•
13
•
2005 vol. 2
For individual solutions of
tert
-amyl methyl ether,
tert
-butyl alcohol, ethyl-
tert
-butyl ether, and 1,1,2-trichlorotrifluoroethane (Freon® 113), and for
internal and surrogate standards, please see our catalog, or visit our
website.
References
1. Butler J.C., E. Phillips, and M. Conoley Application Note AN9197,
Thermo Electron Corporation, 2215 Grand Avenue Parkway, Austin,
TX., 2003.
2. A.L. Hilling and G. Smith, Environmental Testing & Analysis, 10 (3),15-
19, 2001.
Purge and Trap Conditions:
Concentrator:
Tekmar LSC-3100 purge and trap
Trap:
Vocarb 3000 (type K)
Purge:
11 min. @ 40 mL/min. @ ambient temperature.
Dry purge:
1 min. @ 40mL/min. (MCS bypassed using Silcosteel
®
tubing)
Desorb preheat:
245°C
Desorb:
250°C for 2 min., flow 10mL/min.
Bake:
260°C for 8 min.
Interface:
Silcosteel
®
transfer line
1:30 split at injection port. 1mm ID split injection sleeve (cat.# 20972).
Column:
Rtx
®
-VMS, 30m, 0.25mm ID, 1.4µm (cat.# 19915)
Sample:
502.2 Calibration Mix #1 (cat.# 30042)
Drinking Water VOA MegaMix
™
, 524.2 Rev 4 (cat.# 30601)
524 Internal Standard/Surrogate Mix (cat.# 30201)
Ketone Mix, EPA Method 524.2 Rev 4.1 (cat.# 30602)
Compounds at 20 ppb each in 5mL RO water
(ketones at 50ppb; internal standards at 40ppb)
Inj. temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
1.1mL/min.
Dead time:
1.48 min. @ 40°C
Oven temp.:
40°C (hold 2 min.) to 85°C @ 14°C/min. (hold 2 min.)
to 220°C @ 30°C/min. (hold 4 min.).
Det:
Agilent 5971A GC/MS
Transfer line temp.: 280°C
Scan range:
35-300 amu
Tune
PFTBA/BFB
Ionization:
EI
GC_EV00718
Figure 1
12-minute analysis of 84 volatile compounds, using a
short, narrow bore Rtx®-VMS column.
A 30m, 0.25mm ID, 1.4µm Rtx®-VMS capillary
column (cat.# 19915) is an excellent choice for
analyzing the 84 target compounds (Figure 1).
This narrow bore column improves resolution of
traditionally coeluting compounds, such as carbon
tetrachloride / 1,1,1-trichloroethane, while short-
ening the analysis time. Analysis time is less than
12 minutes, and the cycle time is 16 minutes,
which is well below the cycle time of a standard
purge and trap system. This allows the fastest run-
time attainable using a Tekmar 3100 purge and
trap unit coupled to a single GC. A slower initial
temperature ramp rate makes additional resolu-
tion possible.
We recommend using the 30m, 0.25mm ID col-
umn for best resolution of the target gases. At
20ppb in 5mL water, the gases are better than 90%
resolved, using an initial temperature of 40°C
(Figure 1). We encourage laboratories using either
dual purge and trap technology or newer purge
and trap systems with rapid cycle times to use a
20m, 0.18mm ID, 1.0µm Rtx®-VMS column for
sub-10 minute runtimes.
1,2
Whatever your system
for analyzing volatiles, we offer the columns, ana-
lytical standards, GC accessories, and technical
knowledge to get your laboratory running these
analyses quickly and accurately.
Rtx®-VMS (fused silica)
ID df (µm)
temp. limits
length cat. #
price
0.18mm 1.00 -40 to 240/260°C 20-Meter 49914
$385
0.25mm 1.40 -40 to 240/260°C 30-Meter 19915
$445
DrinkingWater VOA MegaMix™, 524.2 Rev. 4.1
(73 components—see Table 1)
2,000µg/mL each in P&T methanol, 1mL/ampul
cat. # 30601 (ea.)
