Eu-ARTECH Eu-ARTECH Spectroscopic Techniques for in situ non invasive Study of Natural Dyestuffs Costanza Miliani Centre of Excellence SMAArt University of Perugia, Italy CNR – ISTM (Institute of Molecular Sciences and Technologies)
Eu-ARTECH Spectroscopic Techniques for in situ non invasive Study of Natural Dyestuffs Costanza Miliani Centre of Excellence SMAArt University of Perugia,
Dec 17, 2015
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Eu-ARTECHEu-ARTECH
Spectroscopic Techniques for in situ non invasive
Study of Natural Dyestuffs
Spectroscopic Techniques for in situ non invasive
Study of Natural Dyestuffs Costanza Miliani Costanza Miliani
Centre of Excellence SMAArt
University of Perugia, Italy
CNR – ISTM (Institute of Molecular Sciences and
Technologies)
Eu-ARTECHEu-ARTECH
Catia Clementi, PhD student
Brenda Doherty, PhD student
Alessandro Sassolini, fellowship
Eu-ARTECHEu-ARTECH
How to study in situ natural dyestuffs ?
1. XRF : elemental analysis of mordents and chelation ions
2. FTIR : molecular analysis of mordents and chelant
3. UV-vis abs : color characterization
4. UV-vis fluo : dye characterization
MOLAB equipments
and lab spectrofluorimeter (Varian)
Eu-ARTECHEu-ARTECH
I. Non invasive portable equipments: x-ray fluorescence
The X-ray fluorescence portable equipment for in situ measurements, is made up by:
1. open beam X-ray generator (W target, excitation energy L=9.671 keV);
2. non-cryogenic silicon drift detector SDD having resolution of 130 eV at 5.9 keV.
Eu-ARTECHEu-ARTECHI. Non invasive portable equipments: fiber optic mid-FTIR
it is easily portable:
weight ~35 Kg
volume 50x50x50 cm3
portable JASCO VIR 9500 spectophotometer:
Midac Illuminator IR radiation source
Michelson interferometer
liquid nitrogen cooled MCT
500 1000 1500 2000 2500 3000 3500 4000
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
2.6
21
80
cm
-1
abso
rban
ce (
a.u.
)
wavenumber (cm-1)
Remspec mid-IR fiber optic sampling probe:
19 chalcogenide glass fibers
spectral range: 900-4000 cm-1
best S/N from 900 to 2000 cm–1
abs of Se-H between 2050 and 2250 cm-1
optical layout:
0°/0° geometry
probe surface distance 2-5 mm
Eu-ARTECHEu-ARTECH
A. Exciting light source: 175 W Xenon lamp, 240-650 nm emission.
B. H-10 Jobin Yvon UV monochromator for selecting the excitation wavelength. C. Quartz fibre-optic Y cable
D. CCD spectrometer Avantes AvaSpec-2048 pixels (200-1100 nm) of high sensitivity (86 photons/counting).
E. Optical filters (interference and cut-on filter) are used to cut-off 2nd order scatter and stray light.
I. Non invasive portable equipments: UV-vis fluorescence
Eu-ARTECHEu-ARTECH
1. weld lakes
Eu-ARTECHEu-ARTECH
K
Ca
Argon
Channels
Cou
nts
0
500
1000
1500
2000
Ca (K)
Weld 1 Weld 2 Weld 3
Ca (K)
Argon
Channels
Cou
nts
W1: Ca, W2: Ca, W3: Ca & K
XRF: the mordant
Eu-ARTECHEu-ARTECH
1000 2000 3000 4000 5000 6000
0.0
0.5
1.0
1.5
2.0 Weld 1 allum carbonate
Log
1/R
wavenumber ( cm-1 )
mid FTIR: the mordant
Eu-ARTECHEu-ARTECH
1000 2000 3000 4000 5000 6000
0.0
0.5
1.0
1.5
2.0 Weld 2 allum carbonate
Log
1/R
wavenumber ( cm-1 )
mid FTIR: the mordant
Eu-ARTECHEu-ARTECH
1000 2000 3000 4000 5000 60000.0
0.5
1.0
Weld 3
Log
1/R
wavenumber ( cm-1 )
51
60
mid FTIR: the mordant
OH comb. band
Eu-ARTECHEu-ARTECH
200 300 400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
Abs
orba
nce
/ a.u
.
