Tiêu chuẩn iso 13909 3 2016

© ISO 2016 Hard coal and coke — Mechanical sampling — Part 3 Coal — Sampling from stationary lots Houille et coke — Échantillonnage mécanique — Partie 3 Charbon — Échantillonnage sur lots statiques IN[.]

Hard c oal and c oke — Mechanical

Part 3:

Ho ille et coke — Éch ntillo n ge méca ique —

Partie 3: Ch rb n — Éch ntillo n ge sur lot statiques

S con edition

2 16-07-0

Refer ence n mb r

ISO 1 9 9-3:2 16(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2016, P blshed in Sw itz rlan

A ll rig hts r eserved Unles otherw ise spe ified, nopar of this p blc tion ma y be r epr od c d or utilz d otherw ise in an form

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written permis ion Permis ion c n be req esed from either ISO at the ad r es below or ISO’s member bod y in the c u try of

F reword i v

1 Sc ope 1

2 Nor mati ve r eferenc es 1

3 Terms an definitions 1

4 Establshing a sampl ng s heme 1

4.1 General 1

4.2 Desig n of the samplng scheme 2

4.2.1 Mate ial to be sampled 2

4.2.2 Division of lots 2

4.2.3 Pr ecision of sampl ng 2

4.2.4 Bias of samplng 3

4.3 Pr ecision of r esult 3

4.3.1 Pr ecision an total v rianc 3

4.3.2 Primary incr ement v rianc 4

4.3.3 Pr ep ration an testing v rianc 4

4.3.4 Numbe of sub-lots an n mbe of increment pe sub-lot 4

4.4 Minimum mas of sample 6

4.5 Mas of primary increment 8

4.6 Siz analysis 9

5 Metho s of samplng fr om wag ons, bar g es and ships 10

5.1 General 1

5.2 Numbe of increment and sub-lot 1

5.2.1 General analysis an moistur e samples 1

5.2.2 C mmon sample 1

5.3 Taking the incr ements 1

5.4 Dis ribution of incr ement 1

5.4.1 Wag ons 1

5.4.2 Bar g es 1

5.4.3 Ships 1

5.4.4 Ran om sele tion of incr ement 1

6 Metho s of samplng fr om stockpies 12

7 S mpl n eq ipment — mechanical aug er 13

8 Handlng and storag e of samples 15

9 S mple preparatio 16

10 Minimization of bias 16

1 1 Causes of bias 1

1 2 Che king for precision and bias 1

11 Ver ification 17

Biblog raphy .18

ISO (he Int ernational Org nization for Stan ardization) is a worldwidefede ation of national s an ards

b dies (ISO membe b dies) The work of pr p ring Int ernational Stan ards is normaly car ied out

through ISO t ech ical committ ees Each membe b dy int er st ed in a subje t for w hich a t ech ical

committ ee has be n es a lshed has the right t o be r pr sent ed on that committ ee Int ernational

org nizations, g ove nmental an non-g ove nmental, in laison with ISO, also take part in the work

ISO cola orat es closely with the Int ernational Ele trot ech ical C mmis ion (IEC) on al matt ers of

ele trot ech ical s an ardization

The proc d r s used t o develo this document an those int en ed for it furthe maint enanc ar

desc ibed in the ISO/IEC Dir ctives, Part 1 In p rticular the dife ent a pro al c it eria ne ded for the

dife ent ty es of ISO document should be not ed This document was draft ed in ac ordanc with the

edit orial rules of the ISO/IEC Dir ctives, Part 2 ( e www.iso.org dir ctives)

A tt ention is drawn t o the p s ibi ity that some of the element of this document ma be the subje t of

p t ent right ISO shal not be held r sponsible for identifying any or al such p t ent right Detais of

any p t ent right identified d ring the develo ment of the document wi be in the Introd ction an / r

on the ISO ls of p t ent de larations r c ived ( e www.iso.org p t ent )

Any trade name used in this document is information given for the convenienc of use s an does not

cons itut e an en orsement

F or an ex lanation on the meaning of ISO spe ific t erms an ex r s ions r lat ed t o conformity

as es ment, as wel as information a out ISO’s adhe enc t o the WTO principles in the Te h ical

