XB/T 619-2015 English PDF (XBT619-2015)

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XB/T 619-2015: Chemical analysis methods of ion type rare earth ore. Determination of total rare earth ion phase
XB/T 619-2015
XB
RARE EARTH INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 14
Chemical analysis methods of ion type rare earth ore -
Determination of total rare earth ion phase
ISSUED ON: APRIL 30, 2015
IMPLEMENTED ON: OCTOBER 01, 2015
Issued by: Ministry of Industry and Information Technology of the People's
Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Method 1: Inductively Coupled Plasma Mass Spectrometry ... 4
3 Method 2: Inductively Coupled Plasma Atomic Emission Spectrometry ... 9
4 Method 3: EDTA Volumetric Method ... 16
5 Quality assurance and control ... 20
Chemical analysis methods of ion type rare earth ore -
Determination of total rare earth ion phase
1 Scope
This Standard specifies the method for determining total rare earth ion phase in ion type
rare earth ore.
This Standard is applicable to the determination of total rare earth ion phase in ion type
rare earth ore. It includes 3 methods: Method 1 Inductively Coupled Plasma Mass
Spectrometry; Method 2 Inductively Coupled Plasma Atomic Emission Spectrometry
and Method 3 EDTA Volumetric Method. The measurement range of Method 1 is:
0.010%~0.50%. The measurement range of Method 2 is: 0.020%~0.50%. The
measurement range of Method 3 is: 0.020%~0.50%. Among them, Method 3 is not
applicable to the determination of samples with an iron content greater than 10 after
leaching or a copper content greater than 5 [Translator’s note: This sentence of original
Chinese is ambiguous and incomprehensible].
2 Method 1: Inductively Coupled Plasma Mass Spectrometry
2.1 Method principle
The test material is leached with ammonium sulfate solution. In dilute nitric acid
medium, argon plasma is used as the ionization source. The mass fractions of fifteen
rare earth elements are determined by mass spectrometry. The sum of the mass fractions
is the total rare earth ion phase. Use the internal standard method to perform calibration.
2.2 Reagents and materials
2.2.1 Hydrogen peroxide (analytical grade).
2.2.2 Nitric acid [high purity (MOS)].
2.2.3 Nitric acid (1+1) (prepared with MOS grade nitric acid).
2.2.4 Ammonium sulfate solution (20 g/L): Weigh 20 g of ammonium sulfate into a 500
mL beaker. Dissolve in 300 mL of water until clear. Transfer to a 1000 mL volumetric
flask. Dilute to volume with water. Mix well.
2.2.5 Lanthanum standard solution: Weigh 0.1000 g of lanthanum oxide [w
(REO) >99.5%, w (La2O3/REO) >99.99%] calcined at 950°C for 1 h and place in a 100
mL beaker. Add 10 mL of nitric acid (2.2.3). Add 2 mL of hydrogen peroxide (2.2.1).
Heat at low temperature until they are completely dissolved. Remove and cool. Transfer
the solution to a 100 mL volumetric flask. Dilute to the scale with water. Mix well. 1
mL of this solution contains 1000 μg of lanthanum oxide.
2.2.6 Cerium standard solution: Weigh 0.1000 g of cerium oxide [w (REO) >99.5%, w
(CeO2/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL beaker. Add 10 mL of
nitric acid (2.2.3). Add 2 mL of hydrogen peroxide (2.2.1). Heat at low temperature
until they are completely dissolved. Remove and cool. Transfer the solution to a 100
mL volumetric flask. Dilute to the scale with water. Mix well. 1 mL of this solution
contains 1000 μg of cerium oxide.
2.2.7 Praseodymium standard solution: Weigh 0.1000 g of praseodymium oxide [w
(REO) >99.5%, w (Pr6O11/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL beaker.
Add 10 mL of nitric acid (2.2.3). Heat at low temperature until they are dissolved.
Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to the scale
with water. Mix well. 1 mL of this solution contains 1000 μg of praseodymium oxide.
