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GB/T 6730.61-2005 English PDF (GBT6730.61-2005)

GB/T 6730.61-2005 English PDF (GBT6730.61-2005)

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GB/T 6730.61-2005: Iron ores -- Determination of carbon and sulfur content -- High frequency combustion with infrared absorption method

This Standard specifies the determination of carbon and sulfur content in iron ores by high frequency combustion with infrared absorption method. This Standard applies to the determination of carbon and sulfur content in natural iron ores, iron concentrates, sinter, pellets and their products. Determination range (mass fraction): carbon 0.01%~2.5%, sulfur 0.001%~2.0%.
GB/T 6730.61-2005
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 73.060.10
D 31
Iron ores - Determination of carbon and sulfur content
- High frequency combustion with infrared absorption
method
ISSUED ON: JULY 21, 2005
IMPLEMENTED ON: JANUARY 01, 2006
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method summary ... 5
4 Reagents and materials ... 5
5 Apparatus ... 6
6 Sampling and sample preparation ... 7
7 Analytical procedures ... 8
8 Calculation of analysis results ... 10
9 Test report ... 13
Appendix A (Normative) Flow chart for acceptance procedure of sample
analysis value ... 15
Appendix B (Informative) Derivation of repeatability and tolerance equations16 Appendix C (Informative) Precision data graph obtained from joint analysis test ... 17
Iron ores - Determination of carbon and sulfur content
- High frequency combustion with infrared absorption
method
WARNING: The personnel using this Standard shall have practical
experience in regular laboratory work. This Standard does not point out all possible safety problems. It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with
the conditions stipulated by relevant national regulations.
1 Scope
This Standard specifies the determination of carbon and sulfur content in iron ores by high frequency combustion with infrared absorption method.
This Standard applies to the determination of carbon and sulfur content in natural iron ores, iron concentrates, sinter, pellets and their products. Determination range (mass fraction): carbon 0.01%~2.5%, sulfur 0.001%~2.0%. 2 Normative references
The following documents contain provisions which, through reference in this Standard, constitute provisions of this Standard. For the dated references, their subsequent amendments (excluding corrections) or revisions do not apply to this Standard. However, the parties who enter into agreement based on this Standard are encouraged to investigate whether the latest editions of these documents are applicable. For undated reference documents, the latest
editions apply to this Standard.
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 6682 Water for laboratory use - Specifications (GB/T 6682-1992, neq ISO 3697:1987)
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)
Note: USE a non-magnetic material to thoroughly mix the samples; USE a non-magnetic spatula to take samples from the entire container by increment sample.
7 Analytical procedures
WARNING: During the analysis, prevent burns and discharge the oxygen
emitted from the combustion of the sample to the outside of the laboratory, to prevent excessive local oxygen concentrations from catching fire.
Carry out high-frequency shielding to effectively avoid radiation danger. 7.1 Number of determinations
According to Appendix A, the same predried sample shall be determined at least twice independently.
Note: ?€?Independent?€? means that the results of the second and any subsequent determinations are not affected by the result of previous determination. In this analytical method, this condition means that the same operator repeats the determination at different times or by different operators, including the use of appropriate recalibration.
7.2 Sample size
WEIGH 0.400 g of sample, accurate to 0.001 g. When the method of 7.6.2 is adopted for analysis, the weighing quantity shall be consistent with that of iron ore standard sample as much as possible.
7.3 Blank test
Along with the sample analysis, do a blank test. According to the sample analysis method, add 1.3 g of pure iron flux (4.6), a tin tube (4.12), and 1.9 g of tungsten particles (4.3). Perform at least three blank tests.
7.4 Preparation of carbon and sulfur standard series
7.4.1 Preparation of carbon standard series
According to Table 2, weigh barium carbonate (4.7), accurate to 0.0002 g; PLACE it in a crucible (5.3) that has been burned and covered with 0.9 g of pure iron flux (4.6); ADD one flattened and folded tin tube (4.12); then cover with 0.4 g of pure iron flux (4.6) and 1.9 g of tungsten particles (4.3) as the carbon standard series.
working state. Determine the best analysis conditions.
7.5.2 COMPLETE the blank calibration; subtract the blank from the subsequent sample measurement.
7.6 Calibration
7.6.1 USE the prepared carbon and sulfur standard series for
simultaneous calibration or separate calibration
Within the measurement range, select a suitable content of standard sample to measure at least three times; perform system linear adjustment. Then, measure the prepared carbon and sulfur standard series; CHECK the linear relationship after calibration; if necessary, further calibrate the working curve.
Note: When preparing a series of standard samples, the content may be appropriately adjusted according to the carbon and sulfur content of the sample to be tested. 7.6.2 USE carbon and sulfur iron ore standard sample for calibration
According to the carbon and sulfur content of the sample to be tested, select three standard samples of the same type of iron ore (The carbon and sulfur content of the sample to be tested is within the range of the carbon and sulfur content of the three standard samples) and measure sequentially. If the measurement result is within the tolerance, confirm the linearity of the system; otherwise re-adjust the linearity of the system. According to the carbon and sulfur content, adjust the standard sample size, so that the weighing quantity of the sample and of the standard sample are as consistent as possible.
7.7 Sample analysis
According to 7.2, weigh the sample; PLACE it in a crucible (5.3) that has been burned and covered with 0.9 g of pure iron flux (4.6); add 1 tin tube (4.12) or 0.2 g of tin particles (4.4); then cover with 0.4 g of pure iron flux (4.6) and 1.9 g of tungsten particles (4.3). USE the same conditions, procedures, and
operations as the measurement of standard samples to measure.
8 Calculation of analysis results
8.1 Measurement of carbon and sulfur content
According to the relationship between the absorption energy and the
concentration of carbon and sulfur, the content of carbon and sulfur is obtained from the calibration curve.
The analysis results of the elements to be tested shall be within the content Rd - Tolerance (repeatability) for repeated measurements in the laboratory; P - Tolerance between laboratories.
8.2.2 Determination of analysis results
According to the procedure in Appendix A, according to formula (1), calculate the independent repeated measurement results. Compare with the repeated measurement tolerance (Rd), to determine the analysis results.
8.2.3 Interlaboratory precision
Interlaboratory precision is used to evaluate the consistency between the final results reported by two laboratories. After the two laboratories report the results in accordance with the same procedures specified in 8.2.2, calculate:
Where:
??1 - The final result reported by laboratory 1;
??2 - The final result reported by laboratory 2;
??12 - The average of the final results.
If |??1-??2|???P (see 8.2.1), the final results are consistent.
8.2.4 Acceptance of analysis values
Acceptance of analysis values is verified using certified standard samples. The procedures are the same as described above. After confirming the precision, the final laboratory result is compared with the standard value Ac. If: a) |??c-Ac|???C, there is no significant difference between the measured value and the standard value;
b) |??c-Ac|>C, there is significant difference between the measured value and the standard value.
Where:
??c - Measured value of standard sample;
Ac - Standard value of standard sample;

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