Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites
A poly(lactic acid)/poly(trimethylene terephthalate) (PLA/PTT) composite was prepared by melt blending to improve the PTT crystallization rate. Morphology analysis of PLA/PTT fractured surfaces demonstrated the compatibility of its components. Thermogravimetric analysis revealed that the thermodegra...
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| Цитувати: | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites / C.-Y. Tsou, C.-L. Wu, Y.-C. Tseng, S.-H. Chiu, M.-C. Suen, W.S. Hung, C.-H. Tsou // Проблемы прочности. — 2017. — № 1. — С. 190-199. — Бібліогр.: 29 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860005690957889536 |
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| author | Tsou, C.-Y. Wu, C.-L. Tseng, Y.-C. Chiu, S.-H. Suen, M.-C. Hung, W.S. Tsou, C.-H. |
| author_facet | Tsou, C.-Y. Wu, C.-L. Tseng, Y.-C. Chiu, S.-H. Suen, M.-C. Hung, W.S. Tsou, C.-H. |
| citation_txt | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites / C.-Y. Tsou, C.-L. Wu, Y.-C. Tseng, S.-H. Chiu, M.-C. Suen, W.S. Hung, C.-H. Tsou // Проблемы прочности. — 2017. — № 1. — С. 190-199. — Бібліогр.: 29 назв. — англ. |
| collection | DSpace DC |
| container_title | Проблемы прочности |
| description | A poly(lactic acid)/poly(trimethylene terephthalate) (PLA/PTT) composite was prepared by melt blending to improve the PTT crystallization rate. Morphology analysis of PLA/PTT fractured surfaces demonstrated the compatibility of its components. Thermogravimetric analysis revealed that the thermodegradation of a PLA/PTT sample was higher than that of PLA. Differential scanning calorimetry was used to evaluate the crystallization behavior. The Avrami equation described the isothermal crystallization kinetics. The Hoffman-Weeks parameters indicated that the PLA presence increased slightly the PTT nucleation. The tests of PLA, PTT, and PLA/PTT specimens in tension showed that a percent elongation of the PLA/PTT composite was between that of PLA and PTT; however, the tensile strength of the PLA/PTT composite was similar to that of PLA.
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UDC 539.4
Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT
Polymer Composites
C.-Y . T sou ,a C .-L . W u ,a Y .-C . T seng ,a S.-H. C h iu ,a M .-C . S uen,b W . S. H u n g ,c and
C .-H . T so u d,e1
a Department of Materials Science and Engineering, National Taiwan University of Science and
Technology, Taipei, Taiwan
b Lee-Ming Institute of Technology, Department of Fashion Business Administration, Taishan, New
Taipei City, Taiwan (R.O.C.)
c R&D Center for Membrane Technology, Chung Yuan University, Chung Li, Taiwan
d Institute of Materials Science and Engineering, Material Corrosion and Protection Key Laboratory
of Sichuan Province, Sichuan University of Science and Engineering, Zigong, China
e Faculties of Biological and Chemical Engineering, Faculties of Materials Engineering, Science and
Technology Innovation Center, Panzhihua University, Panzhihua, China
1 mayko0301@hotmail.com
A poly(lactic acid)/poly(trimethylene terephthalate) (PLA/PTT) composite was prepared by melt
blending to improve the PTT crystallization rate. Morphology analysis o f PLA/PTT fractured
surfaces demonstrated the compatibility o f its components. Thermogravimetric analysis revealed that
the thermodegradation o f a PLA/PTT sample was higher than that o f PLA. Differential scanning
calorimetry was used to evaluate the crystallization behavior. The Avrami equation described the
isothermal crystallization kinetics. The Hoffman-Weeks parameters indicated that the PLA presence
increased slightly the PTT nucleation. The tests o f PLA, PTT, and PLA/PTT specimens in tension
showed that a percent elongation o f the PLA/PTT composite was between that o f PLA and PTT;
however, the tensile strength o f the PLA/PTT composite was similar to that o f PLA.
K eyw ords: poly(lactic acid), poly(trim ethylene terephthalate), tensile properties, nucleation,
crystallization.
In tro d u c tio n . Poly(lactic acid) (PLA) is a biodegradable polymer, differing from
m ost of therm oplastic polym ers since it is com pounded from such renewable materials, as
sugar cane or corn starch. PLA possesses quite prom ising properties; however, the
brittleness o f the m aterial restricts its applicability and processing abilities [1].
Poly(trim ethylene terephthalate) (PTT) has a structure sim ilar to that o f polybutylene
terephthalate and polyethylene terephthalate [2]. As com pared to these two other
terephthalates, PTT dem onstrates higher bending strength, w hich m akes it suitable for
m anufacturing different materials, such as textiles or engineering plastics [2-4]. The
brittleness o f PLA can be im proved by blending it w ith an elastom er [5-22]. The high
therm ostability o f PTT, blended w ith PLA [23] provided the conditions for studying the
nonisothermal crystallization o f PTT/PLA. However, the isothermal crystallization behavior
o f PLA/PTT com posites has not been reported. In the present study, PTT w as used to
enhance the PLA elongation at break through the m elt-com pounding method. The
H offm an-W eeks equation was applied to predict the equilibrium m elting point (Tm ). The
effect o f PLA on the melting, crystallization, and therm ostability o f PLA/PTT specim ens
was examined. D ifferential scanning calorim etry (DSC) and w ide-angle X -ray diffraction
(W XRD) w ere used to analyze the crystallization behavior o f a PLA/PTT composite.
1. E xperim en ta l. PLA w ith a m elt flow index o f 4 -8 g/10 m in (Nature W orks 2002D)
and PTT w ith a m elt flow index o f 25 g/10 m in (ASTM -D1238), were supplied by Shell
© C.-Y. TSOU, C.-L. WU, Y.-C. TSENG, S.-H. CHIU, M.-C. SUEN, W. S. HUNG, C.-H. TSOU, 2017
190 ISSN Q556-Î7ÎX. Проблемы! прочности, 2QÎ7, N І
mailto:mayko0301@hotmail.com
Isothermal Crystallization Kinetics Effect
Chem ical Co. Ltd., USA. PLA/PTT com posites (70/30 w eight ratio) w ere prepared using a
Brabender at 50 rpm and 250oC for 4 min. PLA, PTT, and PLA/PTT com posites were
studied by therm ogravim etric analysis (TGA), DSC, W XRD, and scanning electron
m icroscopy (SEM). TG A was run in the range o f 30 to 650°C at a heating rate o f 20°C/min.
In DSC, the first round was at a rate o f 100°C/min w ithin 0-250°C for 3 m in to avoid
therm al history effects, followed by a decrease from 250°C to 20°C at a rate o f 5, 10, 20,
and 30°C/min, respectively, to observe the m elt crystallization. W XRD spectra were
obtained using a Rigaku m odel RU-H3R. The data were recorded over the range o f 10 to
35° w ith a scanning interval o f 0.05°.
2. R esu lts an d D iscussion.
2.1. Therm ogravim etric Analysis. The TGA curves for PLA, PTT, and PLA/PTT are
shown in Fig. 1. The PLA therm ostability was im proved by the PTT addition, having the
higher thermostability. Table 1 lists TG A values, dem onstrating that at 5 and 10 wt.%
losses, the tem perature o f the com posite was considerably higher than that o f each
constituent due to the PTT addition to the blend.
T a b l e 1
TGA of PLA, PTT, and PLA/PTT Samples
Specimen Tg at 5 wt.% (°C) Tg at 10 wt.% (0C) Char residue at 600OC (%)
PLA 282.4 311.6 0.57
PTT 369.9 379.7 13.35
PLA/PTT 326.7 335.9 11.33
Note. Heating rate = 20°C/min.
