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Study on reducibility and porosity of metallurgical sinter

Abstract

The paper dealt with research on structural properties of metallurgical sinter. It was aimed at studying of sinter porosity and density in relation to its reducibility. For porosity determination was used immersion technique using Archimedes principle. Density was measured by gas pycnometer and apparent density was calculated from results of measured porosity. These properties were studied in relation to temperature 950 degrees C at which reducibility tests of every sample were carried out according to ISO 4695:2007. For the study 7 batches of 5 samples of sinter originated from industrial metallurgical plant were sorted. The porosity and density were discussed for virgin samples before the test of reducibility and for reduced samples after ISO test. The effect of 950 degrees C on the properties was contemplated and SEM analysis was carried out. The samples porosity before reduction test was in range from 5.1% to 9.82% and for the samples after reduction test it was 32.77-44.12%. The density of samples was not significantly affected by temperature with values ranging from 3.65 to 3.82 g cm(-3) for virgin samples, resp. 4.87-5.37 g cm(-3) for samples after reduction.

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Study on reducibility and porosity of metallurgical sinter

Author: Jursová, Simona
Publisher: Elsevier
Year: 2018
DOI: 10.1016/j.aej.2017.03.007
Source: https://dspace.vsb.cz/bitstreams/00ed08a9-b89b-41fe-ad8d-cf719941af63/download
ORIGINAL ARTICLE
S udy on educibili y and po osi y o me allu gical
sin e
Simona Ju so a
a,*
, Pa lina Pus ejo ska
a
, Sil ie B ozo a
b
a
VS
ˇB – Technical Uni e si y o Os a a, Cen e ENET, 17. lis opadu 15, 708 33 Os a a – Po uba, Czech Republic
b
VS
ˇB – Technical Uni e si y o Os a a, Facul y o Me allu gy and Ma e ial Enginee ing, 17. lis opadu 15, 708 33 Os a a –
Po uba, Czech Republic
Recei ed 6 Ap il 2016; e ised 14 Feb ua y 2017; accep ed 4 Ma ch 2017
A ailable online 25 Ma ch 2017
KEYWORDS
Sin e ;
Reduc ion;
Po osi y;
Densi y;
S uc u e
Abs ac The pape deal wi h esea ch on s uc u al p ope ies o me allu gical sin e . I was aimed
a s udying o sin e po osi y and densi y in ela ion o i s educibili y. Fo po osi y de e mina ion
was used imme sion echnique using A chimedes p inciple. Densi y was measu ed by gas pycnome e
and appa en densi y was calcula ed om esul s o measu ed po osi y. These p ope ies we e s udied
in ela ion o empe a u e 950 °C a which educibili y es s o e e y sample we e ca ied ou acco d-
ing o ISO 4695:2007. Fo he s udy 7 ba ches o 5 samples o sin e o igina ed om indus ial me -
allu gical plan we e so ed. The po osi y and densi y we e discussed o i gin samples be o e he es
o educibili y and o educed samples a e ISO es . The e ec o 950 °C on he p ope ies was con-
empla ed and SEM analysis was ca ied ou . The samples po osi y be o e educ ion es was in ange
om 5.1% o 9.82% and o he samples a e educ ion es i was 32.77–44.12%. The densi y o
samples was no signi ican ly a ec ed by empe a u e wi h alues anging om 3.65 o 3.82 g cm
3
o i gin samples, esp. 4.87–5.37 g cm
3
o samples a e educ ion.
Ó2017 Facul y o Enginee ing, Alexand ia Uni e si y. P oduc ion and hos ing by Else ie B.V. This is an
open access a icle unde he CC BY-NC-ND license (h p://c ea i ecommons.o g/licenses/by-nc-nd/4.0/).
1. In oduc ion
Sin e ed i on o es a e consumed by mos o he mode n blas
u naces as he i on eed o he blas u nace eeds ock [1]. The
o ma ion o he sin e s uc u e is highly complex p ocess
accompanied by a la ge numbe o ac o s ela ed o he p o-
cess echnology as well as chemical and physical phenomena
du ing he sin e ing p ocess. Fo op imal p ocessing o sin e
in blas u naces, he knowledge on sin e s uc u e and sin e
educibili y is essen ial. The mine alogical s uc u e, po osi y
o sin e ed ma e ials and i s o ma ion ha e been widely s ud-
ied. Nishioka e ealed ha he po e sizes ha e a g ea in luence
on he e ec i e he mal di usi i y as well as po osi y [2].
