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GB/T 30902-2014: Inorganic chemicals for industrial use - Determination of impurity element - Inductively coupled plasma optical emission spectrometry (ICP-OES) 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 30902-2014: Inorganic chemicals for industrial use - Determination of impurity element - Inductively coupled plasma optical emission spectrometry (ICP-OES)---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/GBT30902-2014 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.060.01 G 10 Inorganic chemicals for industrial use - Determination of impurity element - Inductively coupled plasma optical emission spectrometry (ICP-OES) Issued on. JULY 08, 2014 Implemented on. DECEMBER 01, 2014 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of the People’s Republic of China. Table of ContentsForeword... 3 1 Scope... 4 2 Normative references... 4 3 Terms and definitions... 5 4 Principle... 6 5 Reagents... 6 6 Instruments and apparatuses... 7 7 Procedure... 7 8 Precision... 11 9 Recovery... 11 Appendix A (Informative) Preparation of multi-element standard solutions... 12 Appendix B (Informative) Wavelength of analysis spectral lines of elements to be measured... 13 Appendix C (Informative) Determination method of detection limit... 15ForewordThis Standard was drafted in accordance with the rules given in GB/T 1.1-2009. This Standard was proposed by China Petroleum and Chemical Industry Federation. This Standard shall be under the jurisdiction of Subcommittee on Inorganic Chemical Industry of National Standardization Technical Committee of Chemical (SAC/TC 63/SC 1). Drafting organizations of this Standard. Hubei Xingfa Chemicals Group Co., Ltd., CenerTech Tianjin Chemical Research and Design Institute Co., Ltd., Jiangxi Nuclear Industry Xingzhong Technology Co., Ltd., FINE Chemicals Group Co., Ltd., First Rare Materials Co., Ltd., Guangdong Shantou Quality Measurement Supervision and Inspection Institute, National inorganic salt product quality supervision and Inspection Center. Main drafters of this Standard. Xiong Ping, Ding Ling, Hu Changwen, Cai Laijun, Zhu Zanfang, Du Jianxia, Chen Min, Gong Chuangzhou, Liang Yuan. Inorganic chemicals for industrial use - Determination of impurity element - Inductively coupled plasma optical emission spectrometry (ICP-OES) Warning. Some of the reagents used in this test method are toxic or corrosive, so be careful when operating! If it splashes on the skin, rinse it with water immediately, and in serious cases, treat it immediately; high-pressure argon gas cylinders are used in this test method and shall be operated according to the safety operation regulations of high-pressure cylinders; after igniting the plasma, the torch chamber door shall not be opened to prevent high-frequency radiation from harming the body; pay attention to safe use of electricity.1 ScopeThis Standard specifies the principle, reagents, instruments, apparatuses, analysis steps, precision, and recovery rate for the determination of metallic and non-metallic impurity elements in inorganic chemicals for industrial use using inductively coupled plasma optical emission spectrometry (ICP-OES). This Standard applies to direct injection of liquid samples containing various impurities in inorganic chemicals for industrial use or test solutions after removing the matrix, using an inductively coupled plasma optical emission spectrometer for measurement.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB/T 4470, Analytical spectroscopic methods - Flame emission, atomic absorption and atomic fluorescence - Vocabulary GB/T 4842, Argon 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 6682-2008, Water for analytical laboratory use - Specification and test methods3 Terms and definitionsTerms and definitions determined by GB/T 4470, as well as the following, are applicable to this document. 3.1 plasma An ionized gas with an ionization degree greater than 0.1% and equal positive and negative charges. 3.2 high frequency generator A high-frequency power source that provides high-frequency energy to the coupling coil and plasma. 3.3 plasma torch A device, used to maintain stable discharge in ICP, which is usually composed of three layers of concentric quartz tubes. The outer tube supplies coolant gas, the middle tube supplies auxiliary gas, and the inner tube supplies carrier gas. 3.4 incident power The net power delivered to the coupling coil and plasma by the high frequency generator. 3.5 observation height The height of the exposed area of the plasma torch, i.e., the distance from the center of the observation area to the upper end of the coupling coil.4 PrincipleAfter the liquid sample is brought into the atomization system by the carrier gas for atomization, it enters the axial channel of the plasma in the form of an aerosol, and is fully evaporated, atomized, ionized and excited in the high temperature and inert gas.5 Reagents5.1 Unless other requirements are specified, the reagents used refer to reagents of analytical grade or above. 5.2 Laboratory water shall meet the specifications for water of grade 2 or above in GB/T 6682-2008. 