ADV01-05_1-298

42702

-60 to 330/350°C

0.18

0.18mm

temp. limits

df (µm)

• 3 •

www.restekcorp.com

800-356-1688

w/ data pack

w/data pack

Rtx®-5Sil MS Columns (fused silica)

(Selectivity equivalent to Crossbond

5% diphenyl / 95% dimethyl polysiloxane)

8270 MegaMix™

(76 components)

1,000µg/mL each (3-methylphenol and 4-methylphenol at

500µg/mL each) in methylene chloride:benzene (75:25),

1mL/ampul

Each

5-pk.

10-pk.

31686

31686-510

—

w/data pack

31686-500

31686-520

31786

acenaphthene-d10

chrysene-d12

1,4-dichlorobenzene-d4

naphthalene-d8

perylene-d12

phenanthrene-d10

SV Internal Standard Mix

Each

5-pk.

10-pk.

2,000µg/mL each in methylene chloride, 1mL/ampul

31206

31206-510

—

31206-500

31206-520

31306

4,000µg/mL each in methylene chloride, 1mL/ampul

31006

31006-510

—

31006-500

31006-520

31106

2-fluorobiphenyl

nitrobenzene-d5

-terphenyl-d14

B/N Surrogate Mix (4/89 SOW)

2-fluorophenol

phenol-d6

2,4,6-tribromophenol

Acid Surrogate Mix (4/89 SOW)

compounds, plus benzoic acid, benzidine, and sur-

rogate and internal standards, on our new 20m,

0.18mm ID, 0.18µm Rtx

-5Sil MS column (cat.#

42702). The Rtx

-5Sil MS stationary phase is based

on a silarylene polymer specifically designed for the

demanding GC/MS analysis of semivolatile com-

pounds, and the column exhibits lower bleed than

columns prepared from phenyl/methyl polymers. All

target compounds can be quantified with greater

sensitivity. The thin phase film in this column allows

superior resolution of structural isomers

benzo(b)fluoranthene and benzo(k)fluoranthene

(peaks 83 and 84), while achieving a very short

analysis time of less than15 minutes. Peak shape and

response are excellent, even for active compounds

such as 2,4-dinitrophenol and pentachlorophenol

(peaks 50 and 66). Optimizing the temperature pro-

gram, as well as the physical dimensions of the col-

umn, contributes to better resolution of closely elut-

ing peaks and shortens the analysis time.

In order to achieve the separation shown in Figure

1, care must be taken to optimize injection condi-

tions. To reduce solvent effects that could interfere

with N-nitrosodimethylamine and pyridine (peaks 1

and 2), we chose a splitless inlet liner, rather than a

direct injection liner (e.g., a Uniliner

). A cyclo dou-

ble gooseneck design enables the sample to be com-

pletely volatilized in the injection port prior to con-

densing at the column inlet, and ensures more

reproducible results, relative to a standard (straight)

liner. The 2mm internal diameter provides the best

results with 0.5µL injections. The splitless hold time

also is very important: a change of only several sec-

onds can reduce sensitivity by 50%. We discovered

that a pulsed splitless analysis, using a 0.20 min.

pulse 5psi higher than the column flow backpres-

sure, dramatically improves sample transfer onto the

column. Making the pulse 3 seconds (0.05 min.)

longer than the splitless hold time (0.15 min.)

allows excess solvent to be swept away quickly. The

270ºC injection port temperature vaporizes the

Each

5-pk.

10-pk.

1,000µg/mL each in methylene chloride, 1mL/ampul

31024

31024-510

—

w/ data pack

31024-500

31024-520

31124

5,000µg/mL each in methylene chloride, 1mL/ampul

31062

31062-510

—

w/ data pack

31062-500

31062-520

31162

5,000µg/mL each in methylene chloride, 5mL/ampul

31086

31086-510

—

w/ data pack

31086-500

31086-520

31186

w/ data pack

Each

5-pk.

10-pk.

