ADV06-15_1-412

Table I

Recovery and reproducibility for aliphaticsand aromatics via

low level qu ant ification . Consequently, quality

must be assured for each lot of cartridges and,

Massachusetts TPH SPE fractionation, using new Restek SPE cartridges.

sometimes, even with in lots.

AliphaticFraction

Aromatic Fraction

%Rec.ov

, