GB/T 13219-2018Scandium oxide (English PDF)

1 Scope

GB/T 13219-2018 is the Chinese national standard on scandium oxide, in the field of metallurgy. The /T suffix marks it as a recommended standard: it is not compulsory by itself, but it becomes binding as soon as a contract, a tender or a customer specification calls it up - which in practice is how most foreign buyers meet it. It was issued on 13 July 2018 by the State Administration for Market Regulation; Standardization Administration of China, and has been in force since 1 April 2019. Classification: ICS 77.120.99, CCS H65. This page is published from the official record of the standard held by the Chinese standards administration: the identification, the dates, the classification and the issuing body are taken from there. The clause text, the tables and the numeric limits are in the document itself, which is delivered complete in English translation.

This standard specifies the requirements, test methods, inspection rules and packaging, marking, transportation, storage and quality certificates of scandium oxide. This standard is applicable to scandium oxide produced by extraction method, ion exchange method or extraction chromatography method for use in laser, electric light source, atomic energy, electronics, metallurgy and other fields.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 8170 Rules of rounding off for numerical values & expression and judgement of limiting values

GB/T 12690.2 Chemical analysis methods for non-rare earth impurity of rare earth metals and their oxides - Part 2: Determination of ignition loss content of rare earth oxides - Gravimetric method

GB/T 12690.3 Chemical analysis methods for non-rare earth impurity of rare earth metals and their oxides - Part 3: Determination of water content of rare earth oxides - Gravimetric method

GB/T 17803 Designation system for rare earth products

3 Requirements

3.1 Product designations The products are divided into five designations according to chemical composition: Sc2O3-5N5, Sc2O3-5N, Sc2O3-4N, Sc2O3-3N5, Sc2O3-3N; the method of expressing product designations shall comply with GB/T 17803.

Appendix A

(Informative) Chemical analysis method of metal scandium and its oxide - Determination of the total amount of rare earths - Gravimetric method A.1 Scope This method specifies the determination method for the total amount of rare earths in scandium oxide. This method is suitable for the determination of the total amount of rare earths in scandium oxide. Measuring range: 90.00% ~ 99.50%. A.2 Principle of the method The sample is dissolved in hydrochloric acid; the rare earth is precipitated by ammonia water to separate calcium and magnesium. The precipitate is dissolved by hydrochloric acid; the oxalic acid is used to precipitate rare earths. The total amount of rare earth oxide is determined by gravimetric method after precipitation and ignition. A.3 Reagents A.3.1 Hydrochloric acid (rho =

1.19 g/mL), excellent grade pure. A.3.2 Hydrochloric acid (1 + 1), excellent grade pure. A.3.3 Ammonia (1 + 1), excellent grade pure. A.3.4 Oxalic acid solution (50 g/L), excellent grade pure. A.3.5 Oxalic acid solution (20 g/L), excellent grade pure. A.3.6 Ammonia-ammonium chloride solution (20 g/L), which is adjust to pH 9 ~ 10 with ammonia water (A.3.3). A.3.7 Cresol red indicator (1 g/L), prepared with ethanol. A.4 Specimen The oxide specimen is dried at 105 °C for 2 h, placed in a desiccator, cooled to room temperature, weighed immediately. A.5 Analytical procedures A.5.1 Sample

Appendix B

(Informative) Metal scandium and its oxide chemical analysis method - Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium B.1 Scope This Appendix specifies the method for determining the amount of lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide in scandium oxide. This appendix applies to the determination of lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, yttrium oxide in scandium oxide. This Appendix contains two methods. Method 1 is inductively coupled plasma spectroscopy; the measurement range is (mass fraction): 0.0010% ~ 0.10%; Method 2 is inductively coupled plasma mass spectrometry; the measurement range is (mass fraction): 0.00003% ~ 0.010%. When the measurement ranges of method 1 and method 2 overlap, method 2 is used as the arbitration method. This Appendix also applies to the determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium in scandium. B.2 Inductively coupled plasma spectroscopy (Method 1) B.2.1 Principle of the method The specimen is dissolved in hydrochloric acid; in a dilute hydrochloric acid medium, it is directly excited by an argon plasma light source, for the spectrum determination; the influence of the matrix on the determination is corrected by the matrix matching method. B.2.2 Reagents B.2.2.1 Hydrogen peroxide (30%), excellent grade pure. B.2.2.2 Hydrochloric acid (1 + 1), excellent grade pure. B.2.3 Apparatus B.2.3.1 Inductively coupled plasma spectrometer, resolution <

0.006 nm (at 200 nm) >. B.2.3.2 Light source: Argon plasma light source. B.2.4 Specimen B.2.4.1 Oxide specimens are dried at 105 °C for 2 hours, placed in a desiccator, cooled to room temperature, weighed immediately. B.2.4.2 The surface oxide layer shall be removed from the metal specimen and weighed immediately after sampling. B.2.5 Analytical procedures B.2.5.1 Sample B.2.5.1.1 Oxide sample Weigh

1.000 g of specimen (B.2.5.1), accurate to 0.0001 g. B.2.5.1.2 Metal sample Weigh

