GB/T 16484.3-2009 English PDF (GB/T16484.3-2009)

GB/T 16484.3-2009: Chemical Analysis Methods of Rare Earth Chloride and Light Rare Earth Carbonate - Part 3: Determination of Fifteen REO Relative Contents - Inductively Coupled Plasma Atomic Emission Spectrometry
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GB/T 16484.3-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 14
Replacing GB/T 16484.3-1996
Chemical Analysis Methods of Rare Earth Chloride and
Light Rare Earth Carbonate - Part 3: Determination of
Fifteen REO Relative Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry
ISSUED ON: OCTOBER 30, 2009
IMPLEMENTED ON: MAY 1, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 6 
2 Methods and Principles ... 6 
3 Reagents and Materials ... 7 
4 Instruments ... 9 
5 Test Samples ... 9 
6 Analytical Procedures ... 9 
7 Calculation and Expression of Analytical Result ... 11 
8 Precision ... 11 
9 Quality Assurance and Control ... 14 
Foreword
GB/T 16484-2009 Chemical Analysis Methods of Rare Earth Chloride and Light Rare
Earth Carbonate is divided into 22 parts in total:
---Part 1: Determination of Cerium Oxide Content - Ammonium Ferrous Sulfate
Titrimetry;
---Part 2: Determination of Europium Oxide Content - Inductively Coupled Plasma
Mass Spectrometry;
---Part 3: Determination of Fifteen REO Relative Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry;
---Part 4: Determination of Thorium Oxide Content - Arsenazo Ⅲ
Spectrophotometry;
---Part 5: Determination of Barium Oxide Content - Inductively Coupled Plasma
Atomic Emission Spectrometry;
---Part 6: Determination of Calcium Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 7: Determination of Magnesium Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 8: Determination of Sodium Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 9: Determination of Nickel Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 10: Determination of Manganese Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 11: Determination of Lead Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 12: Determination of Sulfate Radical;
---Part 13: Determination of Ammonium Chloride Content - Distillation-titrimetry;
---Part 14: Determination of Phosphorus Radical Content - Phosphorus-
antimonate-molybdenum Blue Spectrophotometry;
Chemical Analysis Methods of Rare Earth Chloride and
Light Rare Earth Carbonate - Part 3: Determination of
Fifteen REO Relative Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry
1 Scope
This Part of GB/T 16484 stipulates the determination method for 15 rare earth oxide
relative contents in rare earth chloride and light rare earth carbonate.
This Part is applicable to the determination of 15 rare earth oxide relative contents in
rare earth chloride and light rare earth carbonate. The range of determination is shown
in Table 1.
Table 1
2 Methods and Principles
Use hydrochloric acid to dissolve sample. In diluted hydrochloric acid medium, directly
use argon plasma light source for excitation; conduct spectrometry. Adopt coefficient
correction method to correct spectral interference among the elements being
determined.
Elements Determination Range (mass fraction)/%
Determination Range
(mass fraction)/% Elements
Yttrium Oxide
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
Transfer it into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1
mL of this solution contains 1 mg of dysprosium oxide.
3.15 Holmium oxide standard stock solution: weigh-take 0.1000 g of holmium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of holmium oxide.
3.16 Erbium oxide standard stock solution: weigh-take 0.1000 g of erbium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of erbium oxide.
3.17 Thulium oxide standard stock solution: weigh-take 0.1000 g of thulium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of thulium oxide.
3.18 Ytterbium oxide standard stock solution: weigh-take 0.1000 g of ytterbium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of ytterbium oxide.
3.19 Lutetium oxide standard stock solution: weigh-take 0.1000 g of lutetium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of lutetium oxide.
3.20 Yttrium oxide standard stock solution: weigh-take 0.1000 g of yttrium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of yttrium oxide.
3.21 Mixed rare earth standard solution: respectively transfer-take 5.00 mL of the
various rare earth oxide standard stock solutions (3.11 ~ 3.20). Respectively place
them into 100 mL volumetric flask; add 10 mL of hydrochloric acid (3.8); use water to
dilute to the scale; mix it up. 1 mL of this solution respectively contains 50.0 μg of the
various individual rare earth oxides.
3.22 Argon, purity > 99.99%.
4 Instruments
4.1 Inductively coupled plasma atomic emission spectrometer, resolution ratio < 0.006
nm (at 200 nm).
4.2 Light source: argon plasma source.
5 Test Samples
5.1 Preparation of rare earth chloride sample: smash the sample to pieces; promptly
place them into a weighing bottle; immediately weigh it.
5.2 Preparation of light rare earth carbonate: after sample is unsealed, immediately
weigh it.
