Tiêu Chuẩn Iso 09197-2016.Pdf

© ISO 2016 Paper, board and pulps — Determination of water soluble chlorides Papier, carton et pâtes — Détermination des chlorures solubles dans l’eau INTERNATIONAL STANDARD ISO 9197 Third edition 201[.]

P aper, board and pulps —

Pa i er, c arto et p te — Déte mi nati on des chl orur s s ol ubl es

dans l ’ea

T ir d edition

2 16-0 -1

Reference n mb r

ISO 9 97:2 16(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2016, P blshed in Sw itz rlan

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F reword i v

1 Sc ope 1

2 Nor mati ve r eferenc es 1

3 Terms an definitions 1

4 Principle 1

5 Re g ents 1

6 A pparatus 2

7 S mpl n and preparatio of sample 2

8 Proc ed re .2

9 Ex pres io of r esults 3

10 Test rep r t 3

A nne x A (informative)Precisio 5

A nne x B (informative)Laborator y manuals 6

Biblog raphy 7

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 the fol owing URL: F or word - Sup lementary information

The committ ee r sp nsible for thisdocument is ISO/TC6, Pa e , b ard a d p lps

This third edition canc ls an r plac s the se on edition (ISO 9 97 :2 0 ), of w hich it cons itut es a

minor r vision The chang es compar d t o the pr vious edition ar as folows:

— thet ext in 5.4 on the pr p ration of nitric acid has be n cor e t ed;

— thepr cision s at ement has be n mo ed t o Annex A

P aper, board and pulps — Determination ofwater-soluble

This Int ernational Stan ard spe ifies a method for the det ermination of wat er-soluble chlorides in

al ty es of pa e , b ard and pulp The lowe lmit ofthe det ermination is 2 mg of chloride ion pe

ki o ram ofdry sample

2 Normati ve r eferences

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

in ispensa le for it a pl cation F or dat ed r fe enc s, only the edition cit ed a pl es F or u dat ed

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

ISO 1 6, Pa e a d b ard — S mpln to dete mine a e a e q alt y

ISO 2 7, Pa e a d b ard — Determin tio o moi s tur c ontent o a lot — Oven-dr y in meth d

ISO 63 , Pa e ,b ard a d p lps — Dete min tio o dry matte c ontent — Oven-dryin meth d

ISO 7 1 , Pulps — S mpln fr tes tin

3 Terms and definitions

F or the purposes of this document, the folowing t ermsand definitions a ply

3.1

water soluble chlorides

amou t of chloride ion that is extract ed with cold wat er an det ermined u de the con itions spe ified

4 Principle

Pie es ofthe sample un e t es ar extract ed with wat er at ro m t empe atur in a disint egrat or The

r sulting suspension is f ilt er d an an alq ot is used for det ermination of the chloride ion cont ent b

ion chromat ogra hy

During the analy sis, use only r ag ent of r co niz d analytical q alty an only wat er as spe ified in 5.1

5.1 Distiled or demineral zed water, con uctivity les than 0,2 mS/m

5.2 C loride stock solutio , c (Cl) = 1 0 0 mg /l Dry a p rtion of p tas ium chloride, (KCI), at 140 °C

Trans e 2 0,2 mg ther eof to a 1 0 ml v lumetric flask, dis olve the KCI and di ute to the mar k with

wate (5.1) C mmer cialy a vaia le s andar d solutions ma y be used

5.3 C loride matching solution Diute the chloride s ock solution (5.2) to a mas fr action of

chloride ion of, for ex ample, c (Cl) = 1 mg l Do not use chloride matching solutions that ar e mor e than

oneweek old

5.4 Nitric acid, c(HNO

3 ) = 1,3 mol/l Add with caution 8 ml of conc ntr ated nitric acid,

c(HNO

3

)= 1 ,8 mol/l (a out 7 % HNO

3 ), to 5 0ml of wate (5.1) an diute to 1 l

5.5 Additional solutions, asspe ified in the ins ructions for the ion chr omatog raph

6 A pparatus

Glas war an othe a p ratus used for this analy sis shal be sc upulously clean So k al glas war

for 5 min t o 1 min in the nitric acid (5.4) an then rinse thoroughly with wat er (5.1) Clean, in wat er,

