georgia lethal injection drug test - triclinic labs report
DESCRIPTION
Georgia lethal injection drug test - Triclinic Labs ReportTRANSCRIPT
-
R201583.01 Page 2 of 13
Summary One pentobarbital powder sample and a syringe containing a solution with suspended solids provided by Georgia Department of Corrections were analyzed by x-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), and infrared (IR) spectroscopy. Information for the samples provided is listed in Table 1. Table 1. API Samples Provided
Sample Description Triclinic Sample
Number
Pentobarbital Sodium, CAS# 57-33-0, Purity 99.00%, Case # - II-2015-1214
TCL2758
Pentobarbital Sodium, 50mg/mL, Exp. 03/24/2015, Case # - II-2015-1214
TCL2759
Results The filenames for the data collected from the powder sample and the solids from the syringe are summarized in Table 2. The powder sample was able to be analyzed as received. The solids from the syringe were isolated by centrifuging the material, decanting the liquid, and allowing the material to air dry. Table 2. Analytical Testing Filenames
Triclinic Sample Number
XRPD Filename XRPD
Page No. DSC
Filename DSC Page
No. IR
Filename IR Page
No.
TCL2758 RX1-7453 6 DSC2.0911 9 IR782 11
TCL2759 RX1-7454 6 DSC2.0912 10 IR783 11
An overlay of the XRPD patterns for the powder sample and the solids from the syringe is displayed in Figure 1. The pattern for the powder sample provided shows a number of broad discrete diffraction peaks overlaid on a raised baseline, suggesting that this sample contains crystalline and non-crystalline material. The pattern for the solids isolated from the syringe showed a number of broad, discrete, diffraction peaks superimposed on a flat baseline, indicating that this sample is crystalline. Visual comparison of the patterns showed that there were some similar peaks between the patterns, but a number of unique peaks were also observed in the patterns. In order to determine the identity of the materials in the samples, a database search/match analysis was performed. Figure 2 shows an overlay of the XRPD pattern for the powder sample with the database stick patterns for one solid form of pentobarbital sodium, one solid form of pentobarbital, and sodium chloride [1]. These three stick patterns describe all but two broad, low-intensity, high-angle reflections observed in the XRPD pattern for the powder sample. This would suggest that these three components comprise the majority of the sample. Figure 3 shows an overlay of the XRPD pattern for the solids isolated from the syringe and the database stick patterns for two different solid forms of pentobarbital [2]. These two stick patterns
-
R201583.01 Page 3 of 13
describe all but four low-intensity high-angle reflections observed in the pattern for the solids isolated from the syringe. This would suggest that these two components comprise the majority of this sample. The results from the database search for the two patterns would suggest that the two samples contain one common form of pentobarbital, but that the other components comprising these samples are different. The powder sample appears to contain pentobarbital sodium as its other major component, while the solids isolated from the syringe contain another polymorph of pentobarbital as the other major component. This would indicate that the sodium salt of pentobarbital broke apart when preparing the solution in the syringe and polymorphs of the free base ultimately precipitated from the solution in this sample. The powder sample and the solids isolated from the syringe were also analyzed by DSC and the thermograms are presented in Figures 4 and 5, respectively. The DSC results are summarized in Table 3. Table 3. DSC Results
Triclinic Sample Number
DSC Filename
DSC Results a
TCL2758 DSC2.0911 Endos. at ~143 C (b), 220 C (b), 305 C (s), and 316 C (s)
TCL2759 DSC2.0912 Endos. at ~76 C (b), 140 C (b), and 246 C (b)
a. Endos. = endotherms; b = broad; s = sharp.
The thermograms for the two samples are quite different, with the only similarity being that there is an event between 140 and 145 C for both samples. This would suggest that the compositions of the two samples are largely different, but that there may be a common component. This is consistent with the XRPD findings which suggested that there was a common component between the samples, but other components were different. An overlay of the IR spectra for the two samples is presented in Figure 5. As with the XRPD and DSC data, there are similarities between the spectra for the two samples. A number of common bands are observed between the two spectra, but there are also regions that show significant differences. A library search was performed for the powder sample and a solid match was found to a library spectrum of pentobarbital sodium [3]. The spectrum for the solids isolated from the syringe contained a number of additional bands that were not observed in the library spectrum of the pentobarbital sodium. No suitable matches were found that described these additional spectral bands.