6 Analytical Procedures
6.1 Test Portion
Weigh-take 2.00 g of the sample (5), accurate to 0.0001 g.
6.2 Times of Determination
Weigh-take two test portions for parallel determination; take the average value.
6.3 Blank Test
Conduct blank test along with the test portions.
6.4 Preparation of Analytical Test Solutions
6.4.1 Place the test portion (6.1) in a 200 mL beaker; add 10 mL of hydrochloric acid
(3.8). Heat it up, till it completely dissolves (if necessary, dropwise add hydrogen
peroxide (3.6) to facilitate the dissolution). Evaporate it, till it reaches near dryness.
Then, cool it down, transfer it into a 500 mL volumetric flask. Use water to dilute to the
scale, mix it up.
6.4.2 In accordance with the total amount of rare earth oxide contained in the test
portion, respectively take a certain volume of the solution, place it into a 50 mL
GB/T 16484.3-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 14
Replacing GB/T 16484.3-1996
Chemical Analysis Methods of Rare Earth Chloride and
Light Rare Earth Carbonate - Part 3: Determination of
Fifteen REO Relative Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry
ISSUED ON: OCTOBER 30, 2009
IMPLEMENTED ON: MAY 1, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 6 
2 Methods and Principles ... 6 
3 Reagents and Materials ... 7 
4 Instruments ... 9 
5 Test Samples ... 9 
6 Analytical Procedures ... 9 
7 Calculation and Expression of Analytical Result ... 11 
8 Precision ... 11 
9 Quality Assurance and Control ... 14 
Foreword
GB/T 16484-2009 Chemical Analysis Methods of Rare Earth Chloride and Light Rare
Earth Carbonate is divided into 22 parts in total:
---Part 1: Determination of Cerium Oxide Content - Ammonium Ferrous Sulfate
Titrimetry;
---Part 2: Determination of Europium Oxide Content - Inductively Coupled Plasma
Mass Spectrometry;
---Part 3: Determination of Fifteen REO Relative Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry;
---Part 4: Determination of Thorium Oxide Content - Arsenazo Ⅲ
Spectrophotometry;
---Part 5: Determination of Barium Oxide Content - Inductively Coupled Plasma
Atomic Emission Spectrometry;
---Part 6: Determination of Calcium Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 7: Determination of Magnesium Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 8: Determination of Sodium Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 9: Determination of Nickel Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 10: Determination of Manganese Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 11: Determination of Lead Oxide Content - Flame Atomic Absorption
Spectrometry;
---Part 12: Determination of Sulfate Radical;
---Part 13: Determination of Ammonium Chloride Content - Distillation-titrimetry;
---Part 14: Determination of Phosphorus Radical Content - Phosphorus-
antimonate-molybdenum Blue Spectrophotometry;
Chemical Analysis Methods of Rare Earth Chloride and
Light Rare Earth Carbonate - Part 3: Determination of
Fifteen REO Relative Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry
1 Scope
This Part of GB/T 16484 stipulates the determination method for 15 rare earth oxide
relative contents in rare earth chloride and light rare earth carbonate.
This Part is applicable to the determination of 15 rare earth oxide relative contents in
rare earth chloride and light rare earth carbonate. The range of determination is shown
in Table 1.
Table 1
2 Methods and Principles
Use hydrochloric acid to dissolve sample. In diluted hydrochloric acid medium, directly
use argon plasma light source for excitation; conduct spectrometry. Adopt coefficient
correction method to correct spectral interference among the elements being
determined.
Elements Determination Range (mass fraction)/%
Determination Range
(mass fraction)/% Elements
Yttrium Oxide
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
Transfer it into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1
mL of this solution contains 1 mg of dysprosium oxide.
3.15 Holmium oxide standard stock solution: weigh-take 0.1000 g of holmium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of holmium oxide.
3.16 Erbium oxide standard stock solution: weigh-take 0.1000 g of erbium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of erbium oxide.
3.17 Thulium oxide standard stock solution: weigh-take 0.1000 g of thulium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of thulium oxide.
3.18 Ytterbium oxide standard stock solution: weigh-take 0.1000 g of ytterbium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of ytterbium oxide.
3.19 Lutetium oxide standard stock solution: weigh-take 0.1000 g of lutetium oxide
, which is burned at 950 °C for 1 h. Place
it in a 100 mL beaker; add 10 mL of hydrochloric acid (3.8). At a low temperature, heat
it up, till it completely dissolves, then, cool it down to the room temperature. Transfer it
into a 100 mL volumetric flask; use water to dilute to the scale, mix it up. 1 mL of this
solution contains 1 mg of lutetium oxide.
...