1 '- - - - - - - - - - 1- - - - - - - - - - T- - - - - - - - - - 1- - - - - - - - - - ' - - - - - - - - - - 1 - - - - - - - - - - ' - - - - - - - - - - F- - - - - - - - - - 1 - - - - - - - - - - 1- - - - - - - - - - T - - - - - - - - - - T ~
0 1 0 0 2 0 0 3 0 0 4 0 0 5 0 0 6 0 0
Temperature (°C)
Fig. 1. TGA curves for PLA, PTT, and PLA/PTT.
2.2. D ifferen tia l S ca n n in g Calorimetry. The DSC data for a heating rate o f 20°C/min
are presented in Fig. 2. The Tg o f PLA in the com posite becam e a little higher w ith the
addition o f PTT. A slight cold crystallization o f the PLA/PTT com posite m ight apparently
be due to the partial PTT and PLA compatibility. The nonisothermal crystallization o f PLA,
PTT, and PLA/PTT w as studied w ith DSC. The cooling rate ranged from 5 to 30°C/min.
The crystallinity data for PLA, PTT, and PLA/PTT samples at different cooling rates are
sum m arized in Table 2. As is seen, PLA exhibited no crystallinity because o f its slow
crystallization rate, neat PLA was unable to crystallize. To examine the variation o f the
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C.-Y. Tsou, C.-L. Wu, Y.-C. Tseng, et al.
T a b l e 2
DSC Values for PLA, PTT, and PLA/PTT at Different Cooling Rates
Sample Cooling rate
(OC/min)
T °CTmc, C AHm, J/g X t , %
PTT 5 196.7 45.4 45.4
10 191.8 45.0 45.0
20 190.6 43.2 43.2
30 180.5 40.8 40.8
PLA/PTT 5 198.9 19.6 65.3
10 193.1 15.3 51.0
20 191.8 14.4 47.7
30 186.3 12.3 41.0
i ■ i 1 i ■ i ■ i ■ i
0 50 100 150 200 250
Temperature (°C)
Fig. 2. DSC for PLA, PTT, and PLA/PTT (heating rate = 20oC/min).
crystallization degree o f PTT and PLA/PTT samples, depending on the cooling rate
(5 -3 0 oC/min), the crystallinity ( X t ) o f all the samples was determ ined from the peak areas.
The enthalpy is determ ined as
X t = (A H (DSc ) / AH(!00%) )(100/ W ), (1)
w here A H (100%) PTT = 145.48 J/g [24] and W is the w eight fraction o f PTT in the
sample. For PTT and a PLA/PTT com posite, X t decreased w ith a cooling rate. The data
for the nonisotherm al crystallization are listed in Table 3. The m elt crystallization
tem perature (Tmc ) and X t o f the PLA /PTT com posite is higher than that o f neat PTT.
The PLA com ponent in the PLA/PTT com posite can enhance the PTT crystallization rate.
The relative crystallinity o f the PLA/PTT com posite at several isothermal
crystallization tem peratures is given in Fig. 3. The crystallization requires m ere nucleation
and accum ulation o f the m olecular chains, although higher isotherm al crystallization
tem peratures hinder nucleation because the m olecular chain m otion is easier. Therefore, the
nucleation can be controlled; at low tem peratures, the nucleation can easily be reached, but
the m olecular m otion is m ore difficult.
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Isothermal Crystallization Kinetics Effect
T a b l e 3
Avrami Parameters for Various Crystallization Temperatures
Sample Tc , °C A H , J/g X t , % t1/2> min n K , s_1 R 2
PTT 197 50.5 50.6 0.46 2.21 3.894 0.998
199 48.6 48.7 0.71 2.27 1.801 0.997
201 45.3 45.5 1.04 2.55 0.676 0.998
203 41.4 41.4 1.51 2.73 0.173 0.999
205 40.5 40.5 2.06 2.85 0.041 0.997
PLA/PTT 197 17.2 57.3 0.71 2.17 1.508 0.999
199 16.0 53.3 0.86 2.27 0.916 0.998
201 14.1 47.0 1.21 2.45 0.391 0.999
203 13.1 43.7 1.81 2.45 0.134 0.997
205 12.3 41.0 2.67 2.50 0.045 0.999
0 1 2 3 4 5 6 7
Time (min)
Fig. 3. Relative crystallinity of PLA/PTT.