McCann e al. discussed he speci ic hea capaci y as well as
chemical and s uc u al changes o i on o es du ing i s hea ing
[3]. The a en ion was also paid o he s a is ical geome ic
cha ac e is ics o he po e s uc u e. Aizawa and Suwa wo ked
ou a ma hema ical model o de ine e ec s o po osi y, po e
size, shape and hei dis ibu ion [4]. F o
¨hlicho a e al.
analyzed he sin e s uc u e in iew o i anium addi ion o
i [5]. Tian e al. epo ed a cha ac e iza ion o sin e on i s
*Co esponding au ho .
E-mail add esses: simona.ju so[email p o ec ed] (S. Ju so a), pa lina.
[email p o ec ed] (P. Pus ejo ska), [email p o ec ed]
(S. B ozo a).
Pee e iew unde esponsibili y o Facul y o Enginee ing, Alexand ia
Uni e si y.
Alexand ia Enginee ing Jou nal (2018) 57, 1657–1664
HOSTED BY
Alexand ia Uni e si y
Alexand ia Enginee ing Jou nal
www.else ie .com/loca e/aej
www.sciencedi ec .com
h p://dx.doi.o g/10.1016/j.aej.2017.03.007
1110-0168 Ó2017 Facul y o Enginee ing, Alexand ia Uni e si y. P oduc ion and hos ing by Else ie B.V.
This is an open access a icle unde he CC BY-NC-ND license (h p://c ea i ecommons.o g/licenses/by-nc-nd/4.0/).
s uc u al and he mophysical p ope ies owa d was e hea
eco e y applica ions. They used a ac al model o p edic
he e ec i e he mal conduc i i y as a unc ion o po osi y
[6].Bo
¨lu
¨kbasßi e al. s udied po osi y and s uc u e o me allu -
gical sin e in ela ion o i s quali y [7].
Va ious measu emen echniques we e applied o sin e
s uc u e cha ac e iza ion. By Janowski e al. he s e eologic
analysis o a solid g ain o educed hema i e was applied o
de e mina ion o i s po osi y [8]. Sha okha e al. analyzed sin-
e po osi y by applica ion o 3D omog aphy me hod [9,10].
A men ion abou mo phological in es iga ion and educibili y
es ing used o lump o es b and cha ac e iza ion in indus ial
– scale p ocess condi ions was p esen ed in a esea ch pape by
Hanel e al. [11].
Howe e , s udies abou ela ion be ween s uc u al p ope -
ies such as po osi y and educibili y a e no nume ous and a e
associa ed wi h g ea unce ain ies due o he a ia ions in he
s uc u e and composi ion o sin e . This pape wan ed o p e-
sen esul s o esea ch on po osi y and densi y o me allu gi-
cal sin e o igina ed om a Eu opean me allu gical plan in a
iew o sin e educibili y. Fo po osi y de e mina ion was
applied a simple echnique accessible o esea ch ins i u ions
wi h no need o signi ican in es men s. The pu pose o his
pape was o deepen gene al unde s anding o s uc u e me al-
lu gical sin e . The esul s we e in ended o con ibu e o gen-
e al knowledge abou co ela ion be ween sin e s uc u e and
i s educibili y. In he pape we e p esen ed i s esul s o
esea ch on comp ehensi e s uc u al analysis such as po osi y
and densi y. E alua ion o he acqui ed esul s was in ended
o ollowing esea ch on po e dis ibu ion, po e sizes and
shape and speci ic su ace a ea o accessible po es.
Gene ally, he bes me allu gical p ope ies a e con em-
pla ed in sin e wi h po es less han 4 mm equally dispe sed
in he ma e ial [12,13]. Sin e wi h unequally dispe sed big
po es is ha dly educible and li le s ong. The mos s ong is
ha one ha has monoli h s one s uc u e, and on he o he
hand i s educibili y is e y low and p ocessing o his
kind o sin e is ypical o high uel consump ion [14]. The sin-
e po osi y is dec eased by inc easing uel consump ion,
dec easing a io o e u n sin e and dec easing sin e basici y
[15].