Bar ie s t o Trade (TBT), se thefolowing URL:F or word - Sup lementary information

The committ ee r sponsible for this document is ISO/TC 2 , S ld mine al f els , Subcommitt ee SC 4,

S mpln

This se on edition canc ls an r plac s the firs edition (ISO 1 9 9-3:2 0 ), w hich has be n

t ech icaly r vised

ISO 1 9 9 consis s of the fol owing p rt , un e the g ene al title Hard c oal a d c oke — Mecha ic al

s ampln :

— Part 1: G ene al introduc tio

— Part 2 : Co l — S mpln from mov in s tr ams

— Part 3 : Co l — S mpln froms tatio ary lots

— Part 4 : Co l — Prep ration o tes t s amples

— Part 5: Coke — S mpln from mov in s tr ams

— Part 6 : Coke — Prep ration o tes t s amples

— Part 7: Meth ds fr determinin the pr c i s ion o s ampln , s ample pr p ratio a d tes tin

— Part 8: Meth ds o tes tin fr bias

Hard c oal and c oke — Mechanical sampling —

Part 3:

This part of ISO 1 9 9 spe if ies proc d r s for the me hanical sampl ng of co l from s ationary lot ,

for ex mple, from wag ons, barg es, ships an st ockpies These proc d r s ar t o be used w hen it is

not p s ible t o sample the lot d ring lo ding or discharg e ac ording t o ISO 1 9 9- 2 Proc d r s for

sample pr p ration ar given in ISO 1 9 9-4

This p rt of ISO 1 9 9 isa plca le t o me hanical sampl ng from s ationary co l lot , t o o tain samples

from w hich t es samples for the det ermination of mois ur , an for g ene al analy sis inclu ing physical

an chemical t es s, can be pr p r d in ac ordanc with the r q ir ment an r commendations set out

in ISO 1 9 9-4

In this part of ISO 1 9 9, the principles an proc d r s for designing a sampl ng scheme ar given,

t og ethe with ty ical ex mples of a plcations; in ad ition, practic s for the ex ecution of samplng in

dife ent sampl ng situations ar desc ibed The methods desc ibed ar lmit ed t o those on w hich it is

p s iblet o con uct a t es for bias

2 Normati ve r eferences

The folowing r fe enc d document , in w hole or in p rt, ar normatively r fe enc d in this document

an ar indispensa le for it a plcation F r dat ed r fe enc s, only the edition cit ed a pl es F r

un at ed r fe enc s, the lat es edition of the r fe enc d document ( inclu ing any amen ment ) a ples

ISO 1 9 9-1, Hard c oal a d c oke — Mecha ic al s ampln — Part 1: G ene al introduc tio

ISO 1 9 9- 2, Hard c oal a d c oke — Me h nic al s ampln — Part 2 : Co l — S mpln from movin s tr ams

ISO 1 9 9-4, Hard c oal a d c oke — Me h nic al s ampln — Part 4 : Co l — Prep ratio o tes t s amples

ISO 1 9 9-7, Hard c oal a d c oke — Mecha ic al s ampln — Part 7: Meth ds fr dete minin the pr c i s io

o s ampln ,s ample pr p ratio a d tes tin

ISO 1 9 9-8, Hard c oal a d c oke — Mecha ic al s ampln — Part 8: Meth ds o tes tin fr bias

3 Terms and definitions

F or the purposes of this document, the t erms an def initions given in ISO 1 9 9-1a ply

4 Establ shing a sampl ng scheme

The g ene al proc d r for es a l shing a samplng scheme is as fol ow s

a) Define the q alty p ramet ers t o be det ermined an the ty es of samples r q ir d

b) Define the lot

c) Def ine or as umethe pr cision r q ir d ( e 4.3.1).

