Detail of GB/T 18115.4-2021

Introduction of GB/T 18115.4-2021

GB/T 18115.4-2021 Chemical analysis methods of rare earth impurities in rare earth metals and their oxides - Part 4: Determination of lanthanum, cerium, praseodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium contents in neodymium metal and oxide 1 Scope This document specifies the methods for the determination of lanthanum, cerium, praseodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium contents in neodymium metal and oxide. This document is applicable to the determination of lanthanum, cerium, praseodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium contents in neodymium metal and oxide. This document is also applicable to the determination of lanthanum oxide, cerium oxide, praseodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide content in neodymium oxide. This document contains three methods: Inductively coupled plasma-optical emission spectrometry (ICP-OES, Method 1), inductively coupled plasma mass spectrometry (ICP-MS, Method 2), and inductively coupled plasma tandem mass spectrometry (ICP-MS-MS, Method 3). The determination range of Method 1 is shown in Table 1, and that of Methods 2 and 3 is shown in Table 2. Method 2 shall be preferred as the arbitration method in case of an overlap in the analytical range of the three methods. 2 Normative references The following documents contain provisions which, through reference in this text, constitute provisions 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. JJG 768 Verification regulation of emission spectrometer JJF 1159 Calibration specification for quadrupole inductively coupled plasma mass spectrometers 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 inductively coupled plasma tandem mass spectrometer; ICP-MS-MS instrument for which a set of quadrupole mass analyzers is added as an independent mass analyzer in front of the collision/reaction cell of a traditional single quadrupole inductively coupled plasma mass spectrometer, and which works in conjunction with another set of quadrupole mass analyzers after the collision reaction cell to screen and detect the mass of the ions to be determined 3.2 collision/reaction gas gas used in the collision/reaction cell Note: It includes hydrogen, oxygen, helium, ammonia, methane, and other gases. 3.3 oxygen mass shift mode mode where oxygen is used as the collision/reaction gas, with the target ion being the mass number of the product ions generated via reaction between the element to be determined and oxygen Note: In this mode, the mass number of ions detected by the first mass spectrum is different from that detected in the second mass spectrum of the inductively coupled plasma tandem mass spectrometer. 3.4 ammonia mass shift mode mode where ammonia is used as the collision/reaction gas, with the target ion being the mass number of the product ion generated via reaction between the element to be determined and ammonia Note: In this mode, the mass number of ions detected by the first mass spectrum and the second mass spectrum of the inductively coupled plasma tandem mass spectrometer is different. 3.5 oxygen-on-mass mode mode where oxygen is used as the collision/reaction gas, with the target ion being still the mass number of the ions to be determined Note: In this mode, the mass number of ions detected by the first mass spectrum is the same as that detected in the second mass spectrum of the inductively coupled plasma tandem mass spectrometer. 4 Inductively coupled plasma-optical emission spectrometry (Method 1) 4.1 Principle The specimen is dissolved in hydrochloric acid and directly excited by an argon plasma light source in a dilute hydrochloric acid medium for spectral determination. The influence of the matrix on the determination is corrected by matrix matching. 4.2 Reagents Unless otherwise specified, only reagents and distilled water or deionized water of recognized guaranteed reagent quality or water with equivalent purity shall be used during the analysis. 4.2.1 Hydrogen peroxide (30%). 4.2.2 Hydrochloric acid (1+1). 4.2.3 Hydrochloric acid (1+19). 4.2.4 Nitric acid (1+1). 4.2.5 Neodymium oxide matrix solution: Weigh 25.0000 g of neodymium oxide [ω(Nd2O3/REO)≥ 99.999%, ω(REO)≥ 99.5%] that has been ignited at 950 °C for 1 h, place it in a 500-mL beaker, add 75 mL of hydrochloric acid (4.2.2), and heat it at low temperature until completely dissolved, then cool it to room temperature, transfer it to a 500-mL volumetric flask, dilute it to the scale with water, and mix the solution well. 1 mL of this solution contains 50 mg of neodymium oxide. 4.2.6 Praseodymium oxide standard stock solution: Weigh 0.1000 g of praseodymium oxide [ω(Pr6O11/REO)≥99.999%, ω(REO)≥99.5%] that has been ignited at 950 °C for 1 h, place it in a 100-mL beaker, add 10 mL of hydrochloric acid (4.2.2), and heat it at low temperature until completely dissolved, then cool it to room temperature, transfer it to a 100-mL volumetric flask, dilute it to the scale with water, and mix the solution well. Then pipette 10.00 mL of this solution and place it into a 100-mL volumetric flask, dilute it to the scale with hydrochloric acid (4.2.3), and mix it well. 1 mL of this solution contains 100 μg of praseodymium oxide. 4.2.7 Lanthanum oxide standard stock solution: Weigh 0.1000 g of lanthanum oxide [ω(La2O3/REO)≥99.999%, ω(REO)≥99.5%] that has been ignited at 950 °C for 1 h, place it in a 100-mL beaker, add 10 mL of hydrochloric acid (4.2.2), and heat it at low temperature until completely dissolved, then cool it to room temperature, transfer it to a 100-mL volumetric flask, dilute it to the scale with water, and mix it well. 1 mL of this solution contains 1 mg of lanthanum oxide. 4.2.8 Cerium oxide standard stock solution: Weigh 0.1000 g of cerium oxide [ω(CeO2/REO)≥99.999%, ω(REO)≥99.5%] that has been ignited at 950 °C for 1 h, place it in a 100-mL beaker, add 10 mL of nitric acid (4.2.4) and 2 mL of hydrogen peroxide (4.2.1), and heat it at low temperature until completely dissolved, then cool it to room temperature, transfer it to a 100-mL volumetric flask, dilute it to the scale with water, and mix it well. 1 mL of this solution contains 1 mg of cerium oxide. 4.2.9 Samarium oxide standard stock solution: Weigh 0.1000 g of samarium oxide [ω(Sm2O3/REO)≥99.999%, ω(REO)≥99.5%] that has been ignited at 950 °C for 1 h, place it in a 100-mL beaker, add 10 mL of hydrochloric acid (4.2.2), and heat it at low temperature until completely dissolved, then cool it to room temperature, transfer it to a 100-mL volumetric flask, dilute it to the scale with water, and mix it well. 1 mL of this solution contains 1 mg of samarium oxide.

Contents of GB/T 18115.4-2021

Foreword i Introduction v 1 Scope 2 Normative references 3 Terms and definitions 4 Inductively coupled plasma-optical emission spectrometry (Method 1) 5 Inductively coupled plasma mass spectrometry (ICP-MS, Method 2) 6 Inductively coupled plasma tandem mass spectrometry (Method 3)