The Avrami calculation defined the isotherm al crystallization kinetics o f PTT, PTT,
and PLA /PTT samples [25]. The relation betw een X t and tim e t is indicated by
1— X t = exp(— k t n ). (2)
Taking the double natural logarithm o f this calculation, w e get
ln[ ln(1 X t ) ]= n ln t + ln k , (3)
where n is the Avram i exponent and k is the kinetic param eter o f the isotherm al
crystallization. Equation (3) was used to p lo t the linear curves for PLA/PTT data in Fig. 4;
the slope was equal to the A vram i exponent n for the y-intercept corresponding to the
kinetic param eter (k). Those values for all samples are cited in Table 3.
The X t value o f the PLA/PTT com posite shows unessential differences at varying
crystallization temperatures. The Avrami exponents n for the PLA/PTT com posite were
w ithin 2 .0-3.0. D issim ilar n values indicate unlike crystalline forms and nucleation of
crystals. The t y 2 value for isotherm al crystallization w as deduced from the equation:
t m = ( l n 2 к f n . (4)
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C.-Y. Tsou, C.-L. Wu, Y.-C. Tseng, et at.
Fig. 4. Avrami plots for PLA/PTT samples at different isothermal crystallization temperatures.
The k value for all the samples declined w ith the isotherm al crystallization
tem perature, w hich is due to the low er viscosity at higher tem peratures; thus, the kinetic
energy o f the polym er was growing. However, increasing entropy inhibits the form ation o f
crystal nuclei, causing a decrease in the crystal growth. In contrast, the t 1/2 values for all
the samples increased w ith temperature. The presence o f PLA hinders the m otion o f PTT
m olecular chains; then, the k value for PTT w as reduced due to PLA.
The H offm an-W eeks equation
(Tc / y )+ ( 1 - 1 y T (5)
is usually applied to estimate the Tm value o f sem icrystalline materials. The m elting point
(Tm ) o f the m ain crystallization process was set as Tm because o f num erous m elting peaks
appearing during the PTT m elting [26]. The T ° value can be obtained from the
relationship for Tc and T (Fig. 5). In the scheme, linear regression analysis for num erous
points was perform ed, and by extrapolation, the regression line intersected w ith the line
T = T ̂m *- c •
As is shown in Table 4, Tf0 for the PLA/PTT com posite was slightly higher than Tm
o f neat PTT. The m orphology factor y = L /L , w hich is the thickness ratio o f m olecular
chains. W ith know n Tm, the difference in the crystallization regim e can be found from the
L auritzen-H offm an equation for the spherulite growing rate:
: G0 e x p [- U * /r (Tc - Tx ) ]e x p [-K g /T c ( A T ) f ], (6)
( / 11/2 ) = ( ^ t i /2 )o e x p [-U * /R (T c - T„ )]exp[ - K g /T c ( A T ) f ] . (7)
Tsou [18] substituted ( 1 11/2) and ( 1 11/2 )0 for G and G0, respectively, and obtained
K g = noo e T 0 / A h j k B . (8)
The linear regression results on the logarithm ic scale are dem onstrated in Fig. 6,
U * = 4.12 kcal/m ole, Tx = Tg - 516 (K), f = 2Tc /(T ^ + T c ), f is the correction factor.