/ nm
Weld 1 Weld 2 Weld 3
420
411290
500 550 600 650 700 750 800
Abs
orba
nce
/ a.u
.
/ nm
655
668
UV-vis absorption: the colour
Eu-ARTECHEu-ARTECH
Normalized emission spectra of weld lakes (exc:366 nm)
450 500 550 600 650 700 750 800
675663
E
mis
sion
Int
ensi
ty /
a.u.
/ nm
Lake type 1 (Int / 1) Lake type 2 (Int / 1.2) Lake type 3 (Int / 3.4)
525 550
UV-vis fluorescence: the lake
Eu-ARTECHEu-ARTECH 3D UV-vis fluorescence: the lake
Exc. 250-400 nm
Eu-ARTECHEu-ARTECH
500 600 700 800
0
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
545.0
7 , 1
73.5
39
39
0
Wavelength (nm)
250.00
275.00
300.00
325.00
350.00
375.00
450.00 500.00 550.00 600.00 650.00 700.00 750.00 800.00
167.11
154.31
141.50
128.70
115.89
103.09
90.29
77.48
64.68
51.87
39.07
26.27
13.46
0.66
weld1
500 600 700 800
0
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
547.
01 ,
141.
344
39
0
Wavelength (nm)
250.00
275.00
300.00
325.00
350.00
375.00
450.00 500.00 550.00 600.00 650.00 700.00 750.00 800.00
136.19
125.90
115.61
105.32
95.03
84.74
74.45
64.16
53.86
43.57
33.28
22.99
12.70
2.41
weld2
500 600 700 8000
200
400
600
800
1000
Wavelength (nm)
Inte
nsity
(a.
u.)
524.
02 ,
584.
351
39
0
Wavelength (nm)
250.00
275.00
300.00
325.00
350.00
375.00
450.00 500.00 550.00 600.00 650.00 700.00 750.00 800.00
562.76
519.78
476.79
433.80
390.81
347.83
304.84
261.85
218.86
175.88
132.89
89.90
46.92
3.93
weld3
550
525
3D UV-vis fluorescence: the lake
Eu-ARTECHEu-ARTECH
400 500 600 7000
200
Excitation spectra of weld lake 1 and 3 (Varian)
Em
issi
on I
nten
sity
/ a.
u.
/ nm
lake 1 em
= 720 nm lake 3 em= 720 nm
666
UV-vis fluorescence: the lake
Eu-ARTECHEu-ARTECH
mordant max abs max
fluo
Weld lake 1 CO3--
KAl(SO4)2
420 (655) 550 (663)
Weld lake 2 KAl(SO4)2
CO3--
411 (668) 550 (675)
Weld lake 3 Ca & K 411 525Complex luteolin:Al max
fluo = 540 nm Complex apigenin:Al max fluo = 523 nm
Complex luteolin:Mg max fluo = 520 nm
O.S. Wolfbeis et al. Z. Naturforsc 39b, 231-237, 1983
Summary
Eu-ARTECHEu-ARTECH
1. textiles
Eu-ARTECHEu-ARTECH
Sulphur Potassium Calcium
Untreated silk
Mordanted silk
Dyed silk - 1
Dyed silk - 2
XRF: the mordant
Eu-ARTECHEu-ARTECH
Sulphur Potassium Calcium
Untreated wool
Washed wool
Mordanted wool
Dyed wool - 1
Dyed wool - 2
XRF: the mordant
Eu-ARTECHEu-ARTECH
0 1000 2000 3000 4000 5000 6000 7000
0.4
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
silk wool
log(
1/R
)
wavenumber (cm-1)
mid FTIR: the textile
Eu-ARTECHEu-ARTECH
200 300 400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
1.2
A
bsor
banc
e / a
.u.