d) Det ermine the method of combining the inc ement int o samples an the method of sample

pr paration ( e ISO 1 9 9-4 )

e) Det ermine or as ume the v ria i ity of the co l ( e 4.3.2) an the v rianc of pr p ration an

t es ing ( e 4.3.3) Methods for det ermining v ria i ity an v rianc of pr p ration an t es ing ar

given in ISO 1 90 -7

f) Es a lsh the n mbe of sub-lot an the n mbe of inc ement pe sub-lot r q ir d t o at ain the

desir d pr cision ( e 4.3.4)

g) De ide upon the sampl ng int erv l, in t onnes

h) Asc rtain the nominal t op siz of co l for the purpose of det ermining the minimum mas of sample

( e 4.4 an Ta le 1)

The nominal t op siz ma initial y be asc rtained b consulting the consignment detai s, or b

visual es imation, and ma be ve if ied, if ne es ary, b pr lminary t es work

i) Det erminethe minimum a e ag e inc ement mas ( e 4.5)

4.2 Desig n of the sampl ng s heme

4.2.1 Mater ial to be sampled

The firs s ag e in the design of the scheme is t o identify the co l t o be sampled Samples ma be

r q ir d for t echnical ev luation, proc s control, q al ty control and for comme cial r asons b b th

the prod c r an the cust ome It is es ential t o asc rtain ex ctly at w hat s ag e in the co l-han lng

proc s the sample is r q ir d an , as far as practica le, t o design the scheme ac ordingly In some

ins anc s, howeve , it ma pro e impractica le t o o tain samples at the pr fe r d point an , in such

cases, a mor practica le alt ernative is r q ir d

4.2.2 Di visio of lots

A lot ma be sampled as a w hole or as a se ies of sub-lot , e.g co l desp t ched or delve ed o e a pe iod

of time, a ship lo d, a train lo d, a wag on lo d or co l prod c d in a c rtain pe iod (e.g a shif)

It ma be ne es ary t o divide a lot int o a n mbe of sub-lot in orde t o impro e the pr cision ofthe

r sult

F or lot sampled o e long pe iods, it ma be ex edient t o divide the lot int o a se ies of sub-lot ,

o taining a sample for each

4.2.3 Precisio of samplng

Aft er the desir d sample pr cision has be n sele t ed, the n mbe of sub-lot an the minimum n mbe

of inc ement pe sub-lot cole t ed shal be det ermined as desc ibed in 4.3.4, and the a e ag e mas of

the primary inc ement shal be det ermined as desc ibed in 4.5

F or single lot , the q alty v riation shal be as umed as the wors case ( e 4.3.2 an 4.3.3) The

pr cision of samplng achieved ma be measur d using the proc d r of r plcat e sampl ng ( e

ISO 1 9 9-7)

A t the s art of r gular sampl ng of u k own co ls, the wors -case q alty v riation shal be as umed,

in ac ordanc with 4.3.2, 4.3.3 an 4.3.4 When sampl ng is in o e ation, a che k ma be car ied out t o

conf irm that thedesir d pr cision has be n achieved, using the proc d r s desc ibed in ISO 1 9 9-7

If any subseq ent chang e in pr cision is r q ir d, the n mbe of sub-lot an of inc ement shal be

chang ed as det ermined in 4.3.4 an the pr cision at ained shal be r che ked The pr cision shal also

be che ked if the e is any r ason t o sup ose that the v ria i ty of the co l being sampled has inc eased

The n mbe of inc ement det ermined in 4.3.4 a ples t o the pr cision of the r sult w hen thesamplng

e rors ar larg e r lative t o thet es ing e rors, e.g for mois ur cont ent

4.2.4 Bias of samplng

It is of p rticular importanc in samplng t o ensur , as far as p s ible, that the p ramet er t o be measur d

is not alt er d b the sampl ng an sample pr p ration proc s or b subseq ent st orag e prior t o t es ing

This ma r q ir , in some cir ums anc s, a l mit on the minimum mas of primary inc ement se 4.5)

When cole ting samples for mois ur det ermination from lot o e an ext en ed pe iod, it ma be

ne es ary t o lmit he s anding time of samplesb dividing the lot int o a n mbe of sub-lot ( e 4.3.4.1)

