YS/T 509.7-2008 English PDF (YST509.7-2008)

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YS/T 509.7-2008: Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of beryllium oxide content. Chromazurol S and cetyltrimethyl ammonium bromide spectrophotometric method
YS/T 509.7-2008
YS
NON-FERROUS METAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing YS/T 509.8-2006
Methods for Chemical Analysis of Spodumene and
Lepidolite Concentrates - Determination of Beryllium
Oxide Content - Chromazurol S and Cetyltrimethyl
Ammonium Bromide Spectrophotometric Method
ISSUED ON: MARCH 12, 2008
IMPLEMENTED ON: SEPTEMBER 1, 2008
Issued by: National Development and Reform Commission of China
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Method Summary ... 5 
3 Reagents ... 5 
4 Instruments ... 6 
5 Test Piece ... 6 
6 Analytical Procedures ... 6 
7 Calculation of Analysis Result ... 8 
8 Precision ... 8 
9 Quality Assurance and Control ... 9 
Foreword
YS/T 509 Methods for Chemical Analysis of Spodumene and Lepidolite Concentrates
is divided into 11 parts:
---Part 1: Determination of Lithium Oxide Sodium Oxide and Potassium Oxide
Contents - Flame Atomic Absorption Spectrometric Method;
---Part 2: Determination of Rubidium Oxide and Caesium Oxide Contents - Flame
Atomic Absorption Spectrometric Method;
---Part 3: Determination of Silicon Dioxide Content - Gravimetric - Molybdenum
Blue Photometric Method;
---Part 4: Determination of Aluminum Oxide Content - EDTA Compleximetric
Method;
---Part 5: Determination of Ferric Oxide Content - O-phenanthroline Photometric
Method and EDTA Compleximetric Method;
---Part 6: Determination of Phosphorus Pentoxide Content - The Molybdenum
Blue Photometric Method;
---Part 7: Determination of Beryllium Oxide Content - Chromazurol S and
Cetyltrimethyl Ammonium Bromide Spectrophotometric Method;
---Part 8: Determination of Calcium Oxide and Magnesium Oxide Content - Flame
Atomic Absorption Spectrometric Method;
---Part 9: Determination of Calcium Oxide and Magnesium Oxide Content - Flame
Atomic Absorption Spectrometric Method;
---Part 10: Determination of Manganous Oxide Content - Persulfate Oxidation
Photometric Method;
---Part 11: Determination of Loss on Ignition - Gravimetric Method.
This Part is Part 7.
This Part serves as a replacement of YS/T 509.8-2006 Methods for Chemical Analysis
of Spodumenite and Lepidolite Concentrates - The Chromazurol S and Cetyltrimethyl
Ammonium Bromide Photometric Method for the Determination of Beryllium Oxide
Content (the former GB/T 3885.8-1983).
In comparison with YS/T 509.8-2006, this Part mainly has the following changes:
---The text formatting is re-edited;
Methods for Chemical Analysis of Spodumene and
Lepidolite Concentrates - Determination of Beryllium
Oxide Content - Chromazurol S and Cetyltrimethyl
Ammonium Bromide Spectrophotometric Method
1 Scope
This Part specifies the method of determining beryllium oxide content in spodumene
and lepidolite concentrates.
This Part is applicable to the determination of beryllium oxide content in spodumene
and lepidolite concentrates. The range of determination is 0.01% ~ 1.00%.
2 Method Summary
Use hydrofluoric acid to decompose the sample and drive off silicon; use alkali to melt
it; use water to leach it. Beryllium is separated from elements like iron and manganese
in the state of sodium beryllate. Transfer-take part of the clear solution; adjust pH to
11. Beryllium forms a red ternary complex with Chromazurol S and CTMAB. At a
wavelength of 520 nm of the spectrophotometer, measure its absorbance. Use tartaric
acid, sodium citrate, EDTA and triethanolamine to jointly mask the interfering ions.
3 Reagents
Unless it is otherwise specified, only reagents that are confirmed to be analytically pure,
and distilled water or water of equivalent purity are used in the analysis.
3.1 Sodium hydroxide.
3.2 Hydrofluoric acid ( 1.15 g/mL).
3.3 Hydrochloric acid (1 + 4).
3.4 Sodium hydroxide solution (40 g/L).
3.5 Sodium hydroxide solution (10 g/L).
3.6 Sodium citrate solution (200 g/L).
3.7 Tartaric acid solution (150 g/L).
6.4.7 Add 2.0 mL of Chromazurol S solution (3.11) and 2.0 mL of CTMAB anhydrous
ethanol solution (3.12). Use water to dilute to the scale; mix it well. Let it stand for 45
min.
6.4.8 Transfer part of the solution (6.4.7) into a 1 cm cuvette; take the blank solution of
the accompanying sample as a reference. At a wavelength of 520 nm of the
spectrophotometer, measure its absorbance. Through the working curve, find out the
corresponding beryllium oxide content.
6.5 Drawing of Working Curve
6.5.1 Transfer-take 0 mL, 0.50 mL, 1.00 mL, 1.50 mL, 2.00 mL and 2.50 mL of beryllium
oxide standard solution (3.14). Respectively place them in a group of 50 mL beakers.
Proceed in accordance with the steps in 6.4.5 ~ 6.4.7.
6.5.2 Transfer part of the solution (6.5.1) into a 1 cm cuvette; take the reagent blank
as a reference. At a wavelength of 520 nm of the spectrophotometer, measure its
absorbance. Use beryllium oxide content as the x-coordinate; take its absorbance as
the y-coordinate; draw a working curve.
7 Calculation of Analysis Result
The mass fraction w of beryllium oxide, expressed in (%), shall be calculated in
accordance with Formula (1):
Where,
m1---the beryllium oxide content obtained through the working curve, expressed in (μg);
m0---the mass of the sample, expressed in (g);
V1---the volume of the transferred test solution, expressed in (mL);
V0---the total volume of the test solution, expressed in (mL).
8 Precision
8.1 Repeatability
In terms of the determined value of two independent test results obtained under
repeatability conditions, within the range of average value provided below, the absolute
difference between the two results does not exceed the repeatability limit (r); the
circumstance of exceeding the repeatability limit (r) does not exceed 5%. The