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7697A USP

Roger L. Firor

2850 Centerville Rd

Wilmington, DE 19808-1610

USA

7697A 7890 GC UPS 1

2 1 2A 2B RSD% 2.5%

/ 10 mL

20 mL

FID-FID FID-MSD

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2

1 2A 2B

250mL 500mL Brand 6mL 10mL 20mL

Teflon

1 5190-0490

2A 5190-0492

2B 5190-0513

7697A 0.45mm (Restek Siltek

10018) /

2mm SilTite VI

30

0.32mm

7697A (PCM)

EPC 7890

1ml

PCM (NTP)

1 1

(QA) (USP) [1]

/

ICH Q3C

(API)

GC USP

USP USP

GC

USP 1 2

1. A

2. B

3. C

A G43 624 VF-

624ms DB-624 123-1334 B

G16 HP-INNOWax 9091N-113

624 RSD FID (624

NNOWax ) FID/MSD

USP 467

7697A

USP A 7697A 7890

GC //

2mm 5181-

88180 4mm 2103003

FID

VI

/ EPC624

7697A

1.

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3

7697A 13

1.

2. 3.

4.

5.

6.

7.

8.

9.

10.

11.

12.

13.

EPC

EPC

7697A

2 3

/ 140 C 5:1

145 C 5:1

EPC EPC

0.45 mm

p/n CP9104 30 m 0.32 mm 1.80 m VF-624 ms

40 C (5 min) 240 C (2 min)18 C/min

85 C

/ 85 C

100 C

10 mL 20 mL

1 mL 1 mL

40 min 40 min

0.5 min 0.5 min

15 psia (NTP) 15 psia (NTP)

0 10 psia (NTP)

0.10 min 0.10 min

0.05 min 0.05 min

50 mL/min 50 mL/min

20 psi/min 20 psi/min

2 2

1.

PS1

GC

PCM

6

MFS

/

PV1

PV2

PV

OFF

SV1

ON

3

1

2

4

5

6

2. PCM EPC 6 (SV1) GC EPC 6GC

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4

3. PS1PV2 PCM EPC2

PCM

MFS

PV1

PV2

PV

SV1

ON

OFF

PS1

/

3

1

2

4

5

6

6

GC

ChemStation 7697A

4

4. 20 mL15psi (NTP) 20 psi/min 10 psi (NTP)

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5

2 1 2A 2B USP

RSD 20

10ml20ml /

10ml20ml

RSD 2.5%

(RSD) RSD

k USP

DMSODMACDMI

DMSO

RSD RSD

7697A

2.0 psi (NTP) 10.0 psi (NTP)

7697A

K 7697A

200 mL/min

5

VF-624 ms 1 1,2-

VI

10 mL 20 mL 10 mL 20 mL

1

1,1- 2.9 2.0 2.0 2.6

1,1,1- 2.7 2.2 1.9 3.9

3.8 4.4 3.1 3.4

3.9 2.3 1.5 3.1

1,2- 1.6 1.3 1.1 1.7

2A

1.0 0.6 1.3 0.4

1.0 0.5 1.3 0.6

1.2 1.9 1.5 2.3

-1,2 2.4 2.5 2.9 2.8

-1,2 1.5 2.1 1.8 2.8

0.8 0.6 1.4 0.7

3.5 2.9 4.2 2.9

4.1 3.9 4.3 3.2

1,4- 1.4 0.6 1.6 0.5

1.5 2.0 2.1 2.8

1.4 2.1 1.7 3.0

1.6 2.2 2.1 2.7

/ 1.6 2.2 2.0 2.9

1.4 2.2 1.8 3.1

2B

3.9 1.3 3.6 2.7 5.4 4.8 4.4 3.3

4.0 2.5 1.7 1.7

1,2- 1.7 1.6 4.2 4.5

5.9 2.5 2.1 1.6

1.7 0.8 1.5 0.9

2- 1.5 0.7 0.9 0.7

2.7 2.7 1.4 1.7

2. RSD

n = 20

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6

5. USP 46712A2BABC/20 mL

1. 1. 1,1,-2. 1,1,1-3. 4. 5. 1,2-

A

12

3

4

5

1. 2. 3. 4. -1,25. -1,26. 7. 8. 9. 1,4-10. 11. 12. 13. /14.

