134 / 413
Successfully Implement the
Revised USP <467>Method
Continu ed from page 3.
Figure 3
USP residual solvent Class 2 Mixtu re A standard solut ion on an Rtx®-1301 column (G43).
2.acetonitrile (resolution
=
1.35) 3
3. dichloromethane
I
4.0
4.2
4.4
4.6
l. methanol
10. toluene
2. acetonitrile (resolution= 1.35) ll. chlorobenzene
3. dichloromethane
12. ethyl benzene
--¥sYSTEM SUITABILITYCRITERIAMET
....... ,1\.., ....
,_
9. 1,4-dioxane
9
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Ii
14.8 15.0 15.2
i
i
i
i
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I
15.4 156 15.8 16.0
10
20
GCPH00910
4. trans-l,2-dichloroethene
13.
m-xylene/p-xylene
5. cis-l,2-dichloroethene
14. o-xylene
6. tetrahydrofuran
7. cyclohexane
8. methylcyclohexane
9. l ,4-dioxane
Column:
Rtx"-624, 30m,0.32!D, l. 8IJm(caL# 10970)
13
12
n\
Sample:
USP < 467> Class 2 Mixture
A
standard solution (caL# 36271)
in 20mL headspace vial
Inj.:
headspaceinjection (split ratio 1:5),
l rnrn
split liner, Siltek" deactivated
(caL# 20972-214.1)
Inj. temp.:
140"C
Carrier gas:
helium,constantflow
Flow rate:
2.16mL/min., 35.3cm/sec.
Oven temp.:
40"Cfor 20min. to 240"C@
10"C/min. (holdfor 20min.)
Del.:
F!D @240"C
HeadspaceConditions
Instrument:
Tekmar HT3
Transfer line temp.:
lO5°C
Valve oven temp.:
105°C
Sample temp.:
80"C
Sample
equil,
time:
45min.
14
Vial pressure:
10psi
Pressurizetime:
0.5 min.
Loop fill pressure:
5psi
Loopfill time:
2.00min.
Inject time:
l. 00 min.
30min.
Figure 4
USP residual solvent Class 2 Mi xtu re B standard solution on an Rtx®-1301 column (G43).
5
7
3
--L
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8
i
1
4
I
10
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I
12
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i
14
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16
I
I
18
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20
I
6
I
22
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24
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26
8
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12
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3 4
I
10
i
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~
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20
I
6
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7
i
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30
I
I
min.
i
i
I
GCPH00911
l. hexane
2. nitromethane
3. chloroform
4. l,2-dimethoxyethane
5. trichloroethylene
6. pyridine
7. 2-hexanone
8. tetralin
Column:
Rtx"'624, 30m,0.32mm!D, l.8J1m(caL# 10970)
Sample:
USP < 467> Class 2 Mixture
B
standard solution (caL# 36280)
in 20mLheadspace vial
Inj.:
headspace injection (split ratio 1:5),
l rnrn
split
liner
Siltek"
deactivated(caL# 20972-214.1)
Inj. temp.:
140°C
Carier gas:
helium,constant flow
Flow rate:
2.16mLlmin., 35.3cm/sec.
Oven temp.:
40°Cfor 20 min. to 240"C@
10°C/ min. (hold for 20 min.)
Del.:
F!D@ 240"C
HeadspaceConditions
Instrument:
Tekmar HT3
Transfer line temp.:
105°C
Valve oven temp.:
105°C
Sample temp.:
80°C
Sample equil. time:
45 min.
Vial pressure:
lOpsi
Pressurizetime:
0.5 min.
Loopfill pressure:
5psi
Loop fill time:
2.00 min.
Inject time:
l.00 min.
I
i
Global RESTEKAdvantage
· 4·
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