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GB/T 24585-2009: Ferronickel - Determination of Phosphorus, Manganese, Chromium, Copper, Cobalt and Silicon Contents - Inductively Coupled Plasma Atomic Emission Spectrometric Method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 24585-2009: Ferronickel - Determination of Phosphorus, Manganese, Chromium, Copper, Cobalt and Silicon Contents - Inductively Coupled Plasma Atomic Emission Spectrometric Method---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT24585-2009 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.100 H 11 Ferronickel – Determination of Phosphorus, Manganese, Chromium, Copper, Cobalt and Silicon Contents – Inductively Coupled Plasma Atomic Emission Spectrometric Method Issued on. OCTOBER 30, 2009 Implemented on. MAY 01, 2010 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of PRC. Table of ContentsForeword... 3 1 Scope... 4 2 Normative References... 4 3 Principle... 5 4 Reagents... 5 5 Instrument... 7 6 Sampling and Sample Preparation... 9 7 Analysis Procedures... 9 8 Calculation of Results... 11 9 Precision... 13 10 Expression of Analysis Results... 13 11 Test Report... 14 Appendix A (Normative) Performance Test for the Detection Limit (DL) and the Background Equivalent Concentration (BEC) of the Inductively Coupled Plasma Spectrometer... 15 Appendix B (Normative) Standardization of Calibration Curve (Drift Correction) ... 18ForewordThe Appendixes A and B in 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 for Standardization of Pig Iron and Iron Alloy. Organizations responsible for drafting this Standard. Jiuquan Iron & Steel (Group) Co., Ltd.; and Shanxi Taigang Stainless Steel Co., Ltd. Drafting staffs of this Standard. Sun Yuguang, Zhu Weihua, Dai Xuanqian, and Zhang Ruilin. Ferronickel – Determination of Phosphorus, Manganese, Chromium, Copper, Cobalt and Silicon Contents – Inductively Coupled Plasma Atomic Emission Spectrometric Method Warning. The personnel using this Standard shall have practical experience working in the formal laboratory. This Standard does not point out all possible safety issues. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.1 ScopeThis Standard specifies the use of inductively coupled plasma atomic emission spectrometric method (ICP-AES) to determine the contents of phosphorus, manganese, chromium, cobalt, copper and silicon. This Standard is applicable to the determination of phosphorus, manganese, chromium, cobalt, copper and silicon contents in ferronickel. The content ranges of the determined elements are shown in Table 1. The silicon measured by this method is acid-soluble silicon. Table 1 – Content Ranges of the Determined Elements2 Normative ReferencesThe 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, GB/T 4010 Ferroalloys 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 6682 Water for Analytical Laboratory Use - Specification and Test Methods GB/T 20066 Steel and Iron - Sampling and Preparation of Samples for the Determination of Chemical Composition3 PrincipleThe testing material is decomposed by nitric acid and hydrochloric acid. The testing material with high carbon or high silicon content is added with hydrofluoric acid to help dissolving. When perchloric acid emits smoke, it shall expel silicon and fluorine completely.4 ReagentsUnless otherwise specified, only guaranteed reagents and laboratory water complying with the provisions of GB/T 6682 are used in the analysis process. 4.1 High purity nickel, the content of the element to be tested is less than 0.001% (mass fraction). 4.2 High purity iron, the content of the element to be tested is less than 0.001% (mass fraction). 4.3 Hydrochloric acid, ρ is about 1.19g/mL. 4.8 Standard stock solution 4.8.1 Phosphorus standard solution, 1000μg/mL Take 4.3936g of reference dipotassium hydrogen phosphate dried at 105°C ~ 110°C; dissolve it in an appropriate amount of water; transfer it into a 1000 mL volumetric flask; dilute to the mark with water; and mix evenly. 1mL of this solution contains 1000μg of phosphorus. 4.8.4 Cobalt standard solution, 1000μg/mL Take 1.0000g of high-purity cobalt powder (content is greater than 99.9%) in a 600mL beaker; then add 40mL of nitric acid (4.5); cover with a watch glass; heat it to completely dissolve it; slightly boil to discharge nitrogen oxides; cool to room temperature; transfer to a 1000 mL volumetric flask containing 160 mL of nitric acid (4.5); dilute to the mark with water; and mix evenly. 1mL of this solution contains 1000μg of cobalt. 4.8.6 Silicon standard solution, 1000μg/mL After the high-purity silica (content is greater than 99.9%) is sintered to its constant weight at a temperature of 1100°C, it is cooled to room temperature in a desiccator; and take 2.1393g of it into a platinum crucible; and add about 10g of anhydrous sodium carbonate; heated to melting for 15min. 4.8.7 Phosphorus standard solution, 250μg/mL Pipette 25.00mL of phosphorus standard solution (4.8.1) in a 100mL volumetric flask; dilute to the mark with water; and mix evenly. 