[bs 1016-104.2-1991] -- methods for analysis and testing of coal and coke..pdf

8/10/2019 [BS 1016-104.2-1991] -- Methods for analysis and testing of coal and coke..pdf

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BRITISH STANDARD BS 1016-104.2:1991

Methods for

Analysis and testing of

coal and coke

Part 104: Proximate analysis

Section 104.2 Determination ofmoisture content of the general analysissample of coke


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BS 1016-104.2:1991

This British Standard, havingbeen prepared under thedirection of the Solid MineralFuels Standards PolicyCommittee, was published underthe authority of the StandardsBoard and comes into effect on30 April 1991

BSI 07-1999

First published as BS 1016-4,March 1942

Second edition May 1957

Third edition October 1965

Fourth edition October 1973

Fifth edition as BS 1016-104.2,April 1991

The following BSI referencesrelate to the work on thisstandard:

Committee reference SFC/3

Draft for comment 90/53515 DC

ISBN 0 580 19470 1

Committees responsible for thisBritish Standard

The preparation of this British Standard was entrusted by the Solid Mineral

Fuels Standards Policy Committee (SFC/-) to Technical Committee SFC/3,upon which the following bodies were represented:

British Cement Association

British Coal Corporation

British Gas plc

British Steel Industry

Department of Trade and Industry (Standards and Quality Policy Unit,Quality, Design and Education Division)

Electricity Supply Industry in United Kingdom

GAMBICA (BEAMA Ltd.)

Institute of British FoundrymenInstitute of Petroleum

Power Generation Contractors Association (BEAMA Ltd.)

Amendments issued since publication

Amd. No. Date Comments


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BS 1016-104.2:1991

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Contents

Page

Committees responsible Inside front cover

Foreword ii0 Introduction 1

1 Scope 1

2 Definitions 1

3 Principle 1

4 Reagent 1

5 Apparatus 1

6 Preparation of test sample 1

7 Procedure 1

8 Expression of results 2

9 Precision 2

10 Test report 2Publication(s) referred to Inside back cover


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BS 1016-104.2:1991

ii BSI 07-1999

Foreword

This Section of BS 1016 has been prepared under the direction of the SolidMineral Fuels Standards Policy Committee. Part 104 is a revision of the 1973editions of BS 1016-3 and BS 1016-4, which are superseded and withdrawn. This

Section replaces clause 4in BS 1016-4:1973, from which the principal changesare the omission of the direct gravimetric method (in 4.2) and the replacement ofdrying in nitrogen (in 4.3) by heating in air and then cooling in nitrogen.

Part 104 is a further Part numbered under a scheme for rationalizing andrestructuring BS 1016. The new series, when complete, will begin with Part 100,which will include a general introduction. The earlier series of Parts is as follows,with the new Part numbers (which will be given to revisions when they arepublished) in parentheses.

Part 1: Total moisture of coal (Part 101);

Part 2: Total moisture of coke (Part 102);

Part 5: Gross calorific value of coal and coke (Part 105);

Part 6: Ultimate analysis of coal (Part 106);Part 7: Ultimate analysis of coke (Part 106);

Part 8: Chlorine in coal and coke (Part 106);

Part 9: Phosphorus in coal and coke (Part 106);

Part 10: Arsenic in coal and coke (Part 106);

Part 11: Forms of sulphur in coal (Part 106);

Part 12: Caking and swelling properties of coal (Part 107);

Part 13: Tests special to coke (Part 108);

Part 14: Analysis of coal ash and coke ash (Part 114);

Part 15: Fusibility of coal ash and coke ash (Part 113);

Part 16: Methods for reporting results (Part 100);

Part 17: Size analysis of coal (Part 109);

Part 18: Size analysis of coke (Part 110);

Part 20: Determination of Hardgrove grindability index of hard coal(Part 112);

Part 21: Determination of moisture-holding capacity of hard coal (Part 103).

The following Parts in the new series have been published.

Part 104: Proximate analysis;

Part 111: Determination of abrasion index of coal.

Part 104 is divided into four Sections as follows.

Section 104.1: Determination of moisture content of the general analysis

sample of coal; Section 104.2: Determination of moisture content of the general analysissample of coke;

Section 104.3; Determination of volatile matter content;

Section 104.4: Determination of ash.

This Section is related to ISO 687:1974, published by the InternationalOrganization for Standardization (ISO). The principal difference is that in themethod described in ISO 687 the weighing dish is cooled in a desiccator insteadof in an atmosphere of nitrogen.


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There may be alternative methods for carrying out this determination which aremore rapid and/or less labour-intensive than the reference method described in

this Section of BS 1016. Work is in hand on the preparation of a standard for thevalidation of such alternative methods. It is important to demonstrate that analternative method is free from bias when compared to this reference method, andwill give a level of repeatability which is the same as or better than that quotedfor the reference method (see clause 9).

WARNING NOTE. This British Standard does not necessarily detail all theprecautions necessary to comply with the requirements of the Health and Safetyat Work etc. Act 1974 or the Control of Substances Hazardous to HealthRegulations 1988. Attention should be paid to any appropriate precautions andthe method should be operated only by trained personnel.

A British Standard does not purport to include all the necessary provisions of acontract. Users of British Standards are responsible for their correct application.

Compliance with a British Standard does not of itself confer immunityfrom legal obligations.

