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GB/T 20125-2006: Low-alloy steel -- Determination of multi-element 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 20125-2006: Low-alloy steel -- Determination of multi-element 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/GBT20125-2006 NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.080.20 H 11 Low-alloy steel - Determination of multi-element contents - Inductively coupled plasma atomic emission spectrometric method Issued on. MARCH 02, 2006 Implemented on. SEPTEMBER 01, 2006 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of PRC; Standardization Administration of PRC. Table of ContentsForeword... 3 1 Scope... 5 2 Normative references... 6 3 Principles... 6 4 Reagents and materials... 6 5 Instruments and equipment... 12 6 Sampling and preparation of specimen... 14 7 Analytical procedures... 15 8 Result calculation... 17 9 Precision... 18 10 Test report... 19 Appendix A (Normative) Standardized operation of measuring instrument... 20 Appendix B (Informative) Additional information on common precision tests... 231 ScopeThis standard specifies the method for the determination of silicon, manganese, phosphorus, nickel, chromium, molybdenum, copper, vanadium, cobalt, titanium, aluminum, by inductively coupled plasma emission spectrometry. This method is suitable for the determination of silicon, manganese, phosphorus, nickel, chromium, molybdenum, copper, vanadium, cobalt, titanium, aluminum in carbon steel and low alloy steel, which has an iron mass fraction greater than 92%. For the determination range of multi-elements, refer to Table 1. The silicon, titanium, aluminum, which is measured by this method, are acid-soluble silicon, acid-soluble titanium, acid-soluble aluminum. When even only one of the components in the steel exceeds the upper limit of the content range in Table 1, this standard does not apply. In steel, when the mass fraction of carbon and sulfur is greater than 1.0%, AND the mass fraction of tungsten and niobium is greater than 0.10%, this standard is also not applicable.2 Normative referencesThe provisions in following documents become the provisions of this Standard through reference in this Standard. For the dated references, the subsequent amendments (excluding corrections) 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 20066-2006 Steel and iron - Sampling and preparation of samples for the determination of chemical composition GB/T 6379 (all parts) Accuracy (trueness and precision) of measurement methods and results3 PrinciplesThe sample is dissolved by a mixed acid of hydrochloric acid and nitric acid AND diluted to a certain volume.4 Reagents and materialsUnless otherwise stated, only approved reagents of analytical grade and double distilled water or water of equivalent purity are used in the analysis. 4.1 High-purity iron. the mass fraction is greater than 99.98%; the content of the element to be tested is known. 4.7 Yttrium standard solution 4.8 Silicon standard solution 4.8.1 Silicon stock solution, 500.0 µg/mL Weigh 0.5348 g of silica (mass fraction greater than 99.9%, pre-fired at 1000 °C for 1 h, placed in a desiccator and cooled to room temperature). Place it in a platinum crucible, which contains 3 g of anhydrous sodium carbonate. Stir it evenly. Cover (1 ~ 2) g of anhydrous sodium carbonate on the top. 4.9 Manganese standard solution 4.9.1 Manganese stock solution, 1000.0 µg/mL Weigh 1.0000 g of electrolytic manganese [mass fraction greater than 99.9%, use nitric acid (1 + 3) to wash the surface oxide film in advance; 4.10 Phosphorus standard solution 4.10.1 Phosphorus stock solution, 1000.0 µg/mL Weigh 4.3936 g of standard potassium dihydrogen phosphate (KH2PO4) (pre-dried at 105 °C for 1 h. Place it in a desiccator. Cool it to room temperature). Place it in a 500 mL beaker. Use an appropriate amount of water to dissolve it. Boil it. Cool it. Transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well. 1 mL of this solution contains 1000.0 µg of phosphorus. 