analysis of semivolatile organic compounds

4
Introduction Semivolatile organic compounds (SVOCs) are molecules with intermediate volatility, making them abundant in both the vapor and condensed phase at ambient temperatures and pressures 1 . Certain compounds within the class of SVOCs are known to be environmental pollutants. Many government regulatory agencies have established methods and set performance criteria for the measurement SVOCs in a variety of environmental and industrial matrices. For example, United States Environmental Protection Agency (USEPA) method 8270D contains a list of 243 compounds that are suitable for analysis by gas chromatography coupled to mass spectrometry (GC/MS). Method 8270D contains detailed performance specifications necessary for the quantitative analysis of SVOCs. This Application Note demonstrates that the Agilent Intuvo 9000 GC can easily achieve the rigorous calibration specifications established in USEPA 8270D for the quantitative analysis of SVOCs in environmental matrices. ANALYSIS OF SEMIVOLATILE ORGANIC COMPOUNDS Technology Advantage: Agilent Intuvo 9000 GC with Agilent 5977 MSD For more information, visit: www.agilent.com/chem/intuvo

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Page 1: ANALYSIS OF SEMIVOLATILE ORGANIC COMPOUNDS

IntroductionSemivolatile organic compounds (SVOCs) are molecules with intermediate volatility,

making them abundant in both the vapor and condensed phase at ambient

temperatures and pressures1. Certain compounds within the class of SVOCs are

known to be environmental pollutants.

Many government regulatory agencies have established methods and set

performance criteria for the measurement SVOCs in a variety of environmental

and industrial matrices. For example, United States Environmental Protection

Agency (USEPA) method 8270D contains a list of 243 compounds that are suitable

for analysis by gas chromatography coupled to mass spectrometry (GC/MS).

Method 8270D contains detailed performance specifi cations necessary for the

quantitative analysis of SVOCs.

This Application Note demonstrates that the Agilent Intuvo 9000 GC can easily

achieve the rigorous calibration specifi cations established in USEPA 8270D for the

quantitative analysis of SVOCs in environmental matrices.

ANALYSIS OF SEMIVOLATILEORGANIC COMPOUNDS

Technology Advantage: Agilent Intuvo 9000 GC with

Agilent 5977 MSD

For more information, visit:

www.agilent.com/chem/intuvo

Page 2: ANALYSIS OF SEMIVOLATILE ORGANIC COMPOUNDS

ExperimentalInstrumentation

• Agilent Intuvo 9000 GC

• Agilent 5977 MSD with inert ion source with 6 mm and drawout plate

• Agilent DB-5ms UI, 30 m × 0.25 mm, 0.5 µm column

Sample preparation

A mixture of 77 target compounds comprised of acids, bases, neutrals, and six

internal standards were selected.

Standards were prepared in dichloromethane ranging in concentration from 0.1 to

100 µg/mL, and internal standards at a concentration of 40 µg/mL.

Results and DiscussionMethod 8270D allows the use of several different calibration techniques. The

simplest is the calculation of average response factors (RF). The method specifi es

that the relative standard deviation (RSD) in RF must fall within 20 % for a minimum

of fi ve calibration levels.

Figure 1 shows the percent RSDs in RF for 71 out of 77 of the target analytes. For

compounds shown in blue, the concentrations ranged from 0.1 to 100 μg/mL with

the exception of benzoic acid, starting at 4 μg/mL.

Maximum limit

0

5

10

15

20

25

30

N-N

itro

so

dim

eth

ylam

ine

Pyri

din

e2-F

luo

roph

en

ol (s

urr

ogate

)P

hen

ol-

d5 (

su

rro

gate

)P

hen

ol

An

ilin

e2-C

hlo

roph

en

ol

1,3

-Dic

hlo

roben

zen

e1,

4-D

ich

loro

ben

zen

eB

en

zyl alc

oh

ol

1,2-D

ich

loro

ben

zen

e2-M

eth

ylph

en

ol

Bis

(2-c

hlo

rois

opro

pyl

) e

ther

4-M

eth

ylph

en

ol

Hexa

ch

loro

eth

an

eN

itro

ben

zen

e-d

5 (

su

rro

gate

)N

itro

ben

zen

eIs

oph

oro

ne

2-N

itro

ph

en

ol

2,4

-Dim

eth

ylph

en

ol

Ben

zoic

acid

Bis

(2-c

hlo

roe

tho

xy)