/ nm
1: untreated silk 4: mordanted silk 8: dyed silk (bath 3) 9: dyed silk (bath 4)
Absorption spectra of silk
332
373 408
666
UV-vis absorption: the colour
Eu-ARTECHEu-ARTECH
200 300 400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
A
bsor
banc
e / a
.u.
/ nm
2: untreated wool 3: washed wool 5: mortanted wool 6: dyed wool (dye bath 1) 7: dyed wool (dye bath 2)
665
385430
Absorption spectra of wool samples
UV-vis absorption: the colour
Eu-ARTECHEu-ARTECH
400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
inte
nsit
y
wavenumber (cm-1)
exc
: 280 nm
exc: 390 nm
519 536
675
720
Normalized emission spectra of dyed silk (sample 8) at different excitation wavelenghth
UV-vis fluorescence: wavelenght effect (bath 4)
Eu-ARTECHEu-ARTECHUV-vis fluorescence: dyed Silk bath effect
450 500 550 600 650 700 750 8000.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
720
535
inte
nsity
(a.
u.)
wavelenght (nm)
bath 3 bath 4
Emission spectra of dyed silk (exc
: 390 nm)
675
507
Eu-ARTECHEu-ARTECH3D UV-vis fluorescence: dyed Silk
500 600 700 800
20
40
60
80
100
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
140
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
140
Wavelength (nm)
T
500 600 700 800
50
100
150
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
140
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
140
Wavelength (nm)
T
500 600 700 800
20
40
60
80
100
120
140
Wavelength (nm)
T
500 600 700 800
50
100
150
Wavelength (nm)
T
500 600 700 800
50
100
150
Wavelength (nm)
T
39
0
Wavelength (nm)
266.20
290.40
314.60
338.80
363.00
387.20
438.640 466.055 493.470 520.885 548.300 575.715 603.130 630.545 657.960 685.375 712.790 740.205 767.620 795.035
162.32
150.17
138.01
125.85
113.69
101.53
89.37
77.21
65.05
52.89
40.73
28.58
16.42
4.26
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
70
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
70
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
70
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
70
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
70
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
70
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
140
Wavelength (nm)
Inte
nsity
(a.
u.)
39
0
Wavelength (nm)
260.00
270.00
280.00
290.00
300.00
310.00
320.00
330.00
340.00
350.00
360.00
370.00
380.00
390.00
450.00 500.00 550.00 600.00 650.00 700.00 750.00 800.00
148.75
137.65
126.55
115.45
104.36
93.26
82.16
71.06
59.96
48.86
37.77
26.67
15.57
4.47
Bath 3
Bath 4
Eu-ARTECHEu-ARTECHUV-vis fluorescence: dyed wool bath 1
400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
Em
issi
on I
nten
sity
/ a.
u.
/ nm
exc: 280 nm exc: 366 nm exc: 390 nm
560550
675
Normalized emission spectra of dyed wool (sample 6) at different excitation wavelenghth
Eu-ARTECHEu-ARTECH
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
10
20
30
40
50
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
500 600 700 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
39
0
Wavelength (nm)
266.20
290.40
314.60
338.80
363.00
387.20
43 8 .64 0 46 6 .05 5 49 3 .47 0 52 0 .88 5 54 8 .30 0 57 5 .71 5 60 3 .13 0 63 0 .54 5 65 7 .96 0 68 5 .37 5 71 2 .79 0 74 0 .20 5 76 7 .62 0 79 5 .03 5
132.71
122.54
112.37
102.20
92.03
81.86
71.69
61.52
51.35
41.18
31.01
20.84
10.67
0.50
600 650 700 750 800
20
40
60
80
100
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
100
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
100
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
100
120
140
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
675.