2. Expe imen al p ocedu e
Expe imen al wo k was done on se en samples o me allu gi-
cal sin e om he p oduc ion o a Czech me allu gical com-
pany. The samples we e ma ked in Figs. 1–7 acco ding o
he o de o hei p ocessing. Chemical composi ion o he
es ed ma e ial is shown in Tables 1 and 2.
2.1. Reducibili y de e mina ion
Tes s o sin e s educibili y dR/d (%/min) we e conduc ed
acco ding o ISO 4695:2007. The samples o size ange 10.0–
12.5 mm we e o en-d ied o cons an mass a 105 °C±5 °C
and be o e p epa a ion o he es po ions hey we e cooled
o oom empe a u e. The es po ion o 500 g was iso he -
mally educed a 950 °C in a ixed bed o educ ion ube wi h
a emo able pe o a ed pla e inside ensu ing uni o m gas low
using educing gas consis ing 40.0% o CO and 60.0% o N
2
[15]. The po ion was weighed a speci ied ime in e als un il
i s deg ee o educ ion eaches 65%. The deg ee o educ ion
R
, ela i e o he i on (III) s a e a e min is calcula ed, as
ollows (1) [16].
R ¼0:111w1
0:430w2
þm1m
m00:430w2
100

100 ð1Þ
Whe e
m
0
is he s a mass o he es po ion be o e hea ing o
educ ion empe a u e 950 °C [g]
m
1
is he mass o he po ion hea ed o 950 °C and imme-
dia ely be o e s a ing he educ ion [g]
m
is he mass o he es po ion a e educ ion ime [g]
w
1
is he i on (II) oxide con en [%]
w
2
is he o al i on con en [%]
The educibili y index, exp essed as he a e o educ ion a
he a omic a io o O/Fe o 0.9 [%/min] is calcula ed om Eq.
(2) and is p esen ed in Table 3.
dR
d
O
Fe ¼0:9

¼33:6
60  30
ð2Þ
whe e
30
is he ime o a ain a deg ee o educ ion o 30% [min]
60
is he ime o a ain a deg ee o educ ion o 60% [min]
2.2. Po osi y de e mina ion
Po osi y o he es ed sin e s /(%) was de e mined by imme -
sion me hod applying A chimedes p inciple as he buoyan
o ce on a subme ged objec is equal o he weigh o he luid
ha is displaced by he objec . The p ocedu e o po osi y mea-
su ing is p esen ed in Fig. 1.
Figu e 1 Scheme o po osi y measu ing.
1658 S. Ju so a e al.
Fo he inal po osi y calcula ion d y weigh s (a), sus-
pended weigh s o samples (b) and soaked weigh s o samples
(c) (Fig. 2) we e used acco ding o Eq. (1).
U½%¼G3G1
G3G2
100 ð3Þ
whe e
G
1
d y weigh [g]
G
2
suspended weigh [g]
G
3
soaked weigh [g]
Fo each ype o es ed sin e s, i e samples we e aken o
de e mine hei po osi y. The a e age po osi y o sin e s
samples is summa ized in Tables 4 and 5. They p esen po os-
i y o i gin samples and po osi y o samples a e he es o
educibili y.
2.3. Densi y de e mina ion
The appa en densi y q(g/cm
3
) and he ue densi y o he solid
ma ix qs(g/cm
3
) we e de e mined. The ue densi y o samples
was de e mined using gas pycnome e Accupyc 1330, whe eas
he appa en one was calcula ed using da a acqui ed du ing
po osi y measu emen s ollowing A chimedes p inciples, as
ollows (4):
Figu e 2 De ini ion o samples du ing po osi y measu ing.
Figu e 3 Su ace o sample 2 be o e educ ion.
Figu e 4 Su ace o sample 3 be o e educ ion.
Figu e 5 Su ace o sample 2 a e educ ion.
Figu e 6 Su ace o sample 3 a e educ ion.
Reducibili y and po osi y o me allu gical sin e 1659
qZ¼qH2O
G1
G3G2
ð4Þ
whe e
qH2Odensi y o wa e 998 kg m
3
The esul s o densi y measu ing a e p esen ed in Tables 4
and 5.