for eps, scis ors and the disint egrat or used for sample pr p ration

6.1 Wet disinteg rator, a high-spe d mixe , ca a le of disinteg r ating the sample completely w ith

minimum damag e to the fibres

6.2 Ion chromatog rap , ha ving a pump, an inje tor lo p of k own v lume, a column sys em suitable

for the dete mination of chlorides an a con uctivity dete tor

6.3 Syr ing e, Clas A , of ca acity 5 ml an ha ving a pr efite of a out 0,2 µm p r e w idth

6.4 Te -strainer or simia devic e, of s ainles s e l, for r emoving fibres fr om a suspension

7 Sampl ng and pr eparation of sample

If the t es is being made t o ev luat e a pulp lot, the sample shal be sele t ed in ac ordanc with ISO 7 1

If the t es is made on anothe ty e of sample, r port the sour e of the sample an , if p s ible, the

samplng proc d r used From the sample r c ived, sele t spe imens so that they ar r pr sentative

of the w hole sample

The proc d r t o be folowed w hen samplng depen s on the particular cir ums anc s in each case

F or sampl ng from lot of pulp, p pe or b ard, the ins ructions in ISO 7 1 or ISO 1 6, as r lev nt, ar

r commen ed

Sinc the amou t of chlorides in the sample can be ve y low, take car not t o contaminat e it d ring

samplng Wear clean prot ective glo es at al times w hen han lng the sample an the t es pie es

pr p r d from it

The la orat ory w he e the analy sis is made shal be fr efrom d s an fumes from chlorine-containing

subs anc s, such as hydrochloric acid or chlorinat ed solvent Particular car should be taken in mi

l-sit e la orat ories if the mi l uses chlorine or chlorine dio ide as a bleaching ag ent

K eep spe imens prot ect ed, wra ped in aluminium foi or in plas ic b gs, u ti r q ir d for analy sis

Analy se spe imens as so n as p s ible aft er samplng

Det ermine the dry matt er cont ent on a sep rat e spe imen using the proc d r spe if ied in ISO 2 7 (for

p pe an b ard) or in ISO 6 8 (for pulps)

8 Proc edure

Car y out the proc d r in d pl cat e A blank t es shal also be car ied out in paral el with the entir

det ermination

Weigh, t o the near s 0,0 g, a t es pie e, g ene aly of between 2 g an 5 g Splt thick b ard an pulp

she t int o thin e pie es t o faci tat e so king

S le t the siz of the t es pie e so that the mas fraction of chloride ion of the extract is within the

o timum rang e of the ion chromat ogra h

Trans e the weighed t es pie e t o the disint egrat or (6.1) an ad 2 0 ml ± 2 ml of wat er (5.1) at

2 °C± 2 °C

Disint egrat e the t es pie e u ti it is complet ely disint egrat ed, but no long er

Aft er disint egration, so k the t es pie e for a out 1 h w hie s ir ing g ently t o ensur complet e extraction

of chloride Immediat ely aft er st op ing the g entle s ir ing, with raw a p rtion of the suspension, using

the syring e (6.3) If this o e ation is hampe ed b the pr senc of f ibr s or f ibr bun les, use the t ea

s raine or simi ar devic (6.4) t o r mo e f ibrous mat erial It is es ential that the t es pie e solution be

fr e from suspended mat erial

Sinc the o e ation of the ion chromat ogra h (6.2) depen s on it design, no detai ed ins ructionsma

be given he e Ope at e the a p ratus asins ruct ed b the man factur r ( e also An ex A)

F or cal bration, pr p r from the chloride mat ching solution (5.3) a se ies of f ive cal bration solutions,

co e ing a out one de ade of conc ntrations, for ex mple, from 1 mg l t o 1 mg l

R un the calbration solutions an the t es pie e solution on the chromat ogra h as ins ruct ed b the

man factur r of the a p ratus

Plot the r adings for the calbration solutions a ains their chloride ion conc ntrations The f ive p int

for the calbration solutions should fal on a s raight l ne If they fai t o do so, r peat he cal bration with

anothe set of calbration solutions, co e ing a highe or lowe conc ntration rang e, as r lev nt