B

1 2

3

4

5

6

7

8

9

10

11

12

13

14

1.

2.

3.

4. 1,2-

5.

6.

7. 2-

8.

1

2

3

4

5

6

7 8C

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6 VF-624ms

INNOWax

1:1 30 m 0.32 mm 624 INNOWax UPS

A B SilTite

CFT

6

1 2A 2B 7 8 9

7:1 14psi40

40 5min 18/min 240

2min 10

INNOWax

FID

VI

/EPC

FID

624

7697A

6.

7. USP 4671

1. 1,1,-

2. 1,1,1-

3.

4.

5. 1,2-

1 2, 3 4

5

1

2

3

4

5

INNOWax

624

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8

8. USP 4672A

9. USP 4672B

1. 2.

3.

4. 1,2-

5.

6.

7. 2-

8.

INNOWax

624

1

2

3

4

5

6

7

8

1

2

3

4

5

6

7 8

1. 2. 3.

4.

-1,2

5. -1,26. 7. 8. 9. 1,4-10. 11. 12. 13. 14. 15.

1

2

3,64 5

7

8INNOWax

624

15

14

1112

13

9

10

1

2

3 4 5 6 7 8

9

10 11 15

12

13, 14

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9

USP 1 2 624

INNOWax

FID MS 5975C MSD

11 USP

MSD 60

3

10. 5:135 17min 20/min 2405min

624

1. 2. 1,1,-34. 5. -1,26. 7. -1,2, 8. 9. 10., , 1,1,1-

11. 12. 1,2-13. 1,2-14. 15. 16. 1,4-17. 18. 19. 2-20. 21. 22./23. 24.

INNOWax

1. 2.1,1 3. -1,2, THF, 1,1,1- 4. , 1,2 5. , 6. -1,2

, 7. 8. 9. 10. 1,4-11. 1,2-12. 2-13. 14.15.16. ()

17. 18. 19. 20.

Aux EPC not ready

Aux

3

[2]

MSD** FID

40 C 3.5 3.8 4.3 8.1 4.6

150 C 3.5 2.5 2.6 5.1 1.6

240 C 3.5 1.9 1.9 3.8 0.3 *

3. 10 (mL/min)

* Aux EPCnot ready

** 22017.1 cm MSD

INNOWax

624

2019

18

1713, 14, 15

16

12

11

10

9

8

76

5

4

1

2

3

1

2

4

3 5

6 7

810

11

12

13

14 15

1617

18 20, 21, 22, 2319

24

9

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FID MSD 1,4- 2-

MSD

SIM

Aux EPC FID

MSD

4.0 psig

14.7 psi

0 psi

+ Aux = F1 + F2

30 M 0.32 mm 1.80 6 24

Aux EPC

S/S

F1

F2

11. FID-MSD

FID= 80 cm x 0.20 mm

MSD= 137 cm x 0.18 mm

DB-62430 m x 0.32 mm x 1.80 m

12. 2AFID-MSD 20 mL

TIC

FID

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7697A

0.1

EPC

QA USP ICH

FID-MSD

SIM

1. USP 32-NF 27, General Chapter USP Organic

volatile impurities, United States Pharmacopeia.

Pharmacopoeia Convention Inc., Rockville, MD, 8/2009

2. www.agilent.com/chem/flowcalculatorGC

Pressure Flow Calculator Software Revision 2.05

3. Albert E Gudat and Roger L. Firor, Improved Retention

Time, Area Repeatability, and Sensitivity for Analysis ofResidual Solvents, 5989-6079CHCN

www.agilent.com/chem/cn

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www.agilent.com/chem

2011

2011 3 15

5990-7625CHCN