GB/T 18115.4-2021Chemical 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 (English PDF)

Foreword

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

This document is the fourth part of GB/T 18115 "Methods for Chemical Analysis of Rare Earth Impurities in Rare Earth Metals and Their Oxides". GB/T 18115 The following parts have been released.

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

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

---Part 3: Determination of lanthanum, cerium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in praseodymium;

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

---Part 5: Determination of lanthanum, cerium, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in samarium;

---Part 6: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in europium;

---Part 7: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in gadolinium;

---Part 8: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in terbium;

---Part 9: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, holmium, erbium, thulium, ytterbium, lutetium and yttrium in dysprosium;

---Part 10: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, erbium, thulium, ytterbium, lutetium and yttrium in holmium;

---Part 11: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, thulium, ytterbium, lutetium and yttrium in erbium;

---Part 12: Determination of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium in yttrium;

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

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

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

This document replaces GB/T 18115.4-2006 "Methods for Chemical Analysis of Rare Earth Impurities in Rare Earth Metals and Their Oxides".

Determination of the amount of samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium", compared with GB/T 18115.4-2006, except for structural adjustment and editability In addition to the changes, the main technical changes are as follows.

a) Changed the measurement range of some rare earth oxides by inductively coupled plasma emission spectrometry (ICP-OES, method 1), praseodymium oxide The measurement range of europium oxide is changed from "0.0080%~0.200%" to "0.0100%~0.600%"; the measurement range of europium oxide is changed from "0.0050%~0.100%" is changed to "0.0005%~0.100%" (see Table 1,.2006 version of Table 1);

b) The measurement range of inductively coupled plasma mass spectrometry (ICP-MS, method 2) has been changed, and the measurement of lanthanum oxide, cerium oxide, and gadolinium oxide The range is changed from "0.0001%~0.050%" to "0.00002%~0.020%"; praseodymium oxide, samarium oxide, europium oxide, erbium oxide, The measurement range of thulium oxide, ytterbium oxide, lutetium oxide, and yttrium oxide is changed from "0.0001%~0.050%" to "0.00001%~ 0.020%"; the measurement range of terbium oxide, dysprosium oxide, and holmium oxide is changed from "0.0001%~0.050%" to "0.00005%~ 0.020%" (see Table 2, Table 7 of the.2006 edition);

c) Two chapters of "Normative Reference Documents" and "Terms and Definitions" have been added (see Chapter 2 and Chapter 3);

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

e) The pretreatment conditions of method 1 and method 2 samples have been changed from "900°C for 1h" to "105°C for 1h" (see 4.4.1, 5.4.1, 5.1, 14.1 of the.2006 edition);

f) The weighing amount of the sample in Method 1 is changed, in which the oxide sample is changed from 0.200g to 0.500g (see 4.5.1.1,.2006 edition 6.1.1), the metal sample was changed from 0.174g to 0.429g (see 4.5.1.2, 6.1.2 of the.2006 edition);

g) The blank test in Method 1 and the preparation of blank test series of standard solutions have been added (see 4.5.3, 4.5.4.2);

h) The reference spectrum of Method 1 is changed, and the spectrum of Erbium (Er) is changed from 346.220nm to 291.036nm, 337.271nm (see Table 3, Table 3 of the 2006 edition);

i) Part of the expression of precision is changed, and the allowable error is changed to reproducibility (see 4.8.2, 5.8.2, 8.2, 17.2 of the 2006 edition);

j) The instrument requirements of Method 1 and Method 2 are changed (see 4.3, 5.3, 4.1, 4.2, 13.1 of the 2006 edition);

k) Added the reagents required for method 2 determination, including thallium chloride, hydrochloric acid (2.4%), hydrochloric acid (0.331mol/L), thallium internal standard solution, cesium Mix internal standard solution with thallium (see 5.2.3, 5.2.10, 5.2.12, 5.2.34, 5.2.35);