1mL of this solution contains 250μg of phosphorus. 4.8.8 Copper, silicon and phosphorus mixed standard solution Pipette 25.00mL of copper standard solution (4.8.5), 50.00mL of silicon standard solution, (4.8.6) and 20.00mL of phosphorus standard solution (4.8.7), respectively in a 100mL volumetric flask; dilute to the mark with nitric acid (4.5); and mix evenly. 1mL of this solution contains copper, silicon and phosphorus of 250μg, 500μg and 50μg, respectively.5 Instrument5.1 Inductively coupled plasma (ICP) spectrometer After the spectrometer is optimized according to 7.4.1 ~ 7.4.5 and satisfies the performance indicators of 5.1.2 ~ 5.1.5, then it meets the requirements for use. The spectrometer may be either simultaneous or sequential. 5.1.1 Analysis line This Standard does not specify a special analysis line, the recommended analysis line is listed in Table 2.When in use, carefully check the interference of the spectral lines. 5.1.4 Long-term stability Determine the average value of the absolute intensity of the standard calibration solution with the highest concentration of each element for 3 times; and calculate the standard deviation of the 7 average values. The relative standard deviation shall be less than 2.0%. 5.1.5 Background equivalent concentration and detection limit (see Appendix A) Determine according to Appendix A; calculate the background equivalent concentration and detection limit, the result must be lower than the value in Table 3. 5.1.6 Linearity of the curve Analysis Elements Wavelength / nm Possible interference spectral line / nm6 Sampling and Sample PreparationIt shall be performed according to the provisions of GB/T 4010 and GB/T 20066.7 Analysis Procedures7.1 Amount of testing material Take 0.50g of testing material, accurate to 0.0001g. 7.2 Blank test Do a blank test with the testing material. The blank test shall use pure nickel (4.1) and pure iron (4.2) equivalent to the amount of nickel and iron in the testing material to replace the testing material. 7.3 Determination 7.3.1 Preparation of testing material solution 7.3.2 Preparation of calibration curve solution Replace the testing material with pure nickel (4.1) and pure iron (4.2) equivalent to the amount of nickel and iron in the testing material. Follow the operation procedures in 7.3.1.1.Before the final dilution to 100mL, add the standard solutions according to Table 4, then dilute to the mark with water and mix evenly. 7.4 Spectral measurement 7.4.1 Optimization of the instrument Turn on the inductively coupled plasma (ICP) spectrometer, and run it for at least 1h before measuring. 7.4.2 Measurement of emission intensity 7.4.2.1 Measurement of calibration solution First use the zero-concentration calibration solution; and inhale the calibration solution in order of increasing concentration; and inhale deionized water between each inhalation of the solution. Repeat the measurement for at least 2 times, and take the average of the 2 readings. 7.5 Correction of interference line in analysis line First check the spectral interference of each coexisting element on the analysis line of the measured element. 7.6 Drawing of calibration curve Do the linear regression with the net intensity as the Y-axis and the concentration of the measured element (µg/mL) as the X-axis. The calculation of the correlation coefficient shall meet the requirements of 5.1.6.8 Calculation of Results8.1 According to the calibration curve (7.6), the spectral intensity of the test solution is calculated to the concentration of the corresponding element to be measured, expressed in µg/mL. 8.2 Correction of spectral interference It is recommended to use synthetic standard solution as a correction method for spectral interference, the procedure is as follows.9 PrecisionThe precision of this Standard is jointly tested by 8 laboratories; and is determined by statistical analysis in accordance with the provisions of GB/T 6379.1 and GB/T 6379.2. The precision is shown in Table 5.10 Expression of Analysis ResultsThe analysis result is the average value of the results of 2 independent analyses; and the analysis result retains 2 significant figures after the decimal point.11 Test ReportThe test report shall include the following. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of English version of GB/T 24585-2009 be delivered?Answer: The full copy PDF of English version of GB/T 24585-2009 can be downloaded in 9 seconds, and it will also be emailed to you in 9 seconds (double mechanisms to ensure the delivery reliably), with PDF-invoice.Question 2: Can I share the purchased PDF of GB/T 24585-2009_English with my colleagues?Answer: Yes. 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