194 ISSN 0556-171X. npodneubi npounocmu, 2017, N2 1
Isothermal Crystallization Kinetics Effect
T a b l e 4
Hoffman-W eeks and Lauritzen-Hoffman Parameters for PTT and PLA/PTT
Sample T 0 0CTm, C y R2
PLA - - -
PTT 236.2 1.92 0.988
PLA/PTT 240.1 1.75 0.996
150 170 190 210 230 250 270
Tc (°C)
a
150 170 190 210 230 250
r c (°C )
b
Fig. 5. Hoffman-Weeks plots for PTT (a) and PLA/PTT (b).
1 c .303Tc(aT)f (xio!)
Fig. 6. Lauritzen-Hoffman plots for PLA/PTT.
The slope variations reflected the difference in the crystallization regim e. Regim e II
proceeded at 190-210oC [18]; the slope - K g -105 was about —1.68. The nucleation
m echanism for bo th PTT and the PLA /PTT com posite w as according to regim e II.
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C.-Y. Tsou, C.-L. Wu, Y.-C. Tseng, et al.
T a b l e 5
Hoffman-Weeks and Lauritzen-Hoffman Parameters for PTT and PLA/PTT
Samples Kg Regime e R 2
PLA - - - -
PTT 1.480 II 58.5 0.998
PLA/PTT 1.731 II 61.4 0.989
E quation (7) was used to generate the data for K g listed in Table 5, K g values,
representing the slopes, were found from the regression lines. The higher K g value
corresponds to the better nucleation capability [27, 28]. Consequently, PLA at 70% loading
slightly enhanced the PTT nucleation.
2.3. W XRD. The X -ray diffraction peak positions for PLA, PTT, and PLA/PTT are
shown in Fig. 7. The peaks for PLA w ere observed at the angles 20 o f approxim ately 16.6,
19, and 22.2°, w hich correspond to the reflection planes o f (1— 1— 0), (2— 0 — 3), and
(1— 0 — 5), respectively [28]. The PTT peaks were detected at the angles 20 o f approximately
27.4, 24.7, and 23.5°, w hich correspond to the reflection planes o f (1— 0 — 4), (1— 1— 3), and
(1— 0 — 2), respectively [29]; and at other angles 20 o f approxim ately 21.7, 19.5, 16.7, and
15.2°, w hich are consistent w ith the reflection planes o f (— 1— 0 — 2), (0— 1— 2), (0— 1— 2),
and (0— 1— 0), respectively [29]. However, the PLA/PTT com posite exhibited the
characteristic peaks o f both PLA and PTT, im plying that PLA does not change the PTT
crystal forms.
2000
' A ___________________P LA /P TT
0-1----- 1----- >----- 1----- 1----- 1----- 1----- 1------1----- 1----- 1 250-1----- 1----- 1----- 1----- 1----- 1----- 1----- 1----- 1----- 1----- 1
10 15 20 25 30 10 15 20 25 30
20 (deg) 20 (deg)
a b
Fig. 7. Wide-angle X-ray diffraction for PTT, PLA, and PLA/PTT: (a) cold crystallization and (b) melt
crystallization.
2.4. M orphology. The SEM images o f the fractured surfaces o f PLA, PTT, and
PLA/PTT are illustrated in Fig. 8. The fractured surface o f PLA had a smooth m orphology
(Fig. 8a). A fter blending PLA w ith PTT, some PTT pellets dispersed in the PLA matrix
(Fig. 8c). However, the pellets were not seen clearly because the PTT m olecules are
partially com patible w ith the PLA ones.
2.5. Tensile Properties. The tensile properties o f PLA, PTT, and PLA/PTT are
depicted in Fig. 9. The elongation at break for PLA was only 4.1%. A fter blending PLA
w ith PTT, the PLA/PTT com posite revealed a substantial increase in the elongation at break
(6.2%) since PTT is rather elastic and imparts toughness to PLA. Furtherm ore, the tensile
strength o f PLA was sim ilar to that o f the PLA/PTT com posite; this m ight be because o f the
partial com patibility o f PLA and PTT.