3. Resul s and discussion
The educibili y o es ed samples eached alues lowe han
1%min
1
excluding highly basic sample 2. In compliance wi h
many esea ch [16–20] i con i med posi i e e ec o highe
basici y on sin e educibili y. Howe e , educibili y index o
sample 1 wi h highe basici y is no iceably low which ela es
o high FeO con en . Resul s o po osi y measu emen s p o ed
he s ong e ec o high empe a u e on po es olume. I was
no ed ha he po osi y, as measu ed by he wa e displacemen
me hod, ep esen ed he po osi y o closed-po es, anging
om 5.1% o 9.82% o i gin samples be o e educ ion and
much highe alues o samples a e educ ion a 950 °Cin
ange om 32.77% o 44.12%. The po osi y o p esen ed i -
gin samples is lowe han i was men ioned in he li e a u e [6]
wi h a e age po osi y anging om 12% o 24%. Howe e ,
densi y o samples was a ec ed by high empe a u e jus
sligh ly. High empe a u e o educibili y es s inc eased he
densi y a ound 1 g cm
3
. The appa en densi y in ange om
3.65 o 3.82 g cm
3
esponded he expe ience [6].
The mos po ous sample was sample 2 wi h FeO con en
7.00% and ex emely high basici y 2.33. In acco dance wi h
wo ldwide expe ience [21], his sample was e y well educible.
High educ ion index ela es o sample p ope ies such as i s
high basici y and i s high po osi y. Me allu gical sin e wi h
low basici y has a high a io o ayali e which a ec s sin e ing
p ocess wi h ex emely high gene a ion o liquid phase making
Figu e 7 SEM on sample 2 be o e educ ion.
Table 1 Chemical analysis o es ed sin e s – Pa 1.
Sample FeO Fe C Mn S C Zn
[%]
1 13.7 56.10 0.04 0.29 0.15 0.035 0.0038
2 7.00 51.10 0.09 0.24 0.04 0.028 0.0036
3 8.27 55.98 0.11 0.22 0.016 0.040 0.0059
4 7.19 56.55 0.10 0.15 0.014 0.024 0.0061
5 11.6 55.51 0.03 0.43 0.013 0.038 0.018
6 9.50 58.14 0.03 0.05 0.006 0.040 0.052
7 5.54 57.80 0.15 0.44 0.014 0.010 0.0052
Table 2 Chemical analysis o es ed sin e – pa 2.
Sample SiO
2
CaO MgO Al
2
O
3
K
2
O TiO
2
P
2
O
5
[%]
1 8.83 9.46 1.24 1.16 0.05 0.54 0.14
2 6.38 14.90 1.10 1.19 0.03 0.52 0.13
3 8.36 9.51 1.79 0.99 0.02 0.049 0.13
4 8.73 8.26 1.31 0.93 0.05 0.048 0.12
5 8.97 9.37 1.26 0.86 0.01 0.044 0.11
6 8.20 6.91 1.18 1.09 0.07 0.067 0.10
7 8.40 8.20 1.79 1.13 0.06 0.057 0.10
Table 3 Reducibili y o samples.
Sample dR/d [%min
1
] Basici y
1 0.53 1.70
2 1.31 2.33
3 0.81 1.22
4 0.65 0.99
5 0.71 1.80
6 0.89 0.87
7 0.70 0.98
1660 S. Ju so a e al.
he p oduc oo sin e ed esul ing in i s ha d educibili y.
C ea ing o ayali e in he sin e du ing i s p oduc ion is possi-
ble o educe by CaO o CaCO
3
o ming silica es o e i es a
high empe a u es ins ead o ayali e [22].
Howe e , a e he educ ion a 950 °C he po osi y o sam-
ple 2 was no e ained so signi ican . The highes po osi y a e
he educ ion a 950 °C was indica ed in sample 3.