2.2.8 Neodymium standard solution: Weigh 0.1000 g of neodymium oxide [w
(REO) >99.5%, w (Nd2O3/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL beaker.
Add 10 mL of nitric acid (2.2.3). Heat at low temperature until they are dissolved.
Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to the scale
with water. Mix well. 1 mL of this solution contains 1000 μg of neodymium oxide.
2.2.9 Samarium standard solution: Weigh 0.1000 g of samarium oxide [w
(REO) >99.5%, w (Sm2O3/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL
beaker. Add 10 mL of nitric acid (2.2.3). Heat at low temperature until they are
dissolved. Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute
to the scale with water. Mix well. 1 mL of this solution contains 1000 μg of samarium
oxide.
2.2.10 Europium standard solution: Weigh 0.1000 g of europium oxide [w
(REO) >99.5%, w (Eu2O3/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL beaker.
Add 10 mL of nitric acid (2.2.3). Heat at low temperature to dissolve until clear.
Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to the scale
with water. Mix well. 1 mL of this solution contains 1000 μg of europium oxide.
2.2.11 Gadolinium standard solution: Weigh 0.1000 g of gadolinium oxide [w
(REO) >99.5%, w (Gd2O3/REO) >99.99%] calcined at 950 °C for 1 h in a 100 mL
beaker. Add 10 mL of nitric acid (2.2.3). Heat at low temperature to dissolve until clear.
Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to volume
with water. Mix well. 1 mL of this solution contains 1000 μg of gadolinium oxide.
2.2.12 Terbium standard solution: Weigh 0.1000 g of terbium oxide [w (REO) >99.5%,
w (Tb4O7/REO) >99.99%] calcined at 950°C for 1 h and place in a 100 mL beaker. Add
10 mL of nitric acid (2.2.3). Add 2 mL of hydrogen peroxide (2.2.1). Heat at low
temperature until they are dissolved. Remove and cool. Transfer the solution to a 100
mL volumetric flask. Dilute to the scale with water. Mix well. 1 mL of this solution
contains 1000 μg of terbium oxide.
2.2.13 Dysprosium standard solution: Weigh 0.1000 g of dysprosium oxide [w
(REO) >99.5%, w (Dy2O3/REO) >99.99%] calcined at 950℃ for 1 h in a 100 mL beaker.
Add 10 mL of nitric acid (2.2.3). Heat at low temperature to dissolve until clear.
Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to the scale
with water. Mix well. 1 mL of this solution contains 1000 μg of dysprosium oxide.
2.2.14 Holmium standard solution: Weigh 0.1000 g of holmium oxide [w
(REO) >99.5%, w (Ho2O3/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL beaker.
Add 10 mL of nitric acid (2.2.3). Heat at low temperature until they are dissolved.
Remove and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to the scale
with water. Mix well. 1 mL of this solution contains 1000 μg of holmium oxide.
2.2.15 Erbium standard solution: Weigh 0.1000 g of erbium oxide [w (REO) >99.5%,
w (Er2O3/REO) >99.99%] calcined at 950℃ for 1 h and place in a 100 mL beaker. Add
10 mL of nitric acid (2.2.3). Heat at low temperature to dissolve until clear. Remove
and cool. Transfer the solution to a 100 mL volumetric flask. Dilute to the scale with
water. Mix well. 1 mL of this solution contains 1000 μg of erbium oxide.
2.2.16 Thulium standard solution: Weigh 0.1000 g of thulium oxide [w (REO) >99.5%,
w (Tm2O3/REO) >99.99%] calcined at 950°C for 1 h in a 100 mL beaker. Add 10 mL
of nitric acid (2.2.3). Heat at low temperature until dissolved. Remove and cool.
Transfer the solution to a 100 mL volumetric flask. Dilute to the scale with water. Mix
well. 1 mL of this solution contains 1000 μg of thulium oxide.
2.2.17 Ytterbium standard solution: Weigh 0.1000 g of ytterbium oxide [w