GB/T 18115.6-2023Chemical analysis methods of rare earth impurities in rare earth metals and their oxides—Part 6:Determination of lanthanum,cerium,praseodymium,neodymium,samarium,gadolinium,terbium,dysprosium,holmium,erbium,thulium,ytterbium,lutetium and yttrium contents in europium metal and oxide (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents" Drafting.

This document is Part 6 of GB/T 18115 "Chemical Analysis Methods for Rare Earth Impurities in Rare Earth Metals and Their Oxides". GB/T 18115 The following sections have been published.

---Part 1. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in lanthanum;

---Part 2. Determination of the amounts of lanthanum, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in cerium;

---Determination of the amount of lanthanum, cerium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in praseodymium;

---Part 4. Determination of the amounts of lanthanum, cerium, praseodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in neodymium;

---Determination of the amount of lanthanum, cerium, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in samarium;

---Determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in europium;

---Determination of the amount of lanthanum, cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in gadolinium;

---Determination of the amount of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in terbium;

---Determination of the amount of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in dysprosium;

---Determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, erbium, thulium, ytterbium, lutetium and yttrium in holmium;

---Determination of the amount of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, thulium, ytterbium, lutetium and yttrium in erbium;

---Determination of the amount of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, ytterbium, lutetium and yttrium in yttrium;

---Part 13. Determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, lutetium and yttrium in thulium;

---Part 14. Determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and yttrium in ytterbium;

---Part 15. Determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium in lutetium.

This document replaces GB/T 18115.6-2006 "Methods for chemical analysis of rare earth impurities in rare earth metals and their oxides - Lanthanum, cerium, "Determination of the amount of praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium", compared with GB/T 18115.6-2006, except for structural adjustment and compilation In addition to editorial changes, the main technical changes are as follows:

a) The measurement range of inductively coupled plasma mass spectrometry (ICP-MS, method 2) has been changed, lanthanum oxide, cerium oxide, praseodymium oxide, oxidation The measurement range of neodymium, samarium oxide, gadolinium oxide, terbium oxide, and yttrium oxide is changed from "0.00005%~0.050%" to "0.00005%~ 0.0050%" (see Table 2, Table 7 of the 2006 edition);

b) Added "Terms and Definitions" (see Chapter 3);

c) Added description of reagents and water used in analysis (see 4.2, 5.2);

d) The analytical spectral line of inductively coupled plasma optical emission spectrometry (ICP-OES, method 1) has been changed, changing cerium 414.660nm to Cerium 413.380nm; changed gadolinium 310.650nm to gadolinium 310.050nm; added praseodymium 422.293nm; deleted cerium 407.076nm (see Table 3, 2006 version of Table 3);

e) The pretreatment conditions for the samples of Method 1 and Method 2 were changed from "burning at 900°C for 1h" to "baking at 105°C for 1h" (see 4.4.1, 5.4.1, 5.1, 14.1 of the 2006 version);

f) Added the low concentration standard series "0µg/mL, 0.05µg/mL, 0.10µg/mL, 0.50µg/mL, 1.00µg/mL" (see Table 4 and Table 5);

g) Changed part of the expression of precision of Method 1 and Method 2, changing "allowable difference" to "reproducibility" (see 4.8.3, 5.8.3, 2006 Year version 8.2, 17.2);

h) Changed the weighing amount of method 2, changing the weighing amounts of 0.50g, 0.25g and 0.10g corresponding to different contents of rare earth impurities to oxidation 0.500g of material sample (see 5.5.1.1, Table 8 of 2006 edition), 0.432g of metal sample (see 5.5.1.2, Table 8 of 2006 edition);

i) The working curve of method 2 has been changed. The mass concentration of the working curve is from "0ng/mL, 2.0ng/mL, 10.0ng/mL, "50.0ng/mL, 100ng/mL" is changed to "0ng/mL, 0.50ng/mL, 2.00ng/mL, 5.00ng/mL, 10.00 ng/mL, 20.00ng/mL, 50.00ng/mL" (see 5.5.4, 15.5 of the 2006 edition);

j) Method 3 Inductively Coupled Plasma Tandem Mass Spectrometry (ICP-MS-MS) has been added (see Chapter 6).