l) The internal standard elements in the analysis of Method 2 (see 5.5.4, 5.5.5.2, 5.5.5.3.2, 15.4.2, 15.4.3. 15.5);

m) The concentration of method 2 hydrochloric acid eluent is changed, 0.020mol/L is changed to 0.0050mol/L (see 5.2.13, 2006 edition 12.10);

n) Change the rare earth impurity content of the sample of Method 2 and the sample amount to analyze and weigh (see Table 11, Table 8 of the 2006 edition);

o) Change the flow rate of the eluent line of method 2, change "(1.5±0.1)mL/min" to "(1.0±0.1)mL/min"; change The elution time is changed, 20min is changed to 30min; the volume of the collected separation liquid is changed, and the "10mL colorimetric tube" is changed to "10mL or 50mL colorimetric tube" (see 5.5.5.3.1, 5.5.5.3.2, 15.4.3.1, 15.4.3.2 of 2006 edition);

p) Added remarks on the method of adding internal standard in Method 2 (see 5.5.4, 5.5.5.2, 5.5.5.3.2, 5.5.5.4.2, 5.6.2);

q) Added the preparation of the analysis test solution after the TODGA load matrix is separated in the determination of Method 2 (see 5.5.5.4);

r) Deleted quality assurance and control (see Chapter 9 and Chapter 18 of the 2006 edition);

s) Method 3 Inductively Coupled Plasma Tandem Mass Spectrometry (ICP-MS-MS, Method 3) has been added (see Chapter 1, Chapter 6).

Introduction

In the field of analysis of the chemical composition of rare earth products, China has established a test for the total amount of rare earths, non-rare earth impurities, and rare earth impurities.

It is a comprehensive standard system. This series of standards GB/T 18115 "Chemical Analysis Methods of Rare Earth Impurities in Rare Earth Metals and Their Oxides" is based on the original standard Standard GB/T 18115.1~.10-2000 and GB/T 12690.1~.11-1990 as the basis, combined with other relevant standards to form a pair of (Except scandium and promethium) Comprehensive analysis method of rare earth impurities in 15 kinds of rare earth metals and their oxides. This series of standards covers 15 kinds of rare earth elements Element matrix, each element matrix uses 14 kinds of rare earth impurities, respectively, using inductively coupled plasma spectroscopy (ICP-OES), inductively coupled plasma Mass spectrometry (ICP-MS) is used for the determination. Due to the characteristics of rare earths, the interference of rare earth matrix and adjacent elements, trace rare earths in high-purity rare earths The analysis of impurity elements has always been a difficult problem in the field of analytical chemistry. This series of standards has passed a series of scientific tests, On the basis of inspection and verification, the best separation technology is selected and the best test method is explored. In particular, inductive coupling has been added in this revision Plasma tandem mass spectrometry (ICP-MS-MS) solves the problem of the analysis of trace rare earth impurity elements in high-purity rare earths, and meets the needs of new materials And the need for equipment manufacturing has enhanced the applicability of the standard.

Rare earth impurities in rare earth metals and their oxides Chemical analysis methods part 4.

1 Scope

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

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

This document also applies to lanthanum oxide, cerium oxide, praseodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, oxide Determination of holmium, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide content.

This document contains 3 methods. inductively coupled plasma emission spectroscopy (ICP-OES, method 1), inductively coupled plasma mass spectrometry (ICP-OES, method 1), Spectroscopy (ICP-MS, Method 2), Inductively Coupled Plasma Tandem Mass Spectrometry (ICP-MS-MS, Method 3). For the measurement range of Method 1, see Table 1, Method 2 and Method 3's measurement range are shown in Table 2.

When the analysis scope of the three methods overlaps, method 2 is preferred as the arbitration method.

Note: The mass fraction of the content range of rare earth impurities in rare earth metals is the same as the mass fraction of the content range of rare earth oxide impurities in rare earth oxides.

Rare earth impurities in rare earth metals are calculated as elements.