These samples and he changes in hei mic os uc u es
we e s udied h ough SEM analysis. In Figs. 3 and 4 a e shown
he ep esen a i e pic u es o su ace s uc u e o he i gin
samples be o e educ ion p ocess. Sample 2 be o e educ ion
was c ea ed by wide agmen s o e ous elemen s and li le
undis inguished a eas c ea ed mainly by oxygen accompanied
by elemen s such as Na, Mg, Ca, and Si (Table 6). On he su -
ace o sample 3 was de ec ed highe a io o Fe han on he
su ace o sample 2 (Table 7). A e he educ ion es ing he
su ace o bo h samples (Figs. 5 and 6)was isibly no iceably
ans o med. The wide e ous agmen s we e educed in o
small o ma ion. The e we e no iced ib ous a eas c ea ed by
oxygen and accompanying elemen s. Fe ous agmen s on
he su ace o es ed sample 2 and sample 3 we e educed
and a e hei educ ion he e we e de ec ed elemen s such
as O
2
, Mg, Si, Ca, and Al (Tables 8 and 9). Howe e , on
Table 4 Po osi y and densi y o samples be o e educ ion es .
Sample /[%] q
s
[g cm
3
]q[g cm
3
]
1 9.55 4.62 3.65
2 9.82 4.21 3.71
3 6.61 4.42 3.70
4 6.46 4.16 3.76
5 7.26 4.18 3.77
6 7.86 4.39 3.74
7 5.81 4.28 3.82
Table 5 Po osi y and densi y o samples a e educ ion es .
Sample /[%] q
s
[g cm
3
]q[g cm
3
]
1 32.77 4.87 2.96
2 34.28 5.12 3.20
3 44.12 5.10 2.72
4 39.03 5.19 2.86
5 35.49 5.25 3.30
6 35.89 5.19 2.96
7 37.05 5.37 3.11
Table 6 Su ace mic oanalysis o sample 2 be o e.
O
2
Na Mg Al Si Ca Fe
1a 42.52 – – 0.48 0.12 0.19 56.69
2a 55.33 0.62 0.82 3.78 15.11 18.05 6.31
Table 7 Su ace mic oanalysis o sample 3 be o e.
O
2
Na Mg Al Si Ca Fe
1a 22.73 – – 0.28 0.28 0.36 76.35
2a 46.02 0.22 1.24 0.81 23.11 12.08 16.53
Table 8 Su ace mic oanalysis o sample 2 a e .
O
2
Na Mg Al Si Ca Fe
1 0.42 – 0.25 0.20 – 0.80 98.25
1 1.55 – 0.15 0.38 – 0.89 97.03
2 33.27 0.32 1.26 11.35 – 29.70 24.11
3 51.71 0.24 0.15 13.72 0.41 31.86 1.91
Table 9 Su ace mic oanalysis o sample 3 a e .
O
2
Mg Al Si Ca Fe
1 5.57 1.66 1.43 0.60 2.04 88.70
1 3.83 0.65 1.06 0.47 1.42 92.57
2 46.85 0.68 0.48 13.26 32.56 6.17
Reducibili y and po osi y o me allu gical sin e 1661

su ace o sample 3 was de ec ed no Na as i is p esen ed in
Table 9.Figs. 7–10 p esen iew o samples mic os uc u e in
highe magni ude. The analyses o ma gins o samples 2 and
3 be o e and a e educ ion a e documen ed in Figs. 11–14
wi h de ail in o ma ion eco ded in Tables 10–13. In ma gin
s uc u e o i gin samples we e egions in which he p esence
o i on oxides was eco ded. Some e ous oxides con ained
elemen s such as Mg and Ca. The e we e iden i ied highe con-
en o Ca, Si oxides and ace amoun o Fe and P. In he ma -
gin s uc u e o samples 2 and 3 be o e educ ion we e
Figu e 8 SEM on sample 2 a e educ ion.
Figu e 9 SEM on sample 3 be o e educ ion.
Figu e 10 SEM on sample 3 a e educ ion.
Figu e 11 Ma gin o sample 2 be o e educ ion.
Figu e 12 Ma gin o sample 2 a e educ ion.
Figu e 13 Ma gin o sample 3 be o e educ ion.
1662 S. Ju so a e al.
obse ed sha p egions wi h e ous oxides and Si and Ca.
A e 950 °C educ ion in he samples 2 and 3 we e iden i ied
po ous elemen s o almos pu e Fe and da ke segmen s o
Ca and Si oxides. The e was no ed me allic ilm on he la ge
pa icles o Fe oxides in he ma gin s uc u e o sample 3.
The s a is ical e alua ion o acqui ed expe imen al esul s
e ealed a he a low co ela ion be ween po osi y o es ed
samples and hei educibili y (R = 0.426). The po osi y o
s udied samples was a ec ed by sample basici y (R = 0.747).