-
R201583.01 Page 4 of 13
Conclusions Based on the analyses performed in this study, the powder sample is believed to contain pentobarbital sodium, a polymorph of pentobarbital free base, and sodium chloride. The solids isolated from the syringe are believed to contain two different polymorphs of pentobarbital free base.
Experimental XRPD The Rigaku Smart-Lab X-ray diffraction system was configured for reflection Bragg-Brentano geometry using a line source X-ray beam. The x-ray source is a Cu Long Fine Focus tube that was operated at 40 kV and 44 mA. That source provides an incident beam profile at the sample that changes from a narrow line at high angles to a broad rectangle at low angles. Beam conditioning slits are used on the line X-ray source to ensure that the maximum beam size is less than 10 mm both along the line and normal to the line. The Bragg-Brentano geometry is a para-focusing geometry controlled by passive divergence and receiving slits with the sample itself acting as the focusing component for the optics. The inherent resolution of Bragg-Brentano geometry is governed in part by the diffractometer radius and the width of the receiving slit used. Typically, the Rigaku Smart-Lab is operated to give peak widths of 0.1 2 or less. The axial divergence of the X-ray beam is controlled by 5.0-degree Soller slits in both the incident and diffracted beam paths. The powder samples were prepared in a low background Si holder using light manual pressure to keep the sample surfaces flat and level with the reference surface of the sample holder. The single crystal Si low background holder has a small circular recess (7 mm diameter and about 1 mm depth) that holds between 15 and 25 mg of powdered material. Each sample was analyzed from 2 to 40 2 using a continuous scan of 6 2 per minute with an effective step size of 0.02 2. DSC DSC analyses were performed using a TA Instruments Q2000 differential scanning calorimeter equipped with a refrigerated cooling system (RCS). Approximately 3 to 4 mg of each sample was weighted into an aluminum Tzero pan, covered with and aluminum Tzero lid, and crimped. The sample cell was heated from ambient to 350 C at a rate of 10 C/minute. An empty reference pan prepared in the same way was also present in the cell to account for the heat flow properties of the pan. The DSC instrument is controlled using the Thermal Advantage Release 5.2.5. Infrared Spectroscopy IR The IR spectra were acquired utilizing a Thermo Nicolet model 6700 Fourier-transform (FT)-IR spectrophotometer equipped with a deuterated triglycine sulfate (DTGS) detector, a potassium bromide (KBr) beamsplitter, and an electronically temperature controlled (ETC) Ever-Glo IR source. The spectra were acquired using a SMART iTR diamond attenuated total reflectance (ATR) sampling accessory with a spectral range of
-
R201583.01 Page 5 of 13
4000-525 cm-1. Each spectrum is the result of 128 co-added scans acquired at 2 cm-1 resolution. A single beam background scan of the air was acquired before the sample scan allowing presentation of the spectrum in Log 1/R units. A wavelength calibration was performed using polystyrene. (The Omnic 8.2 software package (Thermo-Nicolet) was used to acquire, process, and evaluate the spectral data.)
References
1. International Centre for Diffraction Data PDF-4 2015 Organics Database, downloaded and interfaced with Rigaku PDXL software at Triclinic Labs, card numbers 00-029-1920 and 00-027-1597.
2. International Centre for Diffraction Data PDF-4 2015 Organics Database, downloaded and interfaced with Rigaku PDXL software at Triclinic Labs, card numbers 00-028-1648.
3. Sigma Biological Sample Library, Sample Index #9, Copyright 2008 Thermo Fisher Scientific Inc.
-
R201583.01 Page 6 of 13
Figure 1. Overlay of XRPD patterns for the pentobarbital powder sample and the solids isolated from the syringe.
-
R201583.01 Page 7 of 13
Figure 2. Overlay of the XRPD pattern for the powder sample with the database patterns for pentobartbital sodium.
