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YS/T 509.7-2008Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of beryllium oxide content. Chromazurol S and cetyltrimethyl ammonium bromide spectrophotometric method (English PDF)

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Issued by

National Development and Reform Commission of China

Level / Type

National · Recommended

Issue date

March 12, 2008

Implementation date

September 1, 2008

Scope

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) is available as an English-translated PDF.

YS/T 509.7-2008 - 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%.

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Document preview — YS/T 509.7-2008

National Standard of the People's Republic of China

ICS
77.120.99
Classification
H 64

Issued by: National Development and Reform Commission of China

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 (rho 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

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 9 pages — is available in the English PDF.

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