Che k the cal bration seve al times daiy an w heneve a new set of calbration solutions isused

9 Ex pres ion of r esults

R ead the chloride ion conc ntration of the sample solution from the calbration gra h Calculat e the

mas fraction of chloride ion in the sample from F ormula (1):

w

V

mX Cl

Cl Cl

=

−

1 0

0

,

(1)

w he e

w

Cl

is the mas fraction of chloride ion, in mi lgrams pe kio ram, in the sample;

ρ

Cl

is the chloride ion conc ntration, in mi lgrams pe l tr , of the filt er d sample solution;

ρ

Cl,0

is the chloride ion conc ntration, in mi lgrams pe l tr , of the blan solution;

V is the volume of wat er (5.1) used: the v lume spe if ied is 2 0 ml;

m is the mas , in grams, of sample taken;

X is the mas fraction of dry matt er, ex r s ed as a pe c ntag e, in the sample

Calculat e the mean of the d pl cat es an r p rt r sult below 2 mg kg as “les than 2 mg kg an

r sult of 2 mg kg or mor t o the near s 1 mg kg

10 Test r eport

The r p rt shal inclu e the folowing information:

a) a r fe enc t o this Int ernational Stan ard, ISO 9 97 :2 1 ;

b) thedat e and plac of t es ing;

c) thecomplet e identification of the sample t est ed;

d) ther sult, ex r s ed as in icat ed in Cla use 9;

e) any dep rtur from the proc d r desc ibed in this Int ernational Stan ard or any othe

cir ums anc s w hich can ha e afe t ed the r sult

A nne x A

Precision

A 1 General

The fol owing r sult we e o tained in an int erla orat ory trial con uct ed b the S an ina ian P lp,

Pa e an Bo rd Tes ing C mmitt ee

The r peata i ty an r prod cibi ity lmit r port ed ar es imat es of the ma imum dife enc w hich

should be ex e t ed in 1 of 2 ins anc s, w hen comp ring two t es r sult for mat erial simi ar t o those

desc ibed u de simiar t es con itions These es imat es ma not be v ld for dife ent mat erials or

dife ent t es con itions

NOTE R epe ta ility an reprod cibility limits are calculat ed by multiplying the repe ta ility an

reprod cibility stan ard deviations by 2,7 , where 2,7 = 1,96 √2

A 2 Repeatabi ity

Data not a aia le

A 3 Reproducibi ity

Nine la orat ories analy sed four samples as spe if ied in this Int ernational Standard Each sample was

analy sed in d plcat e The mean mas fraction of chloride ion an the s an ard deviation (between

la orat ories) we e calculat ed ac ording t o ISO/TR 24 9 The r sult ar given in Ta le A.1

Table A.1

Sample

Mean mas

fraction

of chloride ion

R eprod cibi ty

s an ard deviation

C eficient of

v riation

R eprod cibi ity

lmit

mg kg

mg kg

s

R

Co V,R

%

R

mg kg

Machine-glazed (MG)

paper from ble ched

kraf p lp

(14,6) a

a

The value is u der the lower lmit of determination

A nne x B

The proc d r spe if ied in this Int ernational Stan ard r les up n ins rument of conside a le

complexity S ve al man factur rs ha e introd c d such ins rument t o the world market They ar al

b sed on the same principle, but dife in detais

It is a principle of s an ardization not t o spe ify the use of eq ipment prod c d b a p rticular

man factur r The r ason for this is not only that a s an ardization b dy should be neutral with r spe t

t o the competition betwe n comp nies, but also t o a oid spe if ications that wi l un e es ariy pr vent

furthe develo ment of eq ipment

In practic , this means that the course of the analy sis cannot be desc ibed in this International Stan ard

in such detai that it can be used as a la orat ory bench man al F or the pe formanc of the analy sis, a

n mbe ofinformational detai s ha e to be taken from the man factur r’s man al or to be es a lshed

localy in pr lminary tes s Ex mples ar set ings of lq id flow, t empe atur s, p we an waiting times

Bibl og raphy

[1] ISO/TR 2449 , Pa e ,b ard a d p lps — Es timatio o u c ertaint y fr tes t meth ds

ICS  85.060; 85.040

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