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है”ह”ह

IS 9127-3 (2002): Methods for the Petrographic Analysis ofBituminous Coal and Anthracite, Part 3: Method ofDetermining Maceral Group Composition [PCD 7: Solid MineralFuels]

IS 9127( Part 3 ): 20021s0 7404-3:1994

(wi’ly7-w7JT)

Indian Standard

METHODS FOR THE PETROGRAPHIC ANALYSISOF BITUMINOUS COAL AND ANTHRACITE

PART 3 METHOD OF DETERMINING MACERAL GROUP COMPOSITION

( First Revision)

Ics 74.040

G BIS 2002

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

December 2002 Price Group 3

Solid Mineral Fuels Sectional Committee, PCD 7

NATIONAL FOREWORD

This Indian Standard ( Part 3 ) ( First Revision ) which is identical with ISO 7404.3:1994 ‘Methods forthe petrographic analysis of bituminous coal and anthracite — Part 3: Method of determining maceralgroup composition’ issued by the International Organization for Standardization ( ISO ) was adopted bythe Bureau of Indian Standards on the recommendation of Solid Mineral Fuels Sectional Committee andapproval of the Petroleum, Coal and Related Products Division Council.

This standard was published in 1979 which was largely based on lSO/DIS 7404-3. iSO/DIS 7404-3 hassubsequently been published in 1984 and revised in 1994 which is now available as ISO 7404-3:1994‘Methods for the petrographic analysis of bituminous coal and anthracite — Part 3: Method of determiningmaceral group composition’. The Committee, therefore, decided to revise this standard to completelyalign it with ISO 7404-3:1994 and publish as a dual number standard. Consequently, the title has beenmodified as ‘Methods for the petrographic analysis of bituminous coal and anthracite: Part 3 Method ofdetermining maceral group composition’.

The text of ISO Standard has b,een approved as suitable for publication as Indian Standard withoutdeviations. Certain conventions are, however, not identical to those used in Indian Standards. Attentionis particularly drawn to the following:

a) Wherever the words ‘International Standard’ appear referring to this standard, they should beread as ‘Indian Standard’,

b) Comma ( , ) has been used as a decimal marker while in Indian Standards, the current practiceis to use a point ( , ) as the decimal marker,

In this adopted standard, reference appears to certain International Standards for which Indian Standardsalso exist. The corresponding Indian Standards which are to be substituted in their place are listedbelow along with their degree of equivalence for the editions indicated. However, that InternationalStandard cross-referred in this adopted ISO standard, which has subsequently been revised, positionin respect of latest ISO standard has been given:

International Standard

ISO 7404-1:1994 Methods for thepetrographic analysis of bituminouscoal and anthracite — Part 1 :Vocabulary

ISO 7404-2:1985 Methods for thepetrographic analysis of bituminouscoal and anthracite — Part 2: Methodof preparing coal samples

ISO 7404-4:1988 Methods for thepetrographic analysis of bituminouscoal and anthracite — Part 4: Methodof determining microiithotype,carbominerite and mineritecomposition

Corresponding Indian Standard Degree of Equivalence

IS9127 ( Part 1 ) :1992 Methods for Technically equivalentthe petrographic analysis of coal: with minor deviationsPart 1 Definition of terms relating topetrographic analysis of coal ( firstrevision )

IS9127 ( Part 2 ) :2002 Methods forthe petrographic analysis ofbituminous coal and anthracite :Part 2 Method of preparing coalsamples ( first revision )

IS 9127 ( Part 4 ) :2001 Methodsfor the petrographic analysis ofbituminous coal and anthracite:Part 4 Method of determiningmicrolithotype, carbominerite andminerite composition

Identical

do

( Continued on third cover)

IS 9127 (Part 3) :20021s0 7404-3:1994

—

Indian Standard

METHODS FOR THE PETROGRAPHIC ANALYSISOF BITUMINOUS COAL AND ANTHRACITE

PART 3 METHOD OF DETERMINING MACERAL GROUP COMPOSITION

( First Revision)

1 Scope

This part of ISO 7404 specifies a method of deter-mining the proportions of the maceral groups (and theminerals if desired) in coals. It is concerned only withdeterminations made on polished particulate blocksusing reflected white light. If needed, the proportionsof the individual macerals may be determined by thesame procedure. It is not concerned with the deter-mination of the proportions of naturally occurringmaceral associations (i.e. microlithotypes, see1s07404-4).

2 Normative references

The following standards contain provisions which,through reference in this text, constitute provisionsof this part of ISO 7404. At the time of publication, theeditions indicated were valid. All standards are subjectto revision, and parties to agreements based on thispart of ISO 7404 are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated below. Members of IEC and ISO

maintain registers of currently valid InternationalStandards.

ISO 7404-1:1994, Methods for the petrographicanalysis of bituminous coal and anthracite — Part 1:Vocabulary.

ISO 7404-2:1985, Methods for the petrographicanalysis of bituminous coal and anthracite — Part 2.’Method of preparing coal samples.