A s ong e ec o FeO con en on po osi y o hese samples
was no con i med. The e was eco ded a close ela ion
be ween educibili y and ue densi y o samples
(R = 0.896), which was in e p e ed ha he olume o any
open and closed po es o s udied me allu gical sin e had no
a ec ed he sample educibili y.
Figu e 14 Ma gins o sample 3 a e educ ion.
Table 10 Analysis o sample 2 be o e educ ion.
O
2
Mg Al Si Ca Fe
1a 36.20 2.87 0.47 – 0.96 59.51
1a 37.00 2.63 0.49 – 1.03 58.84
2a 45.20 0.47 1.17 14.38 21.63 17.15
2a 45.05 0.47 1.29 14.94 16.37 21.74
3a 47.58 0.42 1.26 17.49 23.84 9.42
3a 48.10 0.43 1.43 17.23 23.58 9.24
Table 11 Analysis o sample 2 a e educ ion.
O
2
Mg Al Si Ca Fe
1 – – – – – 100
1 – – – – – 100
2 29.58 – 0.44 0.36 – 69.61
2 30.16 – 0.52 0.28 – 69.04
3 44.27 – 1.13 16.88 24.53 13.20
4 46.11 – 0.96 19.93 26.45 6.54
Table 12 Analysis o sample 3 be o e educ ion.
O
2
Na Mg Al Si Ca Fe
1a 37.72 – – 0.40 – – 61.89
2a 57.56 0.28 0.28 1.37 16.40 18.97 5.14
3a 35.71 – 1.32 0.49 – 0.63 61.86
Table 13 Analysis o sample 3 a e educ ion.
O
2
Mn Mg Al Si Ca Fe
1 29.78 0.5 0.93 0.60 – – 68.9
2 46.53 – 0.15 1.22 16.39 24.72 10.99
3 – – – – – – 100
Reducibili y and po osi y o me allu gical sin e 1663
4. Conclusions
Indus ial sin e sampled om a me allu gical company was
subjec ed o a comp ehensi e se o cha ac e iza ions on hei
basic s uc u al p ope ies owa d hei educibili y and p o-
cessing in blas u nace eeds ock. Se e al concluding ema ks
could be d awn as ollows:
1. Po osi y o es ed sin e inc eased mul iply a high empe -
a u e, whe eas densi y o samples was no a ec ed by em-
pe a u e signi ican ly.
2. Po osi y o closed po es anged om 5.1% o 9.82% and
a e educ ion 32.77% o 44.12%. Densi y was measu ed
in he ange om 3.65 o 3.82 g cm
3
and o educed sam-
ples om 4.87 o 5.37 g cm
3
.
3. The maximum po osi y was measu ed in sample wi h he
highes educibili y index and basici y. Howe e , he se
o samples did no p o e signi ican s a is ical co ela ion
be ween po osi y and educibili y. The e was con i med
he e ec o sample basici y on hei po osi y. The s udy
e ealed a co ela ion be ween ue densi y and educibili y
o samples excluding he olume o any open and close
po es. Fo e i ied conclusion he sample ange will be
ex ended in u u e wo k.
4. To isually compa e he po e s uc u e o i gin and
educed samples SEM analysis was ca ied ou in combina-
ion wi h EDX o de e mine he elemen composi ion. In
gene al, he po es o bo h samples include mac o-po es o
ca i ies wi h he size o millime e s and mesopo es in he
mic ome e ange. The images indica e he e ec o high
empe a u e on i on oxide educ ion. A e educibili y es
in CO en i onmen a 950 °C, high a io o Fe in co e o
samples, in some poin s eaching 100%, was no ed. The ele-
men al analysis accompanying he images iden i ied mo e
comple e educ ion in sample 2 which was ound o be he
mos po ous i gin sample in he es ing ba ch. SEM anal-
ysis p o ed he posi i e e ec o highe po osi y on educ-
ion o sample.
Acknowledgmen s
This pape was conduc ed wi hin he amewo k o he p ojec
LO1404: Sus ainable de elopmen o ENET Cen e and sup-
po ed by Speci ic esea ch SP2017/98 –Adjus men o syn he-
sis gases o hei u iliza ion in seconda y powe machines.
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