4.16 Cobalt standard solution 4.17 Titanium standard solution 4.17.1 Titanium stock solution, 250.0 µg/mL Weigh 0.2500 g of titanium metal (mass fraction greater than 99.9%). Put it in a 400 mL polytetrafluoroethylene beaker. Add 5 mL of hydrofluoric acid. Immediately add 2 mL of nitric acid (4.3) dropwise. Heat to dissolve it. Cool it. Add 20 mL of sulfuric acid (4.5). Evaporate it at low temperature, until sulfuric acid smoke. Cool to room temperature. Use sulfuric acid (5 + 95), to transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well. 4.18 Aluminum standard solution 4.18.1 Aluminum stock solution, 1000.0 µg/mL Weigh 1.0000 g of pure aluminum (mass fraction greater than 99.9%). Put it in a 500 mL beaker. Add 100 mL of hydrochloric acid (1 + 1). Dissolve it on a water bath at 85 °C (1 ~ 3 days).5 Instruments and equipmentUsual laboratory equipment and inductively coupled plasma atomic emission spectrometer (ICP-AES). 5.1 Inductively coupled plasma atomic emission spectrometer (ICP-AES) If, after the spectrometer is optimized according to 7.4.1 ~ 7.4.5, it meets the performance index of 5.1.2 ~ 5.1.5, THEN, it meets the usage requirements. Spectrometers can be either simultaneous or sequential. However, it must have the function of measuring the internal mark, at the same time. Otherwise, the internal standard method cannot be used. 5.1.4 Long-term stability Make 3 measurements, of the average value of the absolute intensity or intensity ratio of the calibration solution, which has the highest concentration of each element. Calculate the standard deviation of the seven average values. 5.1.5 Background equivalent concentration and detection limit (see Appendix A.2) Elements Wavelength/nm Possible interfering elements For the analysis line, which contains only the element to be detected in the solution, calculate the background equivalent concentration (BEC) and detection line (DL); the results must be lower than the values in Table 3. 5.1.6 Linearity of curve The linearity of the calibration curve is checked by calculating the correlation coefficient, which must be greater than 0.999.6 Sampling and preparation of specimenTake samples AND prepare specimen, according to GB/T 20066 or appropriate national standards.7 Analytical procedures7.1 Sample amount Weigh 0.50 g of sample, accurate to 0.1 mg. 7.2 Blank test (equivalent to No.0) Weigh 0.500 g of high-purity iron (4.1). Make a blank test with the sample. 7.3 Determination 7.3.1 Preparation of specimen solution Place the sample (7.1) in a 200 mL beaker. Add 10 mL of water, 5 mL of nitric acid (4.3). 7.3.2 Preparation of calibration curve solution Weigh 7 parts of 0.500 g high-purity iron (4.1) into a 200 mL beaker. Dissolve it according to step 7.3.1.Cool it to room temperature. Transfer the solution to a 100 mL volumetric flask. Add the standard solution of the analyte, according to Table 4 and Table 5. 7.4 Spectral measurements 7.4.1 Optimization of instrument Turn on ICP-AES and run for at least 1 h, before taking measurements. Measure the most concentrated calibration solution. Adjust the instrument parameters, according to the operating procedures and guidelines, which are provided by the instrument manufacturer. gas (outer, middle or center) flow rate, torch position, entrance slit, exit slit, photomultiplier tube voltage, analysis line wavelength in Table 2, prewash time, integration time. 7.5 Correction of interference lines in analysis lines First check the spectral interference of each coexisting element on the analytical line of the analyte. In the case of spectral interference, obtain the spectral interference correction factor, that is, the mass fraction of the analyte, when the mass fraction of the coexisting element is 1%. 7.6 Plotting of calibration curve Take the net intensity or net intensity ratio as the Y axis; take the concentration of the analyte (µg/mL) as the X axis, for linear regression. The calculation of the correlation factor shall meet the requirements of 5.1.6.8 Result calculationAccording to the calibration curve (7.6), convert the net intensity or net intensity ratio of the test solution to the concentration of the corresponding analyte, expressed in µg/mL.9 PrecisionThe precision data for this standard are determined in 2003, by co-testing (6 ~ 10) levels of multi-elements by (6 ~ 9) laboratories. According to the provisions of GB/T 6379, each laboratory makes 3 measurements for each level of multi-elements.10 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. 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