2,000µg/mL each in methanol, 1mL/ampul

31025

31025-510

—

w/ data pack

31025-500

31025-520

31125

10,000µg/mL each in methanol, 1mL/ampul

31063

31063-510

—

w/ data pack

31063-500

31063-520

31163

10,000µg/mL each in methanol, 5mL/ampul

31087

31087-510

—

31087-500

31087-520

31187

sample with minimal analyte breakdown. GC condi-

tions were adjusted to resolve analytes that coelute

and share ions. Aniline and phenol (peaks 4 and 6),

for example, were resolved by using an initial tem-

perature ramp rate of 14ºC/min., and the key to

resolving isomers benzo(b)fluoranthene and

benzo(k)fluoranthene (peaks 83 and 84) is to be

sure that they elute during the temperature ramp

portion of the program. If the isomers elute during

the final hold time they will not be well resolved. By

using a 0.18mm ID Rtx

-5Sil MS column under

these conditions, you will ensure a rapid and suc-

cessful analysis of the 8270 compounds.

To meet the substantial demand for reference mate-

rials for Method 8270, we offer 8270 MegaMix

™

ref-

erence mix (cat.# 31686)—a formulation of 76 tar-

get compounds in methylene chloride/benzene

(75:25).

continued on page 5

df (µm)

temp. limits

15-Meter

30-Meter

0.25mm

0.25

-60 to 330/350°C

12720

12723

0.50

-60 to 330/350°C

12735

12738

1.00

-60 to 325/350°C

12750

12753

0.28mm

0.25

-60 to 330/350°C

12790

12793

0.50

-60 to 330/350°C

12791

12794

1.00

-60 to 325/350°C

12792

12795

0.32mm

0.25

-60 to 330/350°C

12721

12724

0.50

-60 to 330/350°C

12736

12739

1.00

-60 to 325/350°C

12751

12754

Components listed in

bold

in Figure 1.

Benzidine

1,000µg/mL in methanol, 1mL/ampul

Each

5-pk.

10-pk.

31441

31441-510

—

w/data pack

31441-500

31441-520

31541

Benzoic Acid

1,000µg/mL in methanol, 1mL/ampul

Each

5-pk.

10-pk.

31415

31415-510

—

w/data pack

31415-500

31415-520

31515

2,4-Dinitrophenol

1,000µg/mL in methanol, 1mL/ampul

Each

5-pk.

10-pk.

31291

31291-510

—

w/data pack

31291-500

31291-520

31391

Rtx

-5Sil MS 20m, 0.18mm ID, 0.18µm (cat.# 42702)

Sample:

US EPA Method 8270D mix: 8270 MegaMix

™

(cat.# 31686), benzoic acid (cat.# 31415), benzidine (cat.# 31441),

2,4-dinitrophenol (cat.# 31291)*, Acid Surrogate Mix (4/89 SOW) (cat.# 31063),

B/N Surrogate Mix (4/89 SOW) (cat.# 31062), SV Internal Standard Mix (cat.# 31206)

*2,4-dinitrophenol also is a component of the MegaMix

™

Inj.:

0.5µL, 5ppm each component (2.5ng on column) (2,4-dinitrophenol at 10ppm/5ng on column; 3-methylphenol and

4-methylphenol at 2.5ppm/1.25ng on column), splitless (hold 0.15 min., pressure pulse 0.20 min. @ 30psi),

2mm cyclo double gooseneck inlet liner (cat.# 20907); Agilent 6890

Inj. temp.:

270°C

Carrier gas:

helium, constant flow

Flow rate:

1.2mL/min.

Oven temp.:

40°C (hold 0.5 min.) to 90°C @ 14°C/min., to 330°C @ 22°C/min. (hold 1 min.)

Det.:

Agilent 5973 GC/MS

Transfer line

temp.:

280°C

Scan range:

35-550 amu

Solvent Delay:

1 min.

Tune:

DFTPP

Ionization:

20-Meter

Use this new column for

sub-15 minute analysis of

78 Method 8270D target

compounds.