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GB/T 24198-2009 PDF English

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GB/T 24198-2009: Ferronickel - Determination of nickel silicon phosphorus manganese cobalt chromium and copper contents - Wavelength dispersive X-ray fluorescence spectrometry (Routine method)
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GB/T 24198-2009: Ferronickel - Determination of nickel silicon phosphorus manganese cobalt chromium and copper contents - Wavelength dispersive X-ray fluorescence spectrometry (Routine method)



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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.100 H 11 Ferronickel - Determination of nickel silicon phosphorus manganese cobalt chromium and copper contents - Wavelength dispersive X-ray fluorescence spectrometry (Routine method) Issued on. JULY 8, 2009 Implemented on. APRIL 1, 2010 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration Committee.

Table of Contents

Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Principle... 5 4 Reagents and materials... 5 5 Instrument and equipment... 6 6 Sampling and sample preparation... 7 7 Instrument preparation... 7 8 Analysis steps... 7 9 Calculation of results... 11 10 Precision... 11 11 Test report... 12 Annex A (Normative) Instrument precision test... 14 Annex B (Normative) Sample analysis value acceptance flow chart... 15

Foreword

Annex A and Annex B of this Standard are normative. This Standard was proposed by China Iron and Steel Industry Association. This Standard shall be under the jurisdiction of National Technical Committee on Pig Iron and Ferroalloy of Standardization Administration of China. Main drafting organization of this Standard. Jiuquan Iron and Steel (Group) Co., Ltd. Main drafters of this Standard. Zhu Weihua, Sun Yuguang, Wang Hao, Fu Baorong. Ferronickel - Determination of nickel silicon phosphorus manganese cobalt chromium and copper contents - Wavelength dispersive X-ray fluorescence spectrometry (Routine method) WARNING -- Personnel using this Standard should have formal laboratory work experience. This Standard does not indicate all possible security issues. It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with the conditions set forth in the relevant national regulations.

1 Scope

This Standard specifies the determination of nickel silicon phosphorus manganese cobalt chromium and copper contents by wavelength dispersive X-ray fluorescence spectrometry. It is applicable to the determination of electric furnace, induction furnace, converter and other as-cast conditions or nickel rolling. The range of each element is shown in Table 1.

2 Normative references

The provisions in following documents become the provisions of this Standard through reference in this Standard. For dated references, the subsequent amendments (excluding corrigendum) or revisions do not apply to this Standard, however, parties who reach an agreement based on this Standard are encouraged to study if the latest versions of these documents are applicable. For undated references, the latest edition of the referenced document applies. GB/T 4010, Ferroallys sampling and preparation of samples for chemical analysis GB/T 6379.1, Accuracy (trueness and precision) of measurement methods and results - Part 1.General principles and definitions (GB/T 6379.1-2004, ISO 5725-1.1994, IDT) GB/T 6379.2, Accuracy (trueness and precision) of measurement methods and results - Part 2.Basic method for the determination of repeatability and reproducibility of a standard measurement method (GB/T 6379.2-2004, ISO 5725-2.1994, IDT)

3 Principle

When the primary X-ray emitted from the X-ray tube is irradiated onto the surface of the flat, smooth sample, the resulting characteristic X-ray shall be crystallized by the crystal, and the detector shall measure the X-ray fluorescence intensity at the corresponding 2θ angle of the selected characteristic wavelength. The mass fraction of nickel, silicon, phosphorus,

4 Reagents and materials

4.1 P10 gas (90% argon and 10% methane mixed gas) for flow proportional counter. 4.2 Certified reference material or reference material Certified reference material (CRM) or reference material (RM).

5 Instrument and equipment

5.1 Sample preparation equipment Sample cutting equipment and sample surface polishing equipment. 5.2 X-ray fluorescence spectrometer The analytical accuracy and stability of the simultaneous or sequential wavelength dispersive spectrometer shall meet the requirements of Annex A. 5.2.4 Detector Scintillation counter for heavy element analysis; flow proportional counter for light element analysis. It can also use a sealed proportional counter. 5.2.5 Vacuum system During the measurement process, the vacuum system pressure is generally below 30 Pa and remains constant; for light elements, it shall be less than 20 Pa.

6 Sampling and sample preparation

Refer to the provisions of GB/T 20066 and GB/T 4010. The size of the sample shall depend on the geometry of the sample box. The analytical surface shall be able to cover all the sample box mask, while ensuring the sample thickness of at least 5 mm.

7 Instrument preparation

7.1 Instrument working environment The instrument working environment shall comply with GB/T 16597.

8 Analysis steps

8.1 Measurement conditions Select the appropriate measurement conditions, according to the type of equipment used, the type of sample, elements for analysis, coexisting elements and their content range. 8.2 Plotting and confirmation of calibration curve 8.2.1 Calibration curve plotting Under the selected working conditions, use X-ray fluorescence spectrometer to measure a series of certified reference material (CRM) or reference material (RM) of similar sample smelting process and similar chemical composition. Each sample shall be measured at least 2 times. 8.2.2 Confirmation of calibration curve accuracy According to the selected analysis conditions, use X-ray fluorescence spectrometer to measure certified reference material (CRM) or reference material (RM) of similar sample smelting process and of similar chemical composition. There shall be no statistically significant difference between the analyzed value of the element for analysis and the certified value or standard value Ac. Determine whether there are significant differences according to equation (3). 8.3 Analysis of unknown sample 8.3.1 Standardization of instrument Regularly confirm the analysis of standardized sample. When the instrument drifts, the instrument shall be drilled and calibrated by measuring the X-ray fluorescence intensity of the normalized sample.

9 Calculation of results

Calculate the contents of elements for analysis from the calibration curve, according to the fluorescence intensity measurement of unknown sample, by equation (8) or equation (9).

10 Precision

The precision of this Standard is the result of a common test conducted in 12 laboratories and determined according to GB/T 6379.1 and GB/T 6379.2.See Table 3 for precision.

11 Test report

The test report shall contain the following information. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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