0.862 g of sample (B.2.4.2), accurate to 0.0001 g. B.2.5.2 Number of determinations Weigh two sets of samples; perform parallel determination; take the average value. B.2.5.3 Blank test Do a blank test with the sample. B.2.5.4 Preparation of analysis test solution Place the sample (B.2.5.1) in a 100 mL beaker; add 10 mL of water; add 20 mL of hydrochloric acid (B.2.2.2); heat at low temperature to completely dissolve; evaporate to about 5 mL; cool to room temperature. Transfer to a 100 mL volumetric flask; use water to dilute to the mark; mix well; prepare for use. B.2.5.5 Preparation of standard series solutions Transfer the scandium oxide matrix solution (B.2.2.5) and each rare earth oxide standard solution (B.2.2.6 ~ B.2.2.8) into seven 50 mL volumetric flasks according to Table B.1; add 5 mL of hydrochloric acid (B.2.2.2); use water to dilute to the mark; mix well; prepare a standard series solution; use the standard C.3.3 Hydrochloric acid (1 + 19), excellent grade pure. C.3.4 Nitric acid (1 + 1), excellent grade pure. C.3.5 Hydrofluoric acid, excellent grade pure. C.3.6 Perchloric acid, excellent grade pure. C.3.7 Scandium oxide matrix solution: Weigh 5.0000 g of scandium oxide [w (Sc2O3/SigmaREO) >= 99.9995%, w (SigmaREO) >= 99.5%] that has been burned at 900 °C for 1 h; place it in 200 mL beaker; add 40 mL of hydrochloric acid (C.3.2); heat at low temperature to complete dissolution; evaporate to about 10 mL; cool to room temperature; transfer to a 50 mL volumetric flask; use water to dilute to the mark; mix well. 1 mL of this solution contains 100 mg of scandium oxide. C.3.8 Silicon standard storage solution: Weigh 0.2139 g of spectrally pure silica (spectrally pure) that has been pre-fired at 950 °C for 2 h and placed in a desiccator to cool to room temperature; place it in a platinum crucible (premium grade) which contains 5 g of anhydrous sodium carbonate; mix well; melt at 1000 °C for 20 min; take out and cool it slightly; use hot water to extract it; make its volume reach to 1000 mL. 1 mL of this solution contains 100 µg of silicon. Store it in a plastic bottle. Use pure water to dilute this solution into 1 mL of silicon standard solution containing 10 µg and 1 µg, respectively. C.3.9 Iron standard storage solution: Pipette 1.4298 g of iron trioxide (spectrally pure) dried at 110 °C for 1 h into a 200 mL beaker; add 50 mL of hydrochloric acid (C.3.2) to heat to dissolve; cool to room temperature; transfer it into a 1000 mL volumetric flask; use water to dilute to the mark; mix well. 1 mL of this solution contains 1 mg iron. Use hydrochloric acid (5 + 95) to dilute this solution into 1 mL of iron standard solutions containing 100 µg, 10 µg, 1 µg, respectively. C.3.10 Calcium standard storage solution: Pipette 2.4951 g of calcium carbonate (spectrally pure) baked at 110 °C for 1 h into a 200 mL beaker; add 50 mL of hydrochloric acid (C.3.2) to heat to dissolve; cool to room temperature; transfer it into a 1000 mL volumetric flask; use water to dilute it to the mark; mix well. 1 mL of this solution contains 1 mg of calcium. Use hydrochloric acid (C.3.3) to dilute this solution into 1 mL of calcium standard solutions containing 100 µg, 10 µg, 1 µg, respectively. C.3.11 Zirconium standard storage solution: Weigh 3.5328 g of zirconium oxychloride (ZrOCl2 - 8H2O) (spectrally pure) into a 200 mL beaker; add 5 mL of nitric acid (C.3.4) and 50 mL of water; after heating to dissolve, transfer it into a 1000 mL volumetric flask; use water to dilute it to the mark; mix well. 1 mL of this solution contains 1 mg of zirconium. Use hydrochloric acid (C.3.3) to dilute this solution into 1 mL of zirconium standard solutions containing 100 µg, 10 µg, 1 µg, respectively. this solution into 1 mL of sodium standard solution containing 100 µg, 10 µg, 1 µg, respectively. C.3.18 Nickel standard storage solution: Weigh 1.2730 g of nickel oxide (spectrally pure) that has been baked at 110 °C for 1 h, in a 200 mL beaker; add 50 mL of hydrochloric acid (C.3.2) to dissolve it; cool to room temperature; transfer it into a 1000 mL volumetric flask; use water to dilute to the mark; mix well. 1 mL of this solution contains 1 mg of nickel. Use hydrochloric acid (C.3.3) to dilute this solution into 1 mL nickel standard solutions containing 100 µg, 10 µg, 1 µg, respectively. C.3.19 Standard storage solution of thorium: Weigh 2.3800 g of thorium nitrate [Th(NO3)4 - 4H2O] (spectrally pure) into a 200 mL beaker; add 100 mL hydrochloric acid (C.3.2) to dissolve it; cool to room temperature; transfer it in a 1000 mL volumetric flask; use water to dilute to the mark; mix well. 1 mL of this solution contains 1 mg thorium. Use hydrochloric acid (C.3.3) to dilute this solution into 1 mL of thorium standard solutions containing 100 µg, 10 µg, 1 µg, respectively. C.3.20 Tantalum standard storage solution: Weigh 1.0000 g of metallic tantalum (spectrally pure) into a platinum crucible; add 6 mL ~ 8 mL of hydrofluoric acid (C.3.5); dissolve and evaporate at low temperature to near dryness; use (100 g/L) tartaric acid to extract it; dissolve at slight heat; cool to room temperature; transfer it into a 1000 mL volumetric flask; use water to dilute to the mark; mix well. 1 mL of this solution contains 1 mg of tantalum. Use hydrochloric acid (C.3.3) to dilute this solution into 1 mL of tantalum standard solutions containing 100 µg, 10 µg, 1 µg, respectively. C.3.21 Argon [Phi (Ar) >= 99.99%]. C.4 Instruments C.4.1 Inductively coupled plasma spectrometer, resolution <