Introduction

In the field of chemical composition analysis of rare earth products, my country has established a relatively comprehensive system for the detection of total rare earth content, non-rare earth impurities, rare earth impurities, etc. comprehensive standard system. GB/T 18115 "Methods for chemical analysis of rare earth impurities in rare earth metals and their oxides" for 15 single rare earth metals All rare earth impurities in its oxides (except scandium and promethium) are analyzed using inductively coupled plasma optical emission spectrometry (ICP-OES), inductive coupling, etc.

Ion mass spectrometry (ICP-MS) and inductively coupled plasma tandem mass spectrometry (ICP-MS-MS) have established a series of corresponding The scope analysis method is planned to consist of 15 parts.

---Part 1. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in lanthanum. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in lanthanum and lanthanum oxide.

---Part 2. Determination of the amount of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in cerium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in cerium and cerium oxide.

---Part 3. Determination of the amount of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in praseodymium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in praseodymium and praseodymium oxide.

---Part 4. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in neodymium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in neodymium and neodymium oxide.

---Part 5. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in samarium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in samarium and samarium oxide.

---Part 6. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in europium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in europium and europium oxide.

---Part 7. Determination of the amount of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in gadolinium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in gadolinium and gadolinium oxide.

---Part 8. Determination of the amount of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in terbium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in terbium and terbium oxide.

---Part 9. Determination of the amount of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in dysprosium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in dysprosium and dysprosium oxide.

---Part 10. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in holmium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in holmium and holmium oxide.

---Part 11. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in erbium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in erbium and erbium oxide.

---Part 12. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in yttrium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in yttrium and yttrium oxide.

---Part 13. Determination of the amount of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in thulium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in thulium and thulium oxide.

---Part 14. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in ytterbium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in ytterbium and ytterbium oxide.

---Part 15. Determination of the amounts of cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in lutetium. The purpose is to establish the deposit Testing methods and requirements for rare earth impurities in lutetium and lutetium oxide.

The complex spectral characteristics of rare earth elements and the interference of polyatomic ions of rare earth matrix elements in mass spectrometry analysis have always been a problem in rare earth analysis. difficulties. Therefore, since its release, GB/T 18115 has been committed to introducing new technologies to solve the above technical problems, improving and optimizing the standard method.

Law. GB/T 18115 was first released in 2000, introducing ICP-OES into the field of rare earth analysis, and the method covers all rare earths except thulium, ytterbium, and lutetium.

12 kinds of rare earth matrices, the relative purity of analyzable rare earths reaches 99.99%; the work in 2006 improved ICP-OES and introduced ICP- MS, and the use of micro-column pre-separation technology, solves the problem of rare earth polyatomic ion interference in mass spectrometry analysis, and the relative purity of the analyzable rare earth can reach to 99.999%; in 2010, thulium, ytterbium, and lutetium matrices were added, improving the scope of GB/T 18115 to 15 rare earth matrices; this revision We have further improved the original ICP-OES and ICP-MS, and introduced a new instrument technology ICP-MS- that solves the interference of polyatomic ions in mass spectrometry.

MS meets the needs of the production and manufacturing of new materials and equipment and enhances the applicability of the standard.

GB/T 18115 standardizes the operation of single rare earth relative purity analysis in the rare earth analysis industry, enhances the comparability of test data, and It plays an important guarantee and support role in the improvement of rare earth smelting and separation processes, product quality control and trade.

Rare earth impurities in rare earth metals and their oxides Methods of chemical analysis Part 6.

In europium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, Determination of the amount of erbium, thulium, ytterbium, lutetium and yttrium WARNING. Personnel using this document should have practical experience in regular laboratory work. This document does not address all possible security issues question. Users should have certain professional knowledge and skills and be fully aware of the gas leakage, current leakage, and fire hazards that may be caused by improper operation. disaster or other serious consequences.

1 Scope

This document describes methods for the determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in europium.

This document applies to the determination of the amounts of lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in metallic europium.

This document also applies to lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, and oxide in europium oxide.

Determination of the amount of holmium, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide.

This document contains a total of three methods. inductively coupled plasma optical emission spectrometry (ICP-OES, method 1), the measurement range is shown in Table 1; inductance Coupled plasma mass spectrometry (ICP-MS, method 2), inductively coupled plasma tandem mass spectrometry (ICP-MS-MS, method 3), measurement range See Table 2.

When the analysis scopes of the three methods overlap, Method 2 is recommended as the arbitration method.

Note: The measurement range of the content range of rare earth impurities in rare earth metals is similar to the measurement range of the content range of rare earth oxide impurities in rare earth oxides.

At the same time, rare earth impurities in rare earth metals are measured as elemental substances.