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Chemical analysis methods of ion type rare earth ore - Determination of total rare earth ion phase
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XB/T 619-2015: PDF in English (XBT 619-2015) XB/T 619-2015
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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
(REO) >99.5%, w (Yb2O3/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 ytterbium oxide.
2.2.18 Lutetium standard solution: Weigh 0.1000 g of lutetium oxide [w (REO) >99.5%,
w (Lu2O3/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 lutetium oxide.
2.2.19 Yttrium standard solution: Weigh 0.1000 g of yttrium oxide [w (REO) >99.5%,
w (Y2O3/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 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 yttrium oxide.
for 1 h.
3.2.18 Lutetium oxide: [w (REO) >99.5%, w (Lu2O3/REO) >99.99%], calcined at 950℃
for 1 h.
3.2.19 Yttrium oxide: [w (REO) >99.5%, w (Y2O3/REO) >99.99%], calcined at 950℃
for 1 h.
3.2.20 Cerium standard stock solution: Weigh 0.4000 g of cerium oxide (3.2.6) and
place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). Add 2 mL of hydrogen
peroxide (3.2.1). 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 4 mg of cerium oxide.
3.2.21 Samarium standard stock solution: Weigh 0.500 g of samarium oxide (3.2.9) and
place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 5 mg of
samarium oxide.
3.2.22 Europium standard stock solution: Weigh 0.300 g of europium oxide (3.2.10)
and place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 3 mg of
europium oxide.
3.2.23 Gadolinium standard stock solution: Weigh 0.4000 g of gadolinium oxide (3.2.11)
and place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 4 mg of
gadolinium oxide.
3.2.24 Terbium standard stock solution: Weigh 0.2000 g of terbium oxide (3.2.12) and
place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 2 mg of
terbium oxide.
3.2.25 Dysprosium standard stock solution: Weigh 0.3500 g of dysprosium oxide
(3.2.13) and place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 3.5 mg of terbium oxide.
3.2.26 Holmium standard stock solution: Weigh 0.4000 g of holmium oxide (3.2.14)
and place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 4 mg of
holmium oxide.
3.2.27 Erbium standard stock solution: Weigh 0.3000 g of erbium oxide (3.2.15) and
place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 3 mg of
erbium oxide.
3.2.28 Thulium standard stock solution: Weigh 0.2000 g of thulium oxide (3.2.16) and
place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 2 mg of
thulium oxide.
3.2.29 Ytterbium standard stock solution: Weigh 0.3000 g of ytterbium oxide (3.2.17)
and place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 3 mg of
ytterbium oxide.
3.2.30 Lutetium standard stock solution: Weigh 0.2000 g of lutetium oxide (3.2.18) and
place in a 100 mL beaker. Add 10 mL of nitric acid (3.2.3). 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 2 mg of
lutetium oxide.
3.2.31 Mixed standard stock solution of rare earth oxides: According to Table 5, weigh
the corresponding amount (≥50 mg) of single rare earth oxides (3.2.5~3.2.19) into a
250 mL beaker. Add 20 mL of hydrochloric acid (3.2.2) and 1 mL of hydrogen peroxide
(3.2.1) and heat to dissolve completely. Cool. Transfer to three 500 mL volumetric
flasks respectively. According to Table 5, transfer the corresponding amount (< 50 mg)
of standard stock solution (3.2.20~3.2.29). Combine into the 500 mL volumetric flask
with the same serial number. Add 40 mL of hydrochloric acid (3.2.2). Dilute to the scale
with water. Mix well. 1 mL of this solution contains 2 mg of rare earth oxides.
3.2.32 Argon [φ (Ar) >99.99%]
The test material is leached with ammonium sulfate solution and titrated with disodium
ethylenediaminetetraacetate (EDTA) standard solution at pH 5.5 using xylenol orange
as indicator.