When a co l samplng scheme is implement ed, it shal be che ked for bias in ac ordanc with the

methods given in ISO 1 9 9-8

4.3 Precision of r esults

4.3.1 Pr ecisio and total varianc e

In al methods of samplng, sample pr p ration and analy sis, e rors ar incur ed an the ex e imental

r sult o tained from such methods for any given paramet er wi l deviat e from the true v lue of that

p ramet er Whie the a solut e deviation of a single r sult rom the “ rue” v lue cannot be det ermined,

it is pos ible t o make an es imat e of the pr cision of the ex e imental r sult This is the closenes with

w hich the r sult of a se ies of measur ment made on thesame co l a r e among themselves

It is p s ible t o design a sampl ng scheme b w hich, in principle, an arbitrary level of pr cision can be

achieved

The r q ir d o e al pr cision for a lot is normaly a r ed betwe n the p rties conc rned In the

a senc of such a r ement, a v lue of one t enth of the ash cont ent ma be as umed up t o 1 % ash,

subje t t o a ma imum of 1 % a solut e for ash cont ent a o e 1 %

The theory of the es imation of pr cision is discus ed in ISO 1 9 9-7 The folowing formula is de ived:

is the es imat ed in ex of o e al pr cision of samplng, sample pr p ration an t es ing for

the lot at a 9 % conf idenc level, ex r s ed as pe c ntag e a solut e;

V

I

is the primary inc ement v rianc ;

n is the n mbe of inc ement pe sub-lot ;

m is the n mbe of sub-lot in the lot ;

V

P

is the pr p ration an t es ing v rianc

If the q alty of a co l of a ty e not pr viously sampled is r q ir d, then in orde t o devise a samplng

scheme, as umptions ha e t o be made a out the v ria i ty ( e 4.3.2) The pr cision actual y achieved

for a p rticular lot b the scheme devised can be measur d b the proc d r s given in ISO 1 9 9-7

4.3.2 Pr imar y increment var ianc e

The primary inc ement v rianc , V

Idepen s up n the ty e an nominal t op siz of co l, the degr e

of pr -tr atment an mixing, the a solut e v lue of the p ramet er t o be det ermined an the mas of

inc ement taken

The n mbe of inc ement r q ir d for the g ene al-analy sis sample an the mois ur sample shal be

calculat ed separat ely using the r lev nt v lues of inc ement v rianc an the desir d pr cision If a

common sample is r q ir d, the n mbe of inc ement r q ir d for that sample shal be the gr at er of

the n mbe s calculat ed for the g ene al analy sis sample an the mois ur sample r spe tively

NOTE For man co ls, the inc ement variance for ash is higher than that or moisture an hence, for the same

precision, the n mb r of inc ements req ired for the g neral analysis sample wil b adeq ate for the moisture

sample an for the common sample

The v lue of the primary inc ement v rianc , V

I

r q ir d for the calculation of the pr cision using

F ormula (1) can be o tained b eithe

a) dir ct determination on the co l to be sampled using one of the methods desc ibed in ISO 1 9 9-7, or

b) as uming a v luedet ermined for a simi ar co l from a simi ar co l han l ng an sampl ng sy st em

If neithe of these v lues is a ai a le, a v lueof V

I

= 5 for ash cont ent of u washed an blen ed co ls an

V

I

= 3 for the ash cont ent of washed co ls can be as umed initial y an che ked, aft er the samplng has

be n car ied out, using one of the methods desc ibed in ISO 1 9 9-7

4.3.3 Preparatio and testin var ianc e

The v lue of the pr p ration an t es ing v rianc , V

P, r q ir d for the calculation of the pr cision

using F rmula (1)can be o tained b eithe

a) dir ct determination on the co l to be sampled using one of the methods desc ibed in ISO 1 9 9-7, or

b) as uming a v luedet ermined for a simi ar co l from a simi ar sample pr p ration scheme

If neithe of these v lues is a ai a le, a v lue of 0,2 for ash cont ent can be as umed initial y an

che ked, aft er the pr p ration an t es ing has be n car ied out, using one of the methods desc ibed in

