IS 13360-3-9: Plastics - Methods of Testing, Part 3: Physical and Dimensional Properties, Section 9: Determination of Moisture in Plastics by Coulometric Regeneration of Phosphorus Pentoxide

11 Pages·1999·1.2 MB·English

by  Bureau of Indian Standards

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IS 13360-3-9 (1999): Plastics - Methods of Testing, Part 3:
Physical and Dimensional Properties, Section 9:
Determination of Moisture in Plastics by Coulometric
Regeneration of Phosphorus Pentoxide [PCD 12: Plastics]
“!ान $ एक न’ भारत का +नम-ण”
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“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
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IS 13360 (Part 3/Set 9) : 1999

Indian Standard
SCITSALP - METHODS FO GNITSET
PART 3 PHYSICAL AND DIMENSIONAL PROPERTIES
Section 9 Determination of Moisture in Plastics by Coulometric Regeneration
of Phosphorus Pentoxide
ICS 83.080; 19.060

0 BIS 1999
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

June 1999 Price Group 3
Methods of tseT for scitsalP lanoitceS ,eettimmoC DCP 23
DROWEROF
sihT naidnI dradnatS was adopted yb the uaeruB of naidnI sdradnatS after the draft dezilanif yb the Methods of
tseT for scitsalP lanoitceS ,eettimmoC had neeb devorppa yb the ,muelorteP laoC dna detaleR stcudorP noisiviD
.licnuoC
erutsioM nac ylsuoires effect the ytilibassecorp of .scitsalp hgiH erutsiom tnetnoc yam esuac ecafrus snoitcefrepmi
(that ,si yalps or )gnilbbub or noitadarged yb .sisylordyh Low erutsiom htiw( hgih )erutarepmet yam esuac dilos
phase .noitaziremylop
ehT lacisyhp seitreporp of scitsalp yam eb yltaerg affected yb the erutsiom .tnetnoc
,sremyloP hcus as nolyn 6, that niatnoc gniliob-hgih slairetam hcus as srezicitsalp or hgih slevel of remonom
yam etanimatnoc the citylortcele .llec sihT lliw esuac the llec ot emoceb ,evisnopsernu gniriuqer ti ot eb denaelc
dna recoated. ehT snoitcerid for gninaelc dna gnitaocer the etylortcele llec are nevig ni xennA A for .ecnadiug
elihW gniraperp siht dradnats elbaredisnoc ecnatsissa has neeb devired morf MTSA D 40 19 : 1994 a dradnatS‘
test dohtem for erutsiom ni scitsalp yb cirtemiluoc noitareneger of surohpsohp ’edixotnep deussi yb naciremA
yteicoS for gnitseT dna slairetaM ,)MTSA( .ASU
nI gnitroper the stluser of a test or sisylana edam ecnadrocca’ni htiw siht ,dradnats fi the lanif ,eulav devresbo
or ,detaluclac si ot eb dednuor off, ti llahs eb enod ni ecnadrocca htiw SI 2 : 1960 seluR‘ for gnidnuor off
laciremun seulav .‘)desiver(
IS 13360 (Part 3/Set 9) : 1999
Indian Standard
SCITSALP - METHODS FO GNITSET
PART 3 PHYSICAL AND DIMENSIONAL PROPERTIES
Section 9 Determination of Moisture in Plastics by Coulometric Regeneration
of Phosphorus Pentoxide
4 STNEGAER
1 SCOPE
1.1 sihT standard sebircserp a tset dohtem hcihw is 4.1 ytiruP fo stnegaeR
desu rof eht noitanimreted fo erutsiom ni tsom plastics.
edarg-tnegaeR slacimehc shall eb desu ni all .stset
scitsalP gniniatnoc elitalov ,stnenopmoc hcus as
rehtO sedarg yam eb ,desu dedivorp ti is tsrif
sremonom and ,srezicitsalp yam etanimatnoc eht
deniatrecsa that eht tnegaer is fo yltneiciffus hgih
citylortcele ,llec desu ni eht ,tset gnisuac tcerrocni
ytirup ot timrep its esu tuohtiw gninessel eht ycarucca
.stluser
fo eht .noitanimreted
1.2 sihT tset dohtem is elbatius rof gnirusaem erutsiom
4.2 Purity of Water
revo eht egnar morf 0.005 tnecrep ot tsomla 100
.tnecrep Unless esiwrehto ,detacidni ecnerefer ot retaw shall
eb dootsrednu ot naem edarg 3 tnegaer ,retaw as
2 NORMATIVE REFERENCES denifed ni SI 1070.
ehT gniwollof standards niatnoc snoisivorp ,hcihw
4.3 Acetone (see SI )071
hguorht ecnerefer ni this ,txet etutitsnoc snoisivorp fo
eht standard. At eht emit fo ,iroitacilbup eht snoitide 4.4 Nitrogen, less than 5 pg/g (5 )mpp .retaw
detacidni erew .dilav llA standards era tcejbus ot
NOTE-The negortin reirrac sag llahs eb deilppus ot eht -urtsni
,noisiver and seitrap ot stnemeerga desab no this tnem hguorht ,cillatem ,nobracoroulf ro rehto -emrepmi-erutsiom
standard era degaruocne ot etagitsevni eht ytilibissop elba .gnibut esU fo rehto gnibut yam ton timrep eht tnemurtsni ot
eb ylreporp deorez esuaceb fo cirehpsomta erutsiom gnitaemrep
fo gniylppa eht tsom tnecer snoitide fo eht standards
otni eht .stnemurtsni
detacidni :woleb
4.5 Phosphoric Acid, 85 .tnecrep
IS No. Title
170 : 1984 enotecA (third revision) 4.6 Sodium Tartrate
1070 : 1992 tnegaeR edarg retaw (third revision) 4.7 Potassium Tartrate

