 1: It is acceptable to use manual stirring instead of a magnetic stirrer.
Note 2: Immediately pipette the leaching solution to a 200 mL volumetric flask; add water to
nearly the scale to avoid precipitation.
Note 3: It is recommended to dilute to 200 mL, so that the element concentration in the solution
is consistent with the performance test number specified in Table 3. High concentration test
solutions may also need to be diluted again, to meet the linear response of the instrument in the
high concentration range. In this case, the calibration solution shall also be diluted
simultaneously, with the same dilution ratio as the test solution.
Note 4: If the instrument is consistent with the performance test value, it is not necessary to use
an internal standard (such as yttrium or scandium) to improve performance.
8.4.2 Spectrometer adjustment
8.4.2.1 General requirements
The ICP spectrometer shall first be initially adjusted, according to the manufacturer's
recommendations and laboratory quantitative analysis operations.
8.4.2.2 Performance test
The purpose of the performance test is to evaluate the performance parameters of the
ICP spectrometer, so that all models of spectrometers can be operated under equal
conditions so that the data generated can be compared.
The test is based on the determination of the following three parameters:
- Detection limit (DL);
- Background equivalent concentration (BEC);
- Short-term precision (RSDNmin).
Calculate according to the definitions and formulas in Appendix D.
Try to optimize the instrument parameters in each round as much as possible. If
necessary, perform the instrument operation as many times as possible, until the value
obtained is lower than the value in Table 3. When the element concentration in the
specimen solution is higher than 5000 × DL, RSDN is the only performance parameter
that needs to be evaluated; the measured value shall be lower than the RSDNmin value
in Table 3.
Xi - Element (analyte) content (mass fraction), expressed in %;
m - Sample mass, in grams (g);
ρ1 - Analyte concentration in specimen solution, in micrograms per milliliter
(μg/mL);
ρ0 - Analyte concentration in blank test solution, in micrograms per milliliter
(μg/mL);
Wj - Mass fraction of interfering element in specimen, %;
Iij - Spectral interference coefficient of interfering element (j) on specimen analyte
(i), equivalent to the mass fraction of analyte when the interfering element is 1%,
in %;
V - Final volume of calibration and test solution (recommended 200 mL, see 7.4),
in milliliters (mL).
Overcorrection of spectral interference is undesirable. The maximum allowable
correction value is approximately 10 times the repeatability error of the analyte content
in the verification. If the correction value is greater than this number, the correction is
not applicable to ICP analysis.
Note 1: If there is no element interference, the mass fraction Wj of the interfering element
included in formula (2) is equal to zero.
Note 2: When the recommended final calibration solution volume V = 200 mL and there are no
interfering elements, formula (2) can be simplified to:
9.3 Standardization of calibration curve (drift correction)
The regular inspection and correction of the calibration curve shall be carried out as
follows:
Take two calibration solutions, namely the one with the lowest and highest analyte
content.
In the drawn calibration curve, the intensities of the two calibration solutions are
measured; the correction coefficients α and β are calculated according to formulas (4)
and (5).
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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