5.3 Standard stock solution. The standard stock solution of each analytical element shall be prepared according to the regulations in HG/T 3696.2.6 Instruments and apparatusesInductively coupled plasma atomic emission spectrometer. consisting of a sampling system, an excitation light source, an optical system, a detection system and a data processing system.7 Procedure7.1 Selection of measurement conditions 7.1.1 Analysis spectral line of elements to be measured Refer to Appendix B for the wavelength of the analysis spectral line of elements to be measured. 7.1.5 Gas flow Determine the optimal flow rate of each gas according to the torch and analysis requirements. The argon gas used shall comply with the requirements of GB/T 4842. 7.1.6 Analysis time Washing time and exposure time are determined by the instrument and analysis requirements. 7.2 Elimination of interference 7.2.1 Some interference effects in the light source shall be limited to a certain level by adopting appropriate separation methods and selecting appropriate element spectral line, observation height, incident power and carrier gas flow rate. For spectral interference, methods based on correction of interference factor, matrix separation method, or software provided by the instrument manufacturer can be used for correction. For non- spectral interference, matrix matching or standard addition methods shall be used for correction. 7.3 Sample treatment 7.3.1 Laboratory equipment 7.3.1.1 For general micro and trace analysis, pay attention to the overall cleaning of the laboratory. 7.3.2 Sample pretreatment methods 7.3.2.1 Open container digestion method The sample and reagents are heated in an open container over a flame or on an electric hot plate or in an electric furnace. This method is the most commonly used. This method has lower requirements for equipment and can be used for simultaneous digestion of large batches of samples. The disadvantages are that it takes a long time, the pollution is serious, and the accuracy and precision are poor. 7.3.2.2 Closed container digestion method It is a decomposition method of wet digestion carried out under heat and pressure in a closed container (usually made of polytetrafluoroethylene) by using acid or other reagents. 7.3.3 Liquid solution requirements After the sample is processed, adjust the volume to an appropriate volume according to the content of the element to be measured, and make the sample solution. The sampling volume is determined based on the mass concentration of the element to be measured in the sample and the detection limit of the method; the mass concentration of the element to be measured in the sample solution shall be at least three times the detection limit of the element. See Appendix C for the determination method of detection limit. 7.4 Determination 7.4.1 Qualitative analysis Based on three or more sensitive lines of the element to be measured in the spectrum, qualitatively determine whether the element to be measured is present. Generally, there are two qualitative methods. comparative spectral line method and semi-automatic qualitative analysis. 7.4.2 Semi-quantitative analysis The approximate content of the element to be measured in the sample can be measured, and semi-quantitative analysis results can be obtained using the software provided by the ICP-OES instrument. Generally, there are two semi-quantitative analysis methods. partial calibration method and persistence curve method. 7.4.3 Quantitative analysis8 PrecisionIt can be determined according to GB/T 6379.2. The repeatability precision within the same laboratory can be determined by using the same instrument under the same measurement conditions and by the same person for no less than 11 measurements to determine the laboratory standard deviation and laboratory repeatability.9 RecoveryAdd an appropriate amount of the standard solution of the element to be measured to the sample solution; respectively measure the mass concentration of the sample solution before and after the addition of the standard.Appendix A(Informative) Preparation of multi-element standard solutions A.1 When mixing and preparing commercially available single element standard solutions, the influence of anions on the ions of the element to be measured must be considered. For example, sulfate ions will cause Ba2+ to precipitate out. The influence of chloride ions should be considered when measuring Ag+. A.2 When many elements are measured at the same time, the high-low matching method should be used to prepare the standard series. Avoid large differences in the soluble solids of each standard sample in the series, which may cause significant matrix effects.Appendix B(Informative) Wavelength of analysis spectral lines of elements to be measuredAppendix C(Informative) Determination method of detection limit Prepare 4 ~ 5 standard solutions and blank solutions of the element to be measured with proportional mass concentrations; adjust the instrument to the best working condition; measure the intensity values of the series standard solutions; draw a standard curve; at the same time, measure the mass concentration value of the blank solution 10 times continuously. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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