Summary of pages

This document comprises a front cover, an inside front cover, pages i to iv,

pages 1 and 2, an inside back cover and a back cover.This standard has been updated (see copyright date) and may have hadamendments incorporated. This will be indicated in the amendment table on theinside front cover.


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iv blank


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BS 1016-104.2:1991

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0 Introduction

As coke is hygroscopic, its moisture content will

vary with change of humidity of the atmosphere.Therefore, the moisture in the general analysissample has to be determined whenever portions areweighed out for other analytical determinations(for example, volatile matter content, calorificvalue, cabon and hydrogen content) and whenresults are required on a dry basis. If all the portionstaken for analysis are weighed out on the same dayand at about the same time, one test for moisturecontent should suffice.

1 Scope

This Section of BS 1016 describes a referencemethod for determining the moisture content of thegeneral analysis sample of coke.

NOTE The titles of the publications referred to in this standardare listed on the inside back cover.

2 Definitions

For the purposes of this Section of BS 1016, thedefinitions given in BS 1017-2 apply, together withthe following.

moisture in the general analysis sample

moisture content of the general analysis sample of a

solid mineral fuel after it has attained approximateequilibrium with the atmosphere in the laboratoryand which is removable under specified conditions

3 Principle

A known mass of the coke is heated in air atbetween 190 C and 210 C (see note 1 to 7.2) andmaintained at this temperature until constant inmass. The moisture content is calculated from theloss in mass of the coke.

4 Reagent

4.1 Nitrogen,dry and containing less than 10L ofoxygen per litre.

5 Apparatus

5.1Balance,capable of weighing to thenearest 0.1 mg.

5.2Air oven,capable of maintaining a temperaturewithin the range 190 C to 210 C (see note 1 to 7.2)and in which the atmosphere changes from 3 timesto 8 times per hour.

5.3 Weighing dishes,shallow, of glass withground-on covers or of corrosion-resistant metal

with well-fitting covers, of such a size that the massof coke per unit area does not exceed 0.15 g/cm2(see note 2 to 7.2).

5.4 Cooling vessel,with provision for the nitrogen topass through it at about 15 volumes per hour.

NOTE The provision of a metal plate, preferably of aluminium,inside the vessel will increase the rate of cooling.

6 Preparation of test sample

The coke used for the determination of moisturecontent is the general analysis sample, ground topass a sieve of 212m aperture (see BS 1017-2).Expose the sample in a thin layer for the minimumtime required for the moisture content to reachapproximate equilibrium with the laboratoryatmosphere.

Immediately before weighing out the test portion(see 7.1), mix the test sample for not less

than 1 min, preferably by mechanical means.

7 Procedure

7.1 Test portion

Weigh, to the nearest 0.1 mg, a clean, dry, emptyweighing dish (5.3) with its cover. Add 1 g to 2 g ofthe test sample to the dish in an even layer andreweigh the dish, cover and test portion to thenearest 0.1 mg.

7.2 Determination

Transfer the dish containing the test portion

(see 7.1), without its cover, to the oven (5.2),preheated to a temperature within the range 190 Cto 210 C (see note 1), and heat the dish at thattemperature for a minimum of 60 min (see notes 2and 3). Remove the dish from the oven and replaceits cover. Transfer the dish to the cooling vessel (5.4)through which the nitrogen (4.1) is passing atabout 15 volumes per hour, and weigh the dish, tothe nearest 0.1 mg, when cool.

For further periods each of at least 10 min, reheatthe dish without its cover at the same temperatureas before, then cool and reweigh it with its cover tothe nearest 0.1 mg, until any further change in

mass on successive weighings does not exceed 1 mg.

NOTE 1 The time taken for the determination can beconsiderably shortened if drying is carried out at a temperatureof 320 C in an atmosphere of nitrogen, when heating for 1 h willusually suffice.

NOTE 2 The mass per unit area of the coke layer may beincreased up to 0.25 g/cm2, provided that the heating time isincreased sufficiently (see note 3).

NOTE 3 Heating for 4 h is normally sufficient if the mass ofcoke per unit area does not exceed 0.15 g/cm2, but if the mass perunit area is 0.25 g/cm2, 6 h will probably be required.


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8 Expression of results

The moisture content of the coke, expressed as a

percentage by mass, is given by the formula:

where

m1is the mass of the empty dish plus

cover (in g);

m2is the mass of the dish plus cover plus coke

before heating (in g);

m3is the mass of the dish plus cover plus coke

after heating (in g).Report the result to the nearest 0.1 % (m/m).

NOTE It is recommended that the result is calculated as themean of duplicate determinations.

9 Precision

9.1 Repeatability

The results of duplicate determinations, carried outin the same laboratory by the same operator withthe same apparatus on representative portionsweighed out at the same time from the same testsample, should not differ by more than 0.1 % (m/m).

9.2 ReproducibilitySince the humidity conditions in differentlaboratories will vary, it is not practical to quote alimiting value for reproducibility.

10 Test report

The test report shall include the following:

a) the identification of the sample;

b) the reference to the methodused, i.e. BS 1016-104.2:1991;

c) the results expressed in accordance withclause 8;

d) any unusual features noted during thedetermination;

e) any operations not specified in this standard orregarded as optional.

m2 m3

m2 m1---------------------- 100


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BS 1016-104.2:1991

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Publication(s) referred to

BS 1017, Sampling of coal and coke.

BS 1017-2, Methods for sampling of coke.

ISO 687, Coke Determination of moisture in the analysis sample1)

.

1) Referred to in the foreword only.


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BS 1016-104.2:1991

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