ISO 1 9 9-7

4.3.4 Number of sub-ots and numbe of incr ements per sub-ot

4.3.4.1 General

Then mbe of inc ement taken from a lot in orde t o achieve a p rticular pr cision is a function of the

v ria i ity of the q al ty of the co l in the lot, ir espe tive of the mas of the lot The lot ma be sampled

as a w hole, r sulting in one sample, or divided int o a n mbe of sub-lot r sulting in a sample from each

Such division ma bene es ary in orde t o achieve the r q ir d pr cision, an the ne es ary n mbe of

sub-lot shal be calculat ed using the proc d r given in 4.3.4.2

Anothe important r ason for dividing the lot is t o maintain the int egrity of the sample, i.e t o avoid

bias aft er taking the inc ement, p rticularly in orde t o minimiz los of mois ur d e t o s an ing The

ne d t o do thisis dependent on fact ors such as the time taken t o cole t samples, ambient t empe atur

an h midity con itions, the ease of keeping the sample in sealed containe s d ring cole tion an the

particle siz of the co l It is r commen ed that, if mois ur los is suspe t ed, a bias t es be car ied

out t o comp r the q alty of a r fe enc sample immediat ely aft er extraction with the sample aft er

s an ing for the normal time If bias isfou d, the sample s an ing time should be r d c d b cole ting

samples mor fr q ently, i.e inc easing the n mbe of sub-lot

The ema be othe practical r asonsfor dividing the lot, such as:

a) for convenienc w hen samplng o e a long pe iod;

b) t o keep sample mas es manag ea le.

The designe of a samplng scheme should cat er for the wors case anticip t ed an wi then t end t o

use a highe v lue for V

Ithan ma actual y oc ur w hen the scheme is in o e ation On implementing a

new sampl ng scheme, a che k on the actual pr cision being achieved should be car ied out using the

methods desc ibed in ISO 1 9 9-7 This ma be ne es ary t o achieve the r q ir d pr cision, in w hich

case, the n mbe of sub-lot an inc ement shal be r calculat ed using the proc d r s given in 4.3.4.2

4.3.4.2 Calculatio of numbe of sub-ots and incr ements

The n mbe of sub-lot an n mbe of inc ement r q ir d pe sub-lot is es a l shed using the

folowing proc d r

Det ermine the minimum n mbe of sub-lot r q ir d for practical r asons ( e 4.3.4.1)

Es imat e the n mbe of inc ement in each sub-lot for a desir d pr cision from the folowing formula

[o tained b transp sing F ormula (1)]:

L

2

P

(2)

A v lue of inf inity or a neg tive n mbe in icat es that the e rors of pr p ration an t es ing ar such

that the r q ir d pr cision cannot be achieved with this n mbe of sub-lot In such cases, or if n is

impractica ly larg e, inc ease the n mbe of sub-lot b one of the folowing means:

a) cho se a n mbe cor espon ing t o a convenient mas , r calculat e n from F ormula (2) an r peat

this proc s u ti the v lue of n is a practica le n mbe ;

b) de ide on the ma imum practica le n mbe of inc ement pe sub-lot, n

1, an calculat e m from

A djus m upwards, if ne es ary, t o a convenient n mbe an r calculat e n

Take n as 1 if the final calculat ed v lue is les than 1

NOTE T e formula given in 4.3.4.2 wil g neral y estimat e a higher n mb r for the req ired n mb r of

inc ements T is is b cause they are b sed on the as umption that he q ality of co l has no serial cor elation;

however, serial cor elation is always present o some de re In ad ition, b cause a certain amou t of preparation

an t esting is req ired when me suring the inc ement variance or the sub-lot variance, the preparation an

testing er or are inclu ed more than once

EXAMPLE 1 The lot is 2 0 0 t of washed co l delve ed in 5 0 0 t train lo ds an the r q ir d

a) Initial n mbe of sub-lot

It has be n de ided that he minimum n mbe of sub-lot shal be four;the efor , take four sub-lot

of 5 0 0 t each, ( i.e one sub-lot pe train lo d in this case)

b) Numbe of inc ement pe sub-lot

The efor , take four sub-lot of 40 inc ement each, ( i.e 40 inc ement from each sub-lot, w hich is

un nown;initial y as umed =5;