4.2 Reagents and materials
4.2.1 Hydrochloric acid (analytical grade).
4.2.2 Acetylacetone (1+9).
4.2.3 Hydrochloric acid (1+4).
4.2.4 Ammonia water (1+4).
4.2.5 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 the scale with water. Mix well.
4.2.6 Sulfosalicylic acid solution (100 g/L): Weigh 100 g of sulfosalicylic acid solution
into a 500 mL beaker. Dissolve in 300 mL of water until clear. Transfer to a 1000 mL
volumetric flask. Dilute to the scale with water. Mix well.
4.2.7 Acetylacetone (1+9): Pipette 10 mL of acetylacetone (4.2.2) into a 100 mL
volumetric flask. Dilute to the scale with water. Mix well.
4.2.8 Hexamethylenetetramine solution (200 g/L): Weigh 200 g of
hexamethylenetetramine into a 500 mL beaker. Dissolve in 300 mL of water until clear.
Transfer to a 1000 mL volumetric flask. Add 25 mL of hydrochloric acid (4.2.1). Dilute
to the scale with water. Mix well. Each 100 mL contains 2.5 mL of hydrochloric acid.
4.2.9 Xylenol orange indicator (2 g/L): Weigh 0.2000 g of xylenol orange indicator into
a 250 mL beaker. Dissolve it in 100 mL (1 +1) ethanol solution.
4.2.10 Congo red test paper.
4.2.11 Zinc standard stock solution: Weigh 0.2000 g of metallic zinc [w (Zn) >99.9%]
into a 250 mL beaker. Dissolve in 20 mL hydrochloric acid (4.2.1) until clear. Cool.
Transfer to a 200 mL volumetric flask. Dilute to the scale with water. Mix well. 1 mL
of this solution contains 1 mg of zinc.
4.2.12 Zinc standard solution: Pipette 10 mL of zinc standard stock solution into a 100
mL volumetric flask. Dilute to the scale with water. Mix well. 1 mL of this solution
contains 0.1 mg of zinc.
4.2.13 EDTA standard solution (0.002 mol/L)
Preparation: Weigh 1.5 g of disodium ethylenediaminetetraacetate dried at 80°C for 2
h and dissolve it in 100 mL of water in a 250 mL beaker. Transfer to a 2000 mL
volumetric flask. Dilute to the scale with water. Mix well. Store in a plastic bottle.
Calibration: Pipette 20.00 mL of zinc standard solution (4.2.12) into a 300 mL conical
flask. Add 50 mL of water. Add a small piece of Congo red test paper. Use hydrochloric
acid (4.2.3) and ammonia water (4.2.4) to adjust the test paper to purple-red. The pH
value of the solution is 5~5.5. Add 5 mL of hexamethylenetetramine solution (4.2.8).
Add 2 drops of xylenol orange indicator (4.2.9). Titrate with EDTA standard solution
(4.2.13) until the solution changes from purple-red to bright yellow, which is the end
point. Two people measure 8 portions in parallel. The extreme difference of the volume
of EDTA standard solution (4.2.12) consumed should not exceed 0.10 mL. Take the
average value.
Calculate the concentration of EDTA solution according to formula (3):
Where,
c - EDTA solution concentration, in moles per liter (mol/L);
ρ - mass concentration of zinc standard solution, in milligrams per milliliter (mg/mL);
V1 - volume of zinc standard solution pipetted, in milliliters (mL);
V2 - volume of EDTA standard solution consumed during calibration, in milliliters (mL);
V3 - volume of EDTA standard solution consumed in blank determination, in milliliters
(mL);
M - molar mass of zinc, in grams per mole (g/mol).
4.3 Specimens
Grind the specimen to a particle size of less than 1 mm. Dry it in a drying oven at 105°C
for 1 h. Cool it to room temperature in a desiccator.
4.4 Analysis steps
4.4.1 Test material
Weigh 20.0 g of specimen (4.3) to an accuracy of 0.0001 g.
4.4.2 Number of measurements
Carry out two independent measurements. Take the average value.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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