Qualitative Analysis Results General information Analysis date 2015/04/02 11:57:22 Sample name Measurement date 2015/03/27 09:46:36 File name RX1-7453_Theta_2-
Theta.TXT Operator
Comment
Qualitative analysis results
Phase name Formula Figure of merit Phase reg. detail DB card number
sodium 5-ethyl-5-(1-methylbutyl) barbiturate
C11 H17 N2 Na O3 1.161 ICDD (PDF-4 Organics 2015 RDB)
00-029-1920
5-ethyl-5-(1-methylbutyl)-1,3-diazinane-2,4,6-trione, 5-ethyl-5-(1-methylbutyl)barbituric acid
C11 H18 N2 O3 1.833 ICDD (PDF-4 Organics 2015 RDB)
00-027-1597
NaCl Cl Na 2.282 User (COD3) 150357
Phase data pattern
Inte
nsity (
cps)
0.0e+000
2.0e+003
4.0e+003
6.0e+003
8.0e+003
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 14
.100
0, 6
.263
4
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 12
.000
0, 7
.360
9so
dium
5-e
thyl
-5-(
1-m
ethy
lbut
yl) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 11
.100
0, 7
.958
6so
dium
5-e
thyl
-5-(
1-m
ethy
lbut
yl) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 9.
9900
, 8.8
446
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 8.
9800
, 9.8
417
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 8.
5300
, 10.
3622
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 7.
8500
, 11.
2626
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 6.
9900
, 12.
6537
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 6.
6500
, 13.
3035
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 6.
3500
, 13.
9350
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 5.
9800
, 14.
8019
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 5.
5500
, 15.
9559
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 4.
9800
, 17.
7962
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 4.
6700
, 18.
9882
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 4.
4400
, 19.
9816
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 3.
8600
, 23.
0223
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 3.
5600
, 24.
9925
sodi
um 5
-eth
yl-5
-(1-
met
hylb
utyl
) ba
rbitur
ate,
C11
H17
N2
Na
O3,
, 3.
3600
, 26.
5064
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
7.05
00, 1
2.54
55
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
6.21
00, 1
4.25
085-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
6.01
00, 1
4.72
76
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
5.12
00, 1
7.30
585-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
4.94
00, 1
7.94
15
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.62
00, 1
9.19
56
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.30
00, 2
0.63
92
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.00
00, 2
2.20
61
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
3.48
00, 2
5.57
66
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
3.32
00, 2
6.83
17
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
3.14
00, 2
8.40
125-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.09
00, 2
8.87
065-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.01
00, 2
9.65
535-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
2.92
00, 3
0.59
135-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
2.85
60, 3
1.29
42
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
2.62
00, 3
4.19
59
NaC
l, C
l Na,
(1
1 1)
, 3.2
620,
27.
3179
NaC
l, C
l Na,
(2
0 0)
, 2.8
250,
31.
6468
NaC
l, C
l Na,
(1
1 1)
, 3.2
620,
27.
3179
NaC
l, C
l Na,
(2
0 0)
, 2.8
250,
31.
6468
2-theta (deg)
10 20 30 40
sodium 5-ethyl-5-(1-methylbutyl) barbiturate, C11 H17 N2 Na O3, 00-029-19205-ethyl-5-(1-methylbutyl)-1,3-diazinane-2,4,6-trione, 5-ethyl-5-(1-methylbutyl)barbituric acid, C11 H18 N2 O3, 00-027-1597
NaCl, Cl Na, 150357
-
R201583.01 Page 8 of 13
Figure 3. Overlay of the XRPD pattern for the solids isolated from the syringe with the database patterns for two polymorphs of pentobarbital.
