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YS/T 509.9-2008Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of fluorine content. Ion selective electrode 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 509.9-2008 (Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of fluorine content. Ion selective electrode method) is available as an English-translated PDF.

YS/T 509.9-2008 — This Part specifies the determination method of fluorine content in spodumene and lepidolite concentrates. This Part is applicable to the determination of fluorine content in spodumene and lepidolite concentrates. Measurement range: 1.00%~10.00%.

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Document preview — YS/T 509.9-2008

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 Summary of Method...5
  • 3 Reagents...5
  • 4 Instrument...6
  • 5 Specimen...6
  • 6 Analysis Procedures...7
  • 7 Calculation of the Analysis Results...8
  • 8 Precision...8
  • 9 Quality Assurance and Control...9

Foreword

YS/T 509 Methods for chemical analysis of spodumene and lepidolite concentrates

consists of the following 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 met;

--- Part 8: Determination of calcium oxide and magnesium oxide content - Flame

atomic absorption spectrometric method;

--- Part 9: Determination of fluorine content - Ion selective electrode 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 9.

This Part replaced YS/T 509.10-2006 Methods for Chemical Analysis of Spodumene

and Lepidolite Concentrates - The Ion Selective Electrode Method for the

Determination of Fluorine Content in Lepidolite Concentrates (original GB/T 3885.10-

1983).

Compared with YS/T 509.10-2006, the major changes of this Part are as follows:

--- Re-edit the text format;

Methods for Chemical Analysis of Spodumene

and Lepidolite Concentrates - Determination of

Fluorine Content - Ion Selective Electrode Method

1 Scope

This Part specifies the determination method of fluorine content in spodumene and

lepidolite concentrates.

This Part is applicable to the determination of fluorine content in spodumene and

lepidolite concentrates. Measurement range: 1.00%~10.00%.

2 Summary of Method

The test material is melted and decomposed with sodium hydroxide and sodium

peroxide. In the sodium citrate-potassium nitrate complex buffer solution with pH 7, the

standard addition method is used to determine fluorine with a fluoride ion selective

electrode.

Aluminum seriously interferes with the determination of fluorine. Add the sodium

citrate-potassium nitrate mixed solution to the alkaline solution and adjust to pH 7,

which can eliminate the interference of 10mg of aluminum oxide.

3 Reagents

Unless otherwise specified, only reagents and distilled water confirmed to be

analytically pure or water of equivalent purity are used in the analysis.

3.1 Sodium peroxide.

3.2 Sodium hydroxide.

3.3 Sodium hydroxide solution (20g/L).

3.4 Hydrochloric acid (1+1).

3.5 Hydrochloric acid (1+49).

6 Analysis Procedures

6.1 Test material

Weigh 0.20g of specimen, accurate to 0.0001g.

6.2 The number of determinations

Make parallel determinations of two portions of test materials, and take the average

value.

6.3 Blank test

Do a blank test with the test materials.

6.4 Determination

6.4.1 Place the test material (6.1) in a 30mL nickel crucible; add 3g of sodium hydroxide

(3.2) and 0.5g of sodium peroxide (3.1); drive off the water on the electric furnace. And

place it in a high temperature furnace at 600°C~650°C for 5min~10min to melt; take it

out; and cool.

6.4.2 Clean the outer wall of the crucible with filter paper; place it in a 250mL beaker;

cover the watch glass; soak the melt with hot water; wash the crucible; take it out; and

cool the solution to room temperature.

6.4.3 Transfer the solution (6.4.2) into a 250mL volumetric flask; dilute to the mark with

water; mix well; and let stand.

6.4.4 Pipette 10.00mL of supernatant (6.4.3); put it in a 50mL beaker; add 10mL of

sodium citrate-potassium nitrate mixed solution (3.6); adjust the pH to 7 with

hydrochloric acid (3.4 and 3.5) and sodium hydroxide solution (3.3) on the acidimeter.

Then transfer the solution into a 50mL volumetric flask, dilute to the mark with water

and mix well.

6.4.5 Pour all the test solution (6.4.4) into a 100mL dry beaker; place it on the

electromagnetic stirrer; insert the fluorine electrode and calomel electrode; switch on

the ion meter; measure its dynamic equilibrium potential' and record millivolt value (E1).

Then add 0.20mL~0.50mL of fluorine standard solution (3.7.1) with a micropipette;

measure its dynamic equilibrium potential; and record the millivolt value (E2). The

added amount of fluorine standard solution (3.7.1) shall be such that the value of E1-

E2 is between 15mV~40mV.

NOTE 1: During the measurement process, the temperature shall be kept consistent.

......

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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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