$135
acetone
2-butanone (MEK)
1,1-dichloro-2-propanone
2-hexanone
4-methyl-2-pentanone (MIBK)
Ketones Mix, 524.2 Rev. 4.1
(5 components)
5,000µg/mL each in 90% P&T methanol:10% water, 1mL/ampul
cat. # 30602 (ea.)
$30
bromomethane
chloroethane
chloromethane
dichlorodifluoromethane
trichlorofluoromethane
vinyl chloride
502.2 Calibration Mix #1 (gases)
200µg/mL each in P&T methanol, 1mL/ampul
cat. # 30439 (ea.)
$24
2,000µg/mL each in P&T methanol, 1mL/ampul
cat. # 30042 (ea.)
$35
1. dichlorodifluoromethane
2. chloromethane
3. vinyl chloride
4. bromomethane
5. chloroethane
6. trichlorofluoromethane
7. diethyl ether
8. 1,1-dichloroethene
9. carbon disulfide
10. iodomethane
11. allyl chloride
12. methylene chloride
13. acetone
14.
trans
-1,2-dichloroethene
15. methyl
tert
-butyl ether
16. 1,1-dichloroethane
17. acrylonitrile
18.
cis
-1,2-dichloroethene
19. 2,2-dichloropropane
20. bromochloromethane
21. chloroform
22. methyl acrylate
23. carbon tetrachloride
24. tetrahydrofuran
25. 1,1,1-trichloroethane
26. 2-butanone
27. 1,1-dichloropropene
28. 1-chlorobutane
29. propionitrile
30. methacrylonitrile
31. benzene
32. 1,2-dichloroethane
33. fluorobenzene (IS)
34. trichloroethene
35. dibromomethane
36. 1,2-dichloropropane
37. bromodichloromethane
38. methyl methacrylate
39.
cis
-1,3-dichloropropene
40. toluene
41. chloroacetonitrile
42. 2-nitropropane
43. 1,1-dichloro-2-propanone
44. 4-methyl-2-pentanone
45. tetrachloroethene
46.
trans
-1,3-dichloropropene
47. 1,1,2-trichloroethane
48. ethyl methacrylate
49. dibromochloromethane
50. 1,3-dichloropropane
51. 1,2-dibromoethane
52. 2-hexanone
53. chlorobenzene
54. ethylbenzene
55. 1,1,1,2-tetrachloroethane
56.
m
-xylene
57.
p
-xylene
58.
o
-xylene
59. styrrene
60. bromoform
61. isopropylbenzene
62. 4-bromofluorobenzene (IS)
63. bromobenzene
64.
n
-propylbenzene
65. 1,1,2,2-tetrachloroethane
66. 2-chlorotoluene
67. 1,2,3-trichloropropane
68. 1,3,5-trimethylbenzene
69.
trans
-1,4-dichloro-2-butene
70. 4-chlorotoluene
71.
tert
-butylbenzene
72. pentachloroethane
73. 1,2,4-trimethylbenzene
74.
sec
-butylbenzene
75.
p
-isopropyltoluene
76. 1,3-dichlorobenzene
77. 1,4-dichlorobenzene
78.
n
-butylbenzene
79. hexachloroethane
80. 1,2-dichlorobenzene-d4 (IS)
81. 1,2-dichlorobenzene
82. 1,2-dibromo-3-chloropropane
83. nitrobenzene
84. hexachlorobutadiene
85. 1,2,4-trichlorobenzene
86. naphthalene
87. 1,2,3-trichlorobenzene
Table 1
Method 524.2 analytes and internal standards.
Peaks 1-6 are components of cat. # 30439
;
peaks 13,26,43,44,52 are components of
cat. # 30602
; all other analytes except IS are components of cat. # 30601.