me

than

e2

,4-D

ich

loro

ph

en

ol

1,2

,4-T

rich

loro

ben

zen

eN

aph

thale

ne

4-C

hlo

roan

ilin

eH

exa

ch

loro

bu

tadie

ne

4-C

hlo

ro-3

-me

thyl

ph

en

ol

2-M

eth

yln

aph

thale

ne

Hexa

ch

loro

cyc

lopen

tadie

ne

2,4

,6-T

rich

loro

ph

en

ol

2,4

,5-T

rich

loro

ph

en

ol

2-F

luo

robip

hen

yl (

su

rro

gate

)2-C

hlo

ron

aph

thale

ne

2-N

itro

an

ilin

eD

ime

thyl

ph

thala

te2

,6-D

init

roto

luen

eA

cen

aph

thyl

en

e3

-Nit

roan

ilin

eA

cen

aph

then

e2

,4-D

init

roto

luen

eD

iben

zofu

ran

Die

thyl

ph

thala

te4

-Ch

loro

ph

en

yl-p

hen

yl e

ther

Flu

ore

ne

4-N

itro

an

ilin

eN

-Nit

roso

dip

hen

ylam

ine

Azo

ben

zen

e4

-Bro

mo

ph

en

yl p

hen

yl e

ther

Hexa

ch

loro

ben

zen

eC

arb

azo

lep-

Terp

hen

yl-d

14 (

su

rro

gate

)B

uty

lben

zylp

hth

ala

te3

,3'-

Dic

hlo

roben

zidin

eB

en

zo[a

]an

thra

cen

eD

i-n-

octy

l ph

thala

teB

en

zo[a

]pyre

ne

Bis(

2-c

hlo

roeth

yl)

eth

er

N-N

itro

so

di-

n-p

rop

ylam

ine

Ph

en

an

thre

ne

An

thra

cen

eD

i-n-

bu

tylp

hth

ala

teFlu

ora

nth

en

eP

yre

ne

Bis(

2-e

thyl

hexyl

)ph

thala

teC

hry

sen

eB

en

zo[b

]flu

ora

nth

en

eB

en

zo[k

]flu

ora

nth

en

eIn

den

o[1

,2,3

-cd

]pyre

ne

Dib

en

zo[a

,h]a

nth

racen

eB

en

zo[g

,h,i

]pery

len

e

Resp

on

se f

acto

r R

SD

(%

)

Figure 1. RF percent RSDs below the 8270D 20 % RSD limit for calibration.

Page 3: ANALYSIS OF SEMIVOLATILE ORGANIC COMPOUNDS

Certain compounds such as polyaromatic hydrocarbons tend to saturate the detector

at higher concentrations. In this case, it is common practice to adjust the linear range

to avoid saturation. For the compounds in Figure 1 shown in red, the concentrations

ranged from 0.1 to 50 μg/mL with the exception of benz[a]anthracene, starting at

a concentration of 0.8 μg/mL. The average percent RSD for all the compounds in

Figure 1 was 4.81%.

For the small number of SVOCs that are reactive or labile, calibration using curve

fi tting is preferred. In this case, 8270D specifi es that the correlation coeffi cient must

be greater than 0.99. Figure 2 shows the correlation coeffi cients using weighted

linear regression for the remaining six compounds.

Figure 2. Correlation coeffi cients.

Minimum

0.983

0.985

0.988

0.990

0.992

0.994

0.996

0.998

1.000

1.002

Phenol, 2,4-dinitro-

Phenol, 4-nitro-

Phenol, 2-methyl,

4,6-dinitro-

Phenol, 2,4,6-tribromo-

Phenol, pentachloro-

Benzidine

Co

rrela

tio

n c

oeffi

cein

t

ConclusionFor all of the target analytes comprising a representative mixture of acid, base

and neutral SVOCs, calibration requirements as specifi ed by method 8270D were

easily achieved using the Agilent Intuvo 9000 GC and an Agilent 5977 Series Mass

Selective Detector.

For more detailed information and methodology, refer to Application Note

5991-7256EN2.

Page 4: ANALYSIS OF SEMIVOLATILE ORGANIC COMPOUNDS

www.agilent.com/chem/intuvoInformation, descriptions and specifi cations in this

publication are subject to change without notice.

© Agilent Technologies, Inc. 2016Published in USA, August 1, 2016

5991-7180EN

References1. Weschler, C. J.; Nazaroff, W. W., Semivolatile Organic Compounds in Indoor

Environments, Atmos. Environ. 2008, 42, 9018-9040.

2. The analysis of semivolatile organic compounds using the Agilent 9000 Intuvo

Gas Chromatograph, Agilent Technologies Application Note, publication number

5991-7256EN.