3 APPARATUS 4.8 Sodium Tungstate
4.9 Nitric Acid
3.1 Moisture Analyzer
3.1.1 An nevo elbapac fo gnitaeh eht elpmas ot at tsael 5 TEST SPECIMEN AND SAMPLE
250°C. 5.1 selpmaS yam eb ni eht mrof fo gnidluom ,redwop
detacirbaf shapes, ro dedluom .smeti
3.1.2 A ssapyb evlav metsys rof eht noitarutas
noitneverp fo citylortcele ,llec dedeen no eno epyt fo 5.2 snemicepS yam eb tuc morf detacirbaf shapes ro
.tnemurtsni dedluom .smeti
3.1.3 An citylortcele llec rof gnippart and gnizylortcele 5.3 ecniS eht nemiceps ezis is small, 10 g ro
eht .erutsiom less ees( ,)2.4.7 erac shall eb desicrexe ot erusne that
eht nemiceps is evitatneserper fo eht .elpmas
3.1.4 scinortcelE rof gnitrevnoc eht sisylortcele tnerruc
ot latigid data. 5.4 cipocsorgyH niser samples shall eb detcetorp morf
eht .erehpsomta
3.1.5 latigiD yalpsid rof gnitneserp eht latigid data as
smargorcim fo .retaw 6 NOITARBILAC AND NOITAZIDRADNATS
3.2 elpmaS ,sredloH edam morf ,lekcin stainless ,leets 6.1 ehT noitarbilac rotcaf is denimreted yb using
glass, ro rehto evitcaernon .lairetam slairetam htiw nwonk retaw .tnetnoc
1
IS 13360 (Part 3/Set 9) : 1999
6.2 ruoF sdohtem are debircsed for esu htiw the 6.6 Method for esU htiw muissatoP etartraT
noitarbilac :slairetam etardyhimeH
)i ;retaW sihT dohtem sesu muissatop tartrate etardyhimeh htiw
)ii muidoS tartrate ;etardyhed a laciteroeht water tnetnoc of 3.83 tnecrep as the sisab
of .noitazidradnats
)iii muidoS etatsgnut ,etardyhed dna
)vi muissatoP tartrate. Repeat the steps nevig ni 6.4.1,6.4.2,6.4.3, dna 6.4.4
except esu 25 ot 30 .gm
ehT dednemmocer noitarbilac lairetam si muidos
etatsgnut ,etardyhed hcihw si elbats ni( the suordyhna 6.7 etaluclaC the noitarbilac factor, K, ni smargorcim
)mrof ot serutarepmet evoba 1 .C°000 setartraT nac per margorcim ,gnidaer as :swollof
esopmoced evoba C°022 dna nac esuac noitaroireted
of the detector.
F x W,, 1 000
K=
6.3 Method for Use with Water cRstd - RB)
A ssalg yrallipac )ettepiporcim( si desu ot erusaem a where
nwonk ssam of water, yllacipyt 2 .gm
K= noitarbilac factor ni smargorcim per
6.3.1 Prepare rezylana for esu as debircsed ni 7. margorcim ;)g&g@
6.3.2 lliF the ettepiporcim yb gnidloh ti at tniopdim F= noitcarf of dradnats lairetam detubirtta ot
:retaw
htiw a riap of tweezers dna gnippid ylthgil ni dellitsid
water. water dohtem F = 1.00
muidos tartrate dohtem F = 0.1566
6.3.3 evomeR the erutsiom morf the sedis of the ettepip
htiw tnebrosba .eussit ekaT care ton ot hcuot the dne muidos etatsngut dohtem F = 0.1092
of the ettepip htiw the eussit esuaceb ti lliw brosba the ssam of dradnats ,lairetam ;gm
Wstd =
erutsiom morf the .yrallipac gnidaer for dradnats ,lairetam ;gp dna
d% =
6.3.4 retfA gnillif the ,ettepip ecalp ti ni the elpmas R, = gnidaer for ,knalb .gy
redloh dna set the redloh ni the .nevo 6.8 ehT noitarbilac factor dluohs eb 1 .OO f 0.10. A
factor edistuo these stimil dluow etacidni a melborp
6.3.5 nuR the sisylana- dna record the water retnuoc
hcus as a detanimatnoc or detaroireted detector.
gnidaer as dradnats gnidaer (&). esU na sisylana emit
of 20 setunim dna a erutarepmet of .C°051
7 ERUDECORP
6.4 Method for Use with Sodium Tartrate
7.1 noitaraperP of elpmaS Holders
Dehydrate
7.1.1 fI staob are ,desu yrd as ynam staob as tneinevnoc
sihT dohtem sesu muidos tartrate etardyhed htiw a
at 100 ot C°501 ni a gnitalucric ria nevo for at tsael
laciteroeht water tnetnoc of 15.66 tnecrep as the sisab
1 h.
of .noitazidradnats
7.1.2 evomeR the staob morf the nevo dna yletaidemmi
6.4.1 Prepare the rezylana for esu as debircsed ni 7.
ecalp meht ni a rotaccised ot looc for at tsael 15 nim
6.4.2 hgieW ot the tseraen 0.1 ,gm 10 ot 13 gm of erofeb .gnisu
muidos tartrate etardyhed dna ecalp ni the elpmas
7.1.3 fI staob are ton ,desu neht store the elpmas redloh