196 ISSN 0556-171X. npoôneMbi npounocmu, 2017, № 1
Isothermal Crystallization Kinetics Effect
a b c
Fig. 8. SEM pictures of PLA (a), PTT (b), and PLA/PTT (c).
P L A P T T P L A /P T T
Fig. 9. Tensile strength (1) and elongation at break (2) of PLA, PTT, and PLA/PTT.
C onclusions. The TG A curves revealed that the therm ostability o f PLA/PTT
com posites was higher than that o f pure PLA because o f the higher therm ostability o f PTT.
In addition, the presence o f PLA in the PLA/PTT com posites slightly increased the PTT
nucleation. Therefore, PLA can increase the crystallization rate o f PTT in the PLA/PTT
com posites. W XRD indicated that PLA did not change the typical peaks and crystal forms
o f PTT. Furtherm ore, the elongation at break o f PLA w as enhanced w ith the PTT addition,
and the tensile strength o f the PLA/PTT com posite was sim ilar to that o f PLA because of
the partial com patibility o f PLA and PTT.
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Received 30. 08. 2016
ISSN 0556-171X. Проблемы прочности, 2017, N2 1 199
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| id | nasplib_isofts_kiev_ua-123456789-173597 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 0556-171X |
| language | English |
| last_indexed | 2025-12-07T16:39:45Z |
| publishDate | 2017 |
| publisher | Інститут проблем міцності ім. Г.С. Писаренко НАН України |
| record_format | dspace |
| spelling | Tsou, C.-Y. Wu, C.-L. Tseng, Y.-C. Chiu, S.-H. Suen, M.-C. Hung, W.S. Tsou, C.-H. 2020-12-12T15:00:02Z 2020-12-12T15:00:02Z 2017 Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites / C.-Y. Tsou, C.-L. Wu, Y.-C. Tseng, S.-H. Chiu, M.-C. Suen, W.S. Hung, C.-H. Tsou // Проблемы прочности. — 2017. — № 1. — С. 190-199. — Бібліогр.: 29 назв. — англ. 0556-171X https://nasplib.isofts.kiev.ua/handle/123456789/173597 539.4 A poly(lactic acid)/poly(trimethylene terephthalate) (PLA/PTT) composite was prepared by melt blending to improve the PTT crystallization rate. Morphology analysis of PLA/PTT fractured surfaces demonstrated the compatibility of its components. Thermogravimetric analysis revealed that the thermodegradation of a PLA/PTT sample was higher than that of PLA. Differential scanning calorimetry was used to evaluate the crystallization behavior. The Avrami equation described the isothermal crystallization kinetics. The Hoffman-Weeks parameters indicated that the PLA presence increased slightly the PTT nucleation. The tests of PLA, PTT, and PLA/PTT specimens in tension showed that a percent elongation of the PLA/PTT composite was between that of PLA and PTT; however, the tensile strength of the PLA/PTT composite was similar to that of PLA. en Інститут проблем міцності ім. Г.С. Писаренко НАН України Проблемы прочности Научно-технический раздел Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites Исследование влияния кинетики изотермической кристаллизации на свойства композита PLA/PTT при растяжении Article published earlier |
| spellingShingle | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites Tsou, C.-Y. Wu, C.-L. Tseng, Y.-C. Chiu, S.-H. Suen, M.-C. Hung, W.S. Tsou, C.-H. Научно-технический раздел |
| title | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites |
| title_alt | Исследование влияния кинетики изотермической кристаллизации на свойства композита PLA/PTT при растяжении |
| title_full | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites |
| title_fullStr | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites |
| title_full_unstemmed | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites |
| title_short | Isothermal Crystallization Kinetics Effect on the Tensile Properties of PLA/PTT Polymer Composites |
| title_sort | isothermal crystallization kinetics effect on the tensile properties of pla/ptt polymer composites |
| topic | Научно-технический раздел |
| topic_facet | Научно-технический раздел |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/173597 |
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