ISO 7404-4:1988, Methods for the petrographicanalysis of bituminous coal and anthracite — Part 4:Method of determining microlithotype, carbomineriteand minerite composition.

ISO 7404-5:1994, Methods for the petrographicanalysis of bituminous coal and anthracite — Part 5:Method of determining microscopically thereflectance of vitrinite.

3 Definitions

For the purposes of this part of ISO 7404, the defi-nitions given in ISO 7404-1 apply.

1

—

IS 9127 [Part 3) :20021s0 7404-3:1994

—4 Principle

A representative sample of coal is used to prepare aparticulate block as described in ISO 7404-2. This isexamined using a reflected light microscope and themaceral groups are identified under an immersionmedium by their relative reflectance, colour, size andmorphology. Their propotiions are determined by apoint count procedure.

5 Material

Immersion medium, having a suitable refractiveindex and compatible with the microscope objective.

NOTE 1 It is recommended that an oil with a refractiveindex of 1,5180 as specified in ISO 7404-5 be used, es-pecially if the reflectance of the macerals is to be measured.

6 Apparatus

6.1 Reflected light microscope, having an immer-sion objective of magnification between x 25 andx 60 and an eyepiece of magnification between x 8and x 12. The eyepiece incorporates a fine crosslinegraticule.

6.2 Mechanical stage, capable of advancing thespecimen laterally by equal steps of such length thatonly a negligibly small propotiion of the particlesexamined receives more than one count on the sameparticle. The step length is equal to half the maximumparticle diameter, i.e. 0,5 mm to 0,6 mm for sampleswith a standard top particle size of 1 mm. The stagealso permits a similar stepped advance in the per-pendicular direction. The lateral movement is actuatedpreferably by the counter mechanism, whereas theperpendicular movement may be satisfactorily per-formed manually.

6.3 Counter, capable of registering the counts ineach catego~ and preferably the grand total ofpetrographic components.

6.4 Sample mounting equipment, comprisingslides, modelling clay and Ievelling device.

7 Preparation of coal sample

Prepare and polish a particulate block as described inISO 7404-2.

8 Procedure

Adjust the microscope (6.1 ) for Kohler illumination.Set up the Ievelled particulate block on the stage,place the immersion medium (clause 5) on the sur-face of the block, focus and observe the image in themicroscope. Identify the material lying under theintersection of the crosslines and carry out the pointcount procedure as follows.

Crosslines on

Vitrinite (V), Iiptinite(L) or inertinite (1)

Mounting medium

Minerals (M)

Boundary betweenmacerals or betweenmaceral and mount-ing medium

Empty pore in amaceral or a void

Action

Operate the counter for appro-priate maceral group.

Ignore the point.

Operate the counter for pyrite,shale, etc. or ignore the point(see the last three paragraphsof the introduction andclause 1O).

Examine in turn the material ly-ing immediately adjacent tocrossline intersection in the topright, bottom right, bottom leftand top left quadrants, Take thefirst of these which does nothave a boundary in it, and oper-ate the counter for this material(see figure 1),

Ignore the point

Advance the block by one step in the left-to-right di-rection, and continue counting and traversing thespecimen. At the end of a traverse, advance the blockby a step of at least equal length in the perpendiculardirection to start the next parallel traverse. Choose thestep length to ensure a uniform counting of pointsover the surface of the block.

Count a total of at least 500 points.

2

IS 9127 (Part 3) :20021s0 7404-3:1994

Vitrinite

d Normal C~SS- count point A fvitrinite)

Vitrinite

Inertinite

b] Boundarycase - count point B [inertinitei

Iff!!ae-”trinkeLiptinite

ci Boundaryseso - count point C (iiptinitsi

inertinite

Mounting medium

Vitrinite

d Boundarycaso- tit. point is not sountsd

NOTE — Width of crosslines exaggerated for clarity.

Figure 1 — Normai and boundary cases between macerals or between maceral and mounting medium

3

IS 9127 (Part 3) :20021s0 7404-3:1994

—..

9 Expression of results

Calculate the volume percentage of each component[vitrinite (V), Iiptinite (L)t inertinite (l)], which is equalto the percentage number of points counted on it,expressing the results to the nearest integer. Theform of the results depends on the procedure adoptedwith regard to minerals (see the last three paragraphsof the introduction) and is expressed on one of thefollowing bases:

a) minerals ignored:%V+%L+%I=1OO

b) minerals (M) counted:O\oV+ YoL+Yol+Yo M=l OO

c) minerals matter (MM) calculated:%V+%L+%I+%MM=1OO

In alternative c), minerals are ignored in the pointcount but the volume percentage of mineral matter iscalculated from the determined ash by means of anaccepted empirical relationship.

The procedure adopted and the number of pointscounted shall be indicated in the test report.

