AS 2503.3-2006

Header

About this publication

Preface

1 Scope and general

1.1 Scope

1.2 Referenced documents

1.3 Definition

1.4 Repeatability

1.5 Principle

1.5.1 Loss on ignition (see Section 3)

1.5.2 Determination of silicon, phosphorus, aluminium, iron (III), titanium, manganese, calcium and magnesium oxides (see Section 4)

1.5.3 Determination of sodium, potassium and lithium oxides (see Section 5)

1.6 Safety

2 Sampling and sample preparation

2.1 Scope of Section

2.2 Gross sampling

2.3 Preparation of sample

2.3.1 Crushing

2.3.1.1 Bricks

2.3.1.2 Ground materials

2.3.2 Samples for analysis

2.3.2.1 Preliminary treatment

2.3.2.2 Portion A—to be used for the main analysis

2.3.2.3 Portion B—to be used where iron determination is required

3 Determination of loss on ignition

3.1 Scope of Section

3.2 Apparatus

3.2.1 Balance

3.2.2 Muffle furnace

3.2.3 Drying oven

3.3 Procedure

4 Determination of silicon, phosphorus, aluminium, iron (III), titanium, manganese, calcium and magnesium oxides

4.1 Scope of Section

4.2 Reagents

4.2.1 General

4.2.2 Solid reagents

4.2.2.1 Boric acid.

4.2.2.2 Potassium carbonate/sodium carbonate, anhydrous, mixed in equimolecular proportions.

4.2.2.3 Potassium pyrosulphate.

4.2.3 Solutions

4.2.3.1 Ammonia solution (ς20 880 kg/m3).

4.2.3.2 Ammonia solution (500 mL/L)

4.2.3.3 Ammonium acetate buffer solution.

4.2.3.4 Ammonium acetate buffer solution (100 g/L)

4.2.3.5 Ammonium meta-vanadate solution (2.5 g/L).

4.2.3.6 Ammonium molybdate solution (100 g/L).

4.2.3.7 Ammonium persulphate solution (100 g/L).

4.2.3.8 Base solution

4.2.3.9 Chloroform.

4.2.3.10 Cupferron solution (60 g/L)

4.2.3.11 Ethanol or industrial alcohol (950 mL/L)

4.2.3.12 Hydrochloric acid (ς20 1180 kg/m3).

4.2.3.13 Hydrochloric acid (500 mL/L)

4.2.3.14 Hydrochloric acid (200 mL/L)

4.2.3.15 Hydrochloric acid (50 mL/L)

4.2.3.16 Hydrofluoric acid (ς20 1130 kg/m3).

4.2.3.17 Hydrogen peroxide solution (60 g/L)

4.2.3.18 Hydroxylammonium chloride solution (100 g/L)

4.2.3.19 Nitric acid (ς20 1420 kg/m3).

4.2.3.20 Nitric acid (330 mL/L)

4.2.3.21 Perchloric acid (ς20 1540 kg/m3).

4.2.3.22 1,10-Phenanthroline solution (10 g/L)

4.2.3.23 Phosphoric acid (400 mL/L)

4.2.3.24 Potassium hydroxide solution (250 g/L)

4.2.3.25 Sodium nitrite solution (50 g/L)

4.2.3.26 Sorbitol solution (80 g/L)

4.2.3.27 Sulphuric acid (500 mL/L)

4.2.3.28 Sulphuric acid (100 mL/L)

4.2.3.29 Tin(II) chloride solution (10 g/L)

4.2.3.30 Triethanolamine solution (500 mL/L)

4.2.4 Standard solutions

4.2.4.1 Calcium solution (1 mL = 1.0 mg CaO)

4.2.4.2 EDTA solution (0.05 mol/L approx.)

4.2.4.3 EDTA solution (0.01 mol/L approx.)

4.2.4.4 Iron(III) solution (1 mL = 1.0 mg Fe2O3)

4.2.4.5 Iron(III) solution (1 mL = 0.01 mg Fe2O3)

4.2.4.6 Magnesium solution (1 mL = 1.0 mg MgO)

4.2.4.7 Manganese(II) solution (1 mL = 1.0 mg MnO)

4.2.4.8 Manganese(II) solution (1 mL = 0.01 mg MnO)

4.2.4.9 Phosphorus solution (1 mL = 1.0 mg P2O5)

4.2.4.10 Phosphorus solution (1 mL = 0.1 mg P2O5)

4.2.4.11 Silicon solution (1 mL = 0.5 mg SiO2)

4.2.4.12 Silicon solution (1 mL = 0.04 mg SiO2)

4.2.4.13 Titanium(IV) solution (1 mL = 0.8 mg TiO2)

4.2.4.14 Titanium(IV) solution (1 mL = 0.08 mg TiO2)

4.2.4.15 Zinc solution (0.05 mol/L)

4.2.5 Indicators

4.2.5.1 Dithizone solution (0.25 g/L)

4.2.5.2 Methyl orange solution (0.5 g/L).

4.2.5.3 Methylthymol blue complexone

4.2.5.4 Phenolphthalein solution (10 g/L)

4.2.5.5 Screened calcein

4.3 Apparatus

4.3.1 Steam bath

4.3.2 Glassware

4.3.3 Platinum dish

4.3.4 UV—Visible spectrometer

4.4 Procedure

4.4.1 Blank determination

4.4.2 Preparation of the sample solution

4.4.3 Determination of silicon dioxide

4.4.3.1 Gravimetric determination of insoluble silicon dioxide

4.4.3.2 Spectrometric determination of soluble silicon dioxide

4.4.3.3 Calculation of total silicon dioxide content

4.4.4 Determination of phosphorous pentoxide

4.4.5 Determination of aluminium oxide

4.4.6 Determination of iron(III) oxide

4.4.7 Determination of titanium dioxide

4.4.8 Determination of manganese oxide

4.4.9 Determination of calcium oxide

4.4.10 Determination of magnesium oxide

5 Determination of sodium, potassium and lithium oxides

5.1 Scope of Section

5.2 Reagents

5.2.1 General

5.2.2 Solutions

5.3 Apparatus

5.4 Procedure

5.4.1 Preliminary procedures

5.4.1.1 Blank determination

5.4.1.2 Solution of the sample

6 Test report

Appendix A

A1 Loss on ignition, SiO2, P2O5, Al2O3, Fe2O3, TiO2, MnO, CaO, MgO.

A2 Na2O, K2O, Li2O.

AS 2503.3-1985

AS 2503.3-2006 Rec:2017

DR 06087