00 ,
212.
811
55
0
Wavelength (nm)
363.00
387.20
411.40
435.60
459.80
484.00
508.20
532.40
556.60
603.130 630.545 657.960 685.375 712.790 740.205 767.620 795.035
225.46
208.24
191.01
173.79
156.56
139.34
122.11
104.89
87.66
70.43
53.21
35.98
18.76
1.53
dyed wool Bath 1
Exc. 250-390
Exc. 450-560
Eu-ARTECHEu-ARTECHUV-vis fluorescence: dyed wool bath 2
300 400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
E
mis
sion
Int
ensi
ty /
a.u.
/ nm
exc
: 280 nm
exc: 366 nm
exc
: 390 nm
Normalized emission spectra of dyed wool (sample 7) at different excitation wavelenghth
515
Eu-ARTECHEu-ARTECH
dyed wool bath 2
500 600 700 800
50
100
150
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
50
100
150
200
250
300
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
100
200
300
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
100
200
300
400
500
Wavelength (nm)In
tens
ity (
a.u.
)500 600 700 800
200
400
600
Wavelength (nm)In
tens
ity (
a.u.
)
39
0
Wavelength (nm)
260.00
270.00
280.00
290.00
300.00
310.00
320.00
330.00
340.00
350.00
360.00
370.00
380.00
390.00
450.00 500.00 550.00 600.00 650.00 700.00 750.00 800.00
742.84
685.93
629.01
572.10
515.18
458.27
401.35
344.44
287.52
230.61
173.69
116.78
59.87
2.95
600 650 700 750 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
100
120
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
20
40
60
80
100
120
140
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
50
100
150
200
250
300
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
500
600
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
1000
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
1000
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
1000
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
1000
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
500
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
100
200
300
400
Wavelength (nm)
Inte
nsity
(a.
u.)
600 650 700 750 800
200
400
600
800
1000
Wavelength (nm)
Inte
nsity
(a.
u.)
55
0
Wavelength (nm)
350.00
375.00
400.00
425.00
450.00
475.00
500.00
525.00
550.00
600.00 625.00 650.00 675.00 700.00 725.00 750.00 775.00 800.00
963.05
889.14
815.24
741.34
667.43
593.53
519.62
445.72
371.81
297.91
224.01
150.10
76.20
2.29
Exc. 250-390
Exc. 450-560
Eu-ARTECHEu-ARTECH
mordant max abs max
fluo
wool 1 Ca & K 430 (665) 550 (675)
wool 2 Ca 385 512 (675)
silk 3 Ca & K 408 (666) (536) 675 (720)
silk4 Ca 373 (507) 675 (720)
Summary
Eu-ARTECHEu-ARTECH
400 500 600 700 8000
2000
4000
Em
issi
on I
nten
sity
/ a.
u.
/ nm
Lake type 1 Lake type 2 Lake type 3
Emission spectra of weld lakes (exc:366 nm portable)
400 500 600 700 8000.0
0.2
0.4
0.6
0.8
1.0
Em
issi
on I
nten
sity
/ a.
u.
/ nm
Lake type 1 Lake type 2 Lake type 3 Lake type 1 p. Lake type 2 p. Lake type 3 p.
Normalized emission spectra of weld lakes (exc:366 nm Varian and portable)
UV-vis fluorescence: the lake
Eu-ARTECHEu-ARTECH
400 500 600 7000.0
0.2
0.4
0.6
0.8
1.0
Em
issi
on I
nten
sity
/ a.
u.
/ nm
2: untreated wool 3: washed wool 5: mordanted wool
Emission spectra of undyed wool (exc= 366 nm portable)
448
200 300 400 500 600 700 8000
2000
4000
6000
8000
10000
12000
Em
issi
on I
nten
sity
/ a.
u.
/ nm
Without cut With cut
Emission spectra of undyed silk (exc
= 366 nm portable)
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