NOTE 2 Examples of equations to calculate the mineralmatter, Y. MM, as a volume percentage, are as follows:

% MM = 0,61wA– 0,21 . . (1)

0/0MM =w~

2,07 – 0,01lw~. . . (2)

where

WA

w~

is the ash content, as a mass percentage onthe airdried basis;

is the mineral matter content, as a mass per-centage, given by the equation

W~ = 1,08wA + 0,55w~

where w~ is the sulfur content, as a mass per-centage on the air-dried basis.

Equation (2) is based on assumed relative densitiesof 1,35 and 2,8 for the macerals and mineral matterrespectively.

These equations have been found satisfactory in cer-tain coal basins but may not necessarily apply globally.It is essential for the user to establish suitableequations for the coals being analysed.

10 Precision

10.1 Repeatability limit

The repeatability limit of the determination of the vol-ume percentage of a component is the value of thedifference between two single determinations, eachbased on the same number ;f points counted, carriedout by the same operator on the same block using thesame apparatus, below which 95 ‘Yo of such differ-ences are expected to lie. The repeatability limit maybe calculated from the formula

,-

(4)22r7t

where crt is the theoretical standard deviation.

Provided that the operator makes negligible errors inclassifying the macerals, the results of an analysis aresubject to standard deviations calculable on the basisof the binominal distribution.

Where p YOof the total number of points counted, N,is registered for a given maceral group, the theoreticalstandard deviation, at, of p is given by the equation

(q = 4p(loo–p)

N

Values based on counts of 500 points for the theor-etical standard deviation, coefficient of variation andrepeatability calculated for a range of volume per-centages of a component are given in table 1.

Table 1 — Theoretical standard deviation andrepeatability limit of the percentage of a

component, based on counts of 500 points

Volume ‘Y.,

P

5

20

50

80

95

Standarddeviation,

1,0

1,8

2,2

1,8

1,0

Coefficientof variation,

1oolJ,/p

20

9

4,4

2,3

1,1

Repeatabilitylimit,

_wk-2,8

5,1

6,3

5,1

2,8

NOTE 3 For example, if the volume percentage ofvitrinite in a sample is 80 Y., then an operator can expect toobtain two results differing by less than 5,1 percentagepoints (e.g. 78 % and 83 %) in 19 cases out of 20.

4

IS 9127 (Part3) :20021s0 7404-3:1994

—

10.2 Reproducibility limit

The reproducibility limit of the determination of thevolume percentage of a component is that value ofthe difference between two single determinations,each based on the same number of points counted,carried out by two different operators on two differentsubsamples taken from the same sample, using dif-ferent equipment, below which 95 Y. of such differ-ences are expected to lie. The reproducibility limit isgiven by the formula

I -\

[4)2200

where aO is the observed standard deviation,

Values of the observed standard deviation normallyexceed the values for the theoretical standard devi-ation given in table 1 owing to the misidentification ofthe macerals by different operators and to variationbetween subsamples; they have been found to varyfrom approximately 1,5 to 2,0 times the theoreticalvalues, depending on the rank and the heterogeneityof the coal.

11 Test report

The test report shall include the following information:

a)

b)

c)

d)

e)

f)

9)

h)

a reference to this part of ISO 7404;

all details necessary for identification of the sam-ple;

the name and address of the testing laboratory;

date of test;

the number of points counted;

whether minerals were counted or ignored, orwhether the mineral matter was calculated, and

(if calculated) the equation used;

the results obtained;

any other characteristics of the sample observedduring the analysis that may be relevant to theuse of the results.

NOTE 4 It may also be useful to include nominal magni-fication, point count stage step size and line traverse spac-ing.

5

IS 9127 (Part 3) :20021s0 7404-3:1994

_.. —

Annex A(informative)

Bibliography

[1] International Handbook of Coal Petrography, supplement (1975) and third supplement (1993) may be

published by the International Committee for obtained from Professor D.G. Murchison, Fossil Fuels and

Coal and Organic Petrology (lCCP). Environmental Geochemistry, Drummond Building, Univer-sity of Newcastle, Newcastle-upon-Ty ne, NE1 7RU, United

NOTE 5 The second edition (1963), together with the first Kingdom.

supplement (1971, corrected and revised in 1985), second

6

( Continued from second cover)

—International Standard Corresponding Indian Standard Degree of Equivalence

ISO 7404-5:1994 Methods for the IS 9127 ( Part 5 ) :1986 Methods Technically notpetrographic analysis of bituminous for the petrographic analysis equivalent. However,coal and anthracite — Part 5: Method of coal : Part 5 Microscopical IS 9127 ( Part 5 ) isof determining microscopically the determination of the reflectance of being considered forreflectance of vitrinite vitrinite revision to align it with

1s0 7404-5:1994

In reporting the results of a test or analysis made in accordance with this standard, if the final value,observed or calculated, is to be rounded off, it shall be done in accordance with IS 2:1960 ‘Rules forrounding off numerical values ( revised)’.

c153

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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken Up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issueof ‘BIS Catalogue’ and ‘Standards : Monthly Additions’.

This Indian Standard has been developed from Doc : No. PCD 7 ( 1841 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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