GB/T 30903-2014 PDF English
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GB/T 30903-2014: Inorganic chemicals for industrial use - Determination of impurity element - Inductively coupled plasma mass spectrometry (ICP-MS)
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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 mass spectrometry (ICP-MS) Issued on. JULY 08, 2014 Implemented on. DECEMBER 01, 2014 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of the People's Republic of China.
Table of Contents
Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Terms and definitions... 5 4 Principle... 6 5 Reagents... 6 6 Instruments, devices... 6 7 Analysis steps... 7 8 Precision... 11 9 Recovery rate... 11 Annex A (normative) Quartz sub-boiling distillation unit... 13 Annex B (normative) Detection limit determination method... 14Foreword
This 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 Chemicals of National Technical Committee on Chemical of Standardization Administration of China (SAC/TC 63/SC 1). The drafting organizations of this Standard. Hubei Xingfa Chemical Group Co., Ltd., Foshan Quality Metrology Supervision and Inspection Center, CNOOC Tianjin Chemical Research and Design Institute, Jiangxi Nuclear Industry Xingzhong Technology Co., Ltd., Guangdong Pioneer Rare Materials Co., Ltd., and National Inorganic Salt Product Quality Supervision and Inspection Center. Main drafters of this Standard. Xiong Ping, Liang Chiqiong, Gong Chuangzhou, Xu Hui, Zhu Liu, Du Jianxia, Song Bo, Liu Yonghao. Inorganic chemicals for industrial use - Determination of impurity element - Inductively coupled plasma mass spectrometry (ICP-MS) WARNING -- Some of the reagents used in this test method are toxic or corrosive. Be careful when operating! If splashed on the skin, rinse with water immediately, and seek medical treatment immediately in severe cases. This test method uses high-pressure argon cylinders, which shall be operated in accordance with the safe 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 Scope
This Standard specifies the principle, reagents, instruments, equipment, analytical procedures, precision and recovery rate for the determination of metallic and non- metallic impurity elements in inorganic chemical products by inductively coupled plasma mass spectrometry (ICP-MS). This Standard is applicable to liquid samples containing multiple metal and non-metal impurity elements in inorganic chemical products or direct sampling after removing the matrix. Determination is carried out using inductively coupled plasma mass spectrometry (ICP-MS).2 Normative references
The 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, Argon3 Terms and definitions
For the purposes of this document, the terms and definitions defined in GB/T 4470 as well as the followings apply. 3.1 plasma An ionized gas with a degree of ionization greater than 0.1% and equal positive and negative charges. 3.2 radio frequency generator An RF power source provides RF energy to the coupling coil and plasma. 3.3 inductively coupled plasma; ICP A torch flame that is formed by applying high frequency power to a coil coupled to a plasma torch. 3.4 plasma torch A device used to maintain stable discharge in ICP, usually composed of three concentric quartz tubes. The outer tube is fed with cooling gas, the middle tube is fed with auxiliary gas, and the inner tube is fed with carrier gas. 3.5 incident power The net power delivered by the high frequency generator to the coupled coil and plasma.4 Principle
The specimen solution is introduced into the atomization system by the carrier gas (argon) for atomization, and then enters the plasma center in the form of aerosol. It is de-solvated, vaporized, dissociated and ionized in high temperature and inert atmosphere, and converted into positive ions with positive charge.5 Reagents
5.1 Chemical reagents shall be of high purity and purified (such as quartz sub-boiling distillation equipment, see Annex A). Common inorganic acids include nitric acid (HNO3), hydrochloric acid (HCl), hydrofluoric acid (HF), perchloric acid (HClO4), sulfuric acid (H2SO4), and aqua regia (1HNO3 +3HCl).6 Instruments, devices
Inductively coupled plasma mass spectrometer. consists of an injection system, torch and plasma, ion lens system, vacuum system, mass analyzer, detector and data processing system.7 Analysis steps
7.1 Selection of measurement conditions 7.1.1 Incident power Select the best power according to the characteristics of the sample to be tested and the instrument conditions. The general range is 0.8 kW~1.6 kW. 7.2 Interference and elimination Interferences in inductively coupled plasma mass spectrometry can be roughly divided into two categories. One is mass spectrometry interference, which mainly includes oxide ion interference, divalent ion interference, polyatomic ion interference and isobaric interference. 7.3 Sample processing 7.3.1 Laboratory equipment 7.3.1.1 For general micro and trace analysis, attention shall be paid to the overall cleanliness of the laboratory. When ultra-trace or high-demand analysis is performed, an ultra-clean laboratory is generally required. 7.3.2 Sample pretreatment methods 7.3.2.1 Open vessel digestion method The specimen and reagent are heated in an open container over a flame or on a hot plate or in an electric furnace. This method is the most commonly used. This method has low equipment requirements and can be used to digest a large number of samples at the same time. The disadvantages are that it takes a long time, is more polluting, and has poor accuracy and precision. 7.3.2.2 Closed container digestion method A decomposition method that uses acid or other reagents to perform wet digestion under heat and pressure in a sealed container (usually made of polytetrafluoroethylene). 7.3.2.4 Alkali metal melting method A variety of alkali metal fluxes, such as lithium metaborate, lithium tetraborate, sodium carbonate, sodium hydroxide, sodium peroxide, corresponding potassium salts and alkali metal fluorides (especially potassium bifluoride) are mixed with the sample and melted at high temperature. 7.3.2.5 Separation and pre-enrichment methods The separation process can remove possible matrix effects and interferences and achieve pre-enrichment to reduce the limit of quantitation. The main methods include solvent extraction, ion exchange, and co-precipitation/adsorption. 7.3.3 Requirements for liquid solutions After the sample is digested, it is fixed to an appropriate volume according to the content of the element to be measured to prepare a specimen 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 specimen solution is at least three times the detection limit of the element. The determination method of the detection limit is shown in Annex B.8 Precision
Determined in accordance with GB/T 6379.2. The precision of indoor repeatability in the same laboratory can be determined by the indoor standard deviation and indoor repeatability when the same instrument is used under the same measurement conditions and the number of measurements by the same person is not less than 11 times.9 Recovery rate
Add an appropriate amount of the standard solution of the element to be measured to the specimen solution. Measure the mass concentration of the specimen solution before and after the addition of the spike.Annex A
(normative) Quartz sub-boiling distillation unitAnnex B
(normative) Detection limit determination method Prepare 4~5 standard solutions of the elements to be tested and a blank test solution with proportional mass concentrations. Adjust the instrument to the best working state. Measure the response intensity values of the series of standard solutions. Draw a standard curve. At the same time, measure the mass concentration value of the blank test solution for 10 consecutive times. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