Pr p ration an t es ing v rianc , V

P, u k own;initial y as umed =0,2

a) Initial n mbe of sub-lot

Take a dai y sample ( i.e m = 2 in orde t o avoid risk of bias b o e night t orag e of samples)

b) Numbe of inc ement pe sub-lot

n=

×

=4

4

25

EXAMPL 3 The lot is 8 0 0 t of blen ed co l in a single lo d an the r q ir d o e al pr cision, P

L, is

0,5 % ash The q alty v riation is k own an the folowing v lues ha e be n det ermined:

primary inc ement v rianc , V

The cust ome r q ir s a r sult b sed on at leas two samples

b) Numbe of inc ement pe sub-lot

This neg tive n mbe in icat es that he e rors of pr p ration and t es ing ar such that the r q ir d

o e al pr cision cannot be achieved with this n mbe of sub-lot

It could be de ided that 5 inc ement is the ma imum practica le n mbe in a sub-lot an from

,

,

This gives a practical sampl ng method of dividing the lot int o f ive sub-lot an taking 5 inc ement

from each

4.4 Minimum mas of sample

F or mos paramet ers, p rticularly siz analy sis an those that ar particle-siz r lat ed, the pr cision

of the r sult is lmit ed b the a i ty of the sample t o r pr sent al the p rticle siz s in the mas of co l

being sampled

The minimum mas of a sample is depen ent on the nominal t opsiz of the co l, the pr cision r q ir d

for the p ramet er conc rned and the r lationship of that p ramet er t o p rticle siz Some simiar

r lationship a ples at al s ag es of pr p ration Theat ainment of this mas wi not, in it elf, guarant ee

the r q ir d pr cision, be ause pr cision is also depen ent on the n mbe of inc ement in the sample

an their v ria i ty ( e 4.3.4)

Values for the minimum mas of samples for g ene al analy sis t o r d c the v rianc d e t o the

p rticulat e natur of the co l t o 0,0 , cor esp n ing t o a pr cision of 0,2 % with r g rd t o ash, ar

given in Ta le 1, column 2 ( e CSIRO r p rt

[1]

) Ta le 1, column 3 gives the cor esp n ing minimum

mas es of divided samples for t otal mois ur analy sis, w hich ar a pro imat ely 2 % of the minimum

mas es for g ene al analy sis, subje t t o an a solut e minimum of 0,6 kg

The minimum mas of sample, m

S, for othe desir d levels of pr cision for det ermination of ash ma be

calculat ed from F ormula (4 )

is the r q ir d pr cision, with r g rd t o ash, d e t o the p rticulat e natur of the co l

When a co l is r gularly sampled un e the same cir ums anc s, the pr cision o tained for al the

r q ir d q alty paramet ers shal be che ked ( e ISO 1 9 9-7) an the mas es ma be adjust ed

ac ordingly Howeve , the mas es shal not be r d c d below the minimum r q ir ment laid down in

the r lev nt analy sis s an ards

When pr paring co l t o prod c samples for multiple use, ac ount hal also be taken of the in ivid al

mas es an siz dis ribution of the t es samples r q ir d for each t es

Table 1 — Minimum mas of sample for g neral analysis and determination of total

moisture co tent

Nominal t op siz of co l

Gene al analy sis samples an

common samples

Samples for det ermination of

t otal mois ur cont ent

NO E 1 The mas es for the general analysis an c mmon samples have be n determined to red c the varianc d e to the

par iculate nature of c al to0,01, c r espon in toa pre ision of 0,2% ash

NO E 2 Ext a tion of the total-mois ure sample f om the c mmon sample is described in ISO 1 9 9-4

4.5 Mas of pr imar y increment

The mas , m

I

in kio rams, of an inc ement aken b a me hanical aug er ( e Clause 7) from a s ationary

lot of co l can be calculat ed from F ormula (5)

d is the diamet er of the aug er tube, in metr s;

l is the depth of penetration of the aug er, in metr s;

r is the bulk density of the co l, in kio rams pe m

3