.redloh nihtiw the .nevo
6.4.3 ecalP elpmas redloh dna stnetnoc ni the .nevo
7.2 Initial Settings
6.4.4 Repeat as debircsed ni 6.3.5.
7.2.1 tsujdA the ecruos negortin erusserp ot 35 f 3 kPa.
6.5 Method for esU htiw muidoS etatsgnuT 7.2.2 tsujdA the negortin wolf lortnoc evlav ot a wolf
etardyheD rate of 70 f 20 .etunim/3mc sihT tnemtsujda llahs eb
edam htiw the elpmas nevo .desolc
sihT dohtem sesu muidos etatsgnnt htiw a laciteroeht
water tnetnoc of 10.92 tnecrep as the sisab of 7.2.3 tsujdA the rezylana dnuorgkcab tnuoc rate yb
.noitazidradnats gnittes the margorcim water tnetnoc ot a gnitnuoc rate
of 0.8 f 0.3 etunim/gp for the tnoPuD .tnemurtsni
Repeat the steps nevig ni 6.4.1,6.4.2,6.4.3, dna 6.4.4
except esu 15 ot 19 .gm 7.2.4 tsujdA the nevo erutarepmet lortnoc ot the
2
IS 13360 (Part 3/Set 9) : 1999
deriuqer tset erutarepmet rof eht citsalp gnieb Expected erutsiom tnernoC Approximate Sample Size,
.dezylana )tnecrep( )g(
0.005 ot 0.1 2
NOTE - ehT lairetam noitacificeps llahs eb dekcehc rof eht
0.1 ot 0.5 0.5
deriuqer tset .erutarepmet fI eht tset erutarepmet si ,nwonknu ti
0.5 ot 1.0 0.2
lliw evah ot eb denimreted yllatnemirepxe ees( xennA .)B
1 5ot 0.05
5 to10 0.02
7.3 Determination of Blank
7.4.3 nruteR eht elpmas redloh ot eht rezylana .nevo
7.3.1 nepO eht rezylana nevo and tes a deird elpmas
redloh ydaer rof .noitresni 7.4.4 Adjust eht emit lortnoc ot eht deriuqer tset .emit
7.3.2 esopxE eht redloh and rezylana nevo ot eht 7.4.5 At eht dne fo eht deriuqer tset ,emit drocer eht
yrotarobal erehpsomta rof 20 f 3 .sdnoces ecalP eht retaw retnuoc gnidaer as eht elpmas ,gnidaer R,.
elpmas redloh ni nevo and .esolc ehT gnimit doirep
7.4.6 teseR eht retaw retnuoc ot .orez
starts at eht instant eht nevo rood is denepo and sdne
7.4.7 evomeR eht elpmas redloh morf eht .nevo
nehw ti is .desolc
7.4.8 nehW eht elpmas has ,delooc evomer ti morf eht
7.3.3 teseR eht retaw retnuoc ot .orez
elpmas redloh and hgiew ti ot f 0.1 ,gm 4ti .)elpmas(
7.3.4 Adjust eht emit lortnoc ot eht deriuqer tset emit
NOTE sihT- dohtem sah neeb nettirw rof slairetam taht od ton
rof eht citsalp gnieb .dezylana
erehda ta eht elpmas .redloh slairetaM taht od erehda llahs eb
dehgiew erofeb gnicalp ni eht elpmas .redloh
7.3.5 At eht dne fo eht deriuqer tset ,emit drocer eht
retaw retnuoc gnidaer as eht blank, R,.
8 CALCULATION
NOTE roF- gnol tset ,semit eht emit deriuqer ot enimreted eht
0.1
knalb (RJ yam eb denimreted yb gninimreted eht dnuorgkcab erutsioM ,tnetnoc tnecrep = K(R, R,) x
tnuoc etar dna)C( eht detalumucca dnuorgkcab (B) retfa 10 nim A4
evah ,despale neht gniylpitlum siht tnuoc etar yb gniniamer emit
erehw
dna gnidda ti ot eht detalumucca :dnuorgkcab
gnidaer rof ,elpmas ;gp
R, = ,,B + C t( - 10 )nim =
4
= gnidaer rof blank, ;gp
BR
erehw
K = noitarbilac rotcaf ,gnidaer gu/gu (shall eb
raen )ytinu ;)7.6( and
gnidaer rof blank, pg
R, =
A4 = mass fo eht elpmas ni .gm
detalumucca dnuorgkcab retfa 10
% =
,setunim pg
9 TROPER
c = dnuorgkcab tnuoc ,etar ;etun im/gp and ehT tset troper shall edulcni eht gniwollof :noitamrofni
t = latot sisylana ,emit setunim
)a etelpmoC noitacifitnedi fo eht elpmas detset
7.4 Determination of Sample Moisture gnidulcni epyt fo ,lairetam ,ecruos -cafunam
s’rerut edoc and ,mrof
7.4.1 evomeR eht elpmas redloh morf .nevo
)b etaD fo ,tset
7.4.2 ecalP etairporppa elpmas ezis ni eht elpmas )c laudividnI nemiceps ,sgnidaer
redloh ees( .)etoN ehT redloh shall eb dellif and
)d laudividnI nemiceps blanks ,sgnidaer
denruter ot eht nevo nihtiw 20 f 3 .sdnoces
)e laudividnI nemiceps erutsiom ,sgnidaer
NOTE - elpmaS ezis si desab no eht detcepxe erutsiom tnetnoc )f laudividnI nemiceps erutsiom ,tnetnoc and
fo eht .elpmas ehT gniwollof elbat yam eb desu sa a :ediug
)g egarevA erutsiom .tnetnoc