Qualitative Analysis Results General information Analysis date 2015/04/02 12:14:47 Sample name Measurement date 2015/03/27 09:46:36 File name RX1-7454_Theta_2-
Theta.TXT Operator
Comment
Qualitative analysis results
Phase name Formula Figure of merit Phase reg. detail DB card number
5-ethyl-5-(1-methylbutyl)-1,3-diazinane-2,4,6-trione, 5-ethyl-5-(1-methylbutyl)barbituric acid
C11 H18 N2 O3 1.253 ICDD (PDF-4 Organics 2015 RDB)
00-027-1597
5-ethyl-5-(1-methylbutyl)barbituric acid
C11 H18 N2 O3 1.468 ICDD (PDF-4 Organics 2015 RDB)
00-028-1648
Phase data pattern
Inte
nsity (
cps)
0.0e+000
5.0e+003
1.0e+004
1.5e+004
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
7.05
00, 1
2.54
55
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
6.21
00, 1
4.25
085-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
6.01
00, 1
4.72
76
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
5.12
00, 1
7.30
585-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
4.94
00, 1
7.94
15
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.62
00, 1
9.19
56
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.30
00, 2
0.63
92
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.00
00, 2
2.20
61
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
3.48
00, 2
5.57
66
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
3.32
00, 2
6.83
17
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
3.14
00, 2
8.40
125-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.09
00, 2
8.87
065-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.01
00, 2
9.65
535-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
2.92
00, 3
0.59
135-
ethy
l-5-
(1-m
ethy
lbut
yl)-
1,3-
diaz
inan
e-2,
4,6-
trio
ne, 5
-eth
yl-5
-(1-
met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
2.85
60, 3
1.29
42
5-et
hyl-
5-(1
-met
hylb
utyl
)-1,
3-di
azin
ane-
2,4,
6-tr
ione
, 5-e
thyl
-5-(
1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
2.62
00, 3
4.19
59
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
13.8
000,
6.3
997
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
6.21
00, 1
4.25
085-
ethy
l-5-
(1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
6.07
00, 1
4.58
12
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
5.07
00, 1
7.47
785-
ethy
l-5-
(1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
4.92
00, 1
8.01
51
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
4.66
00, 1
9.02
93
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
4.29
00, 2
0.68
78
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.95
00, 2
2.49
08
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.74
00, 2
3.77
16
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
3.28
00, 2
7.16
51
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
2.94
00, 3
0.37
825-
ethy
l-5-
(1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
2.86
50, 3
1.19
34
5-et
hyl-
5-(1
-met
hylb
utyl
)bar
bitu
ric
acid
, C
11 H
18 N
2 O
3, ,
2.63
50, 3
3.99
535-
ethy
l-5-
(1-m
ethy
lbut
yl)b
arbi
turic
acid
, C
11 H
18 N
2 O
3, ,
2.62
00, 3
4.19
59
2-theta (deg)
10 20 30 40
5-ethyl-5-(1-methylbutyl)-1,3-diazinane-2,4,6-trione, 5-ethyl-5-(1-methylbutyl)barbituric acid, C11 H18 N2 O3, 00-027-15975-ethyl-5-(1-methylbutyl)barbituric acid, C11 H18 N2 O3, 00-028-1648
-
R201583.01 Page 9 of 13
Figure 4. DSC thermogram for pentobarbital powder sample.
143.16C 219.70C
305.09C
316.18C
-4
-3
-2
-1
0
He
at
Flo
w (
W/g
)
0 50 100 150 200 250 300 350
Temperature (C)
Sample: TCL2757Size: 2.4250 mgMethod: Ramp
DSCFile: T:...\2015051\Data\DSC\DSC2.0911Operator: TLCRun Date: 26-Mar-2015 15:58Instrument: DSC Q2000 V24.11 Build 124
Exo Up Universal V4.5A TA Instruments
-
R201583.01 Page 10 of 13
Figure 5. DSC thermogram for solids isolated from the syringe.
76.13C
139.58C
245.95C
-2.0
-1.5
-1.0
-0.5
0.0
0.5
He
at
Flo
w (
W/g
)
0 50 100 150 200 250 300 350
Temperature (C)
Sample: 304-32-2Size: 5.6540 mgMethod: Ramp
DSCFile: T:...\2015051\Data\DSC\DSC2.0912Operator: TLCRun Date: 26-Mar-2015 16:38Instrument: DSC Q2000 V24.11 Build 124
Exo Up Universal V4.5A TA Instruments
-
R201583.01 Page 11 of 13
Figure 6. Overlay of the IR spectra for pentobarbital powder sample and the solids isolated from the syringe.
-
R201583.01 Page 12 of 13
Figure 7. Overlay of the IR spectrum of the pentobarbital powder sample and a library spectrum for pentobarbital sodium.
-
R201583.01 Page 13 of 13
Figure 8. Overlay of the IR spectrum of the pentobarbital powder sample, the solids isolated from the syringe, and a library spectrum for pentobarbital sodium.
Signature: Unable to v erif y digital signature. The data has been changed.
TCL2757; Pentobarbital
0.00
0.10
0.20
0.30
0.40
0.50
Lo
g
Signature: Unable to v erif y digital signature. The data has been changed.
#304-32-2; Pentobarbital (f rom TCL2758)
0.2
0.4
0.6
0.8
Lo
g
Signature: Not signed
PENTOBARBITAL SODIUM--DEA SCHEDUL
0.2
0.4
0.6
0.8
1.0
Ab
s
1000 1500 2000 2500 3000 3500
Wav enumbers (cm-1)