3
IS 13360 (Part 3/Set 9) : 1999
ANNEX A
(Foreword and Clause B- 1.3)
DIRECTIONS FOR CLEANING AND RECOATING THE ELECTROLYTIC CELL
A-l evomeR the citylortcele llec morf the .tnemurtsni A-l.8 ,niagA evomer the citylortcele llec morf the
tnemurtsni dna ylppa muucav ot eno port.
A-l.1 tcennoC eno port of the llec ot a ecruos of
muucav hcus as a (water) rotaripsa or muucav pmup 9.l-A Prepare a 2 ot 8 noitulos yb emulov of tnegaer
htiw noitcus .ksalf grade (85 )tnecrep cirohpsohp dica ni .enoteca
2.l-A hsulF the llec htiw dellitsid water at tsael evif 01.1-A lliF the llec htiw the cirohpsohp dica .noitulos
,semit ot evomer the dlo .gnitaoc wardhtiW the excess .noitulos
3.l-A hsulF the llec htiw enoteca at tsael evif .semit ETON - oD ton hsulf eht llec htiw ssecxe cirohpsohp dica
,noitulos hcihw yam esuac a pu-dliub fo cirohpsohp dica dna
4.l-A yrD the llec for 2 nim yb gnitaripsa ria hguorht etavitcaed eht :llec
the .llec
A-l.11 yrD the llec for 2 nim yb gnitaripsa ria hguorht
A-1.5 llatsnieR the llec ni the tnemurtsni dna hsilbatse the .llec
negortin .wolf ehT detaocnu llec dluohs ton esuac the
21.1-A llatsnieR the llec ni the tnemurtsni dna
tnuoc ot .esaercni fI ti does ton ,esaercni go ot
etylortcele the llec yb gnigrup ti htiw negortin for at
step .3.1-A fI ti does ,esaercni rehtruf gninaelc of the
tsael 30 nim erofeb gninrut no the .remit
llec si ,deriuqer proceed htiw step .6.1-A
ehT-ETON llec yam eb dezylortcele edistuo eht tnemurtsni yb
6.l-A lliF the llec htiw detartnecnoc cirtin dica dna gniylppa a V-56 cd ot eht sedortcele elihw gnigrup eht llec htiw
tel ti dnats for flah na .ruoh .negortin
7.l-A niarD the ,dica hsulf the llec lareves semit htiw A-1.13 nehW the metsys si yltneiciffus yrd so that ti
dellitsid water, dewollof yb enoteca dna etaripsa .yrd yam eb ,decnalab proceed htiw tnemurtsni
noitarbilac (see 6).

ANNEX B

(Clause 7.2.4)
SELECTION OF TEST TEMPERATURE AND TIME
B-l noitceleS of the proper test erutarepmet dna emit ot a level where gnizylana the elpmas for ssel naht na
si netfo a esimorpmoc neewteb llec efil (that ,si emit lanoitidda etunim segnahc the tnatluser tnuoc yb 1~
litnu gnitaocer si )yrassecen dna emit of .sisylana hgiH .tnecrep fI the latot emit si ssel naht 20 ,nim the emit
serutarepmet yam degrade the elpmas dna evlove dna erutarepmet are .yrotcafsitas ;I the emit si greater
remonom or rezicitsalp gnisuac ssol of .ytivitisnes Low naht 30 ,setunim repeat steps 1.l-B dna 2.l-B at a
serutarepmet ecuder the noitulove of erutsiom dna erutarepmet C°01 .rehgih
gnolorp the .sisylana noitceleS of the mumitpo test
3.l-B ,fI after gnikam lareves tests rednu the
erutarepmet dna emit ,si therefore, a rorre-dna-lairt snoitidnoc denimreted ni 1.l-B dna ,2.1-B ssol of
process. ytivitisnes si ,devresbo naelc dna recoat the llec (see
xennA )A dna rewol the erutarepmet of erutuf tests yb
B-l.1 tceleS the nemiceps ezis ot niatnoc tuoba 2 gm
1ooc.
of erutsiom dna set the erutarepmet at .C°011
ETON - detsegguS tset snoitidnoc rof scitsalpdetceles era nevig
2.l-B ezylanA the elpmas litnu the tnuoc rate secuder
ni xennA .C

4
IS 13360 (Part 3/Set 9) : 1999
ANNEX C
(Clause B-l .3)
C-l detsegguS tseT snoitdnoC rof detceleS scitsalP era nevig ni elbaT 1.
Table 1 Suggested Test Conditions for Selected Plastics
SI Plastics Temperature Test Time Sample Size
No. (“C) (Minutes) 69
(1) (2)
(3) (4) (5)
)i Polyamide 175 30 0.2
ii) Thermoplastic polyester 150 45 1
iii) Ionomer 150 30 1
iv) Polyolefin 150 20 2
v) Polycarbonate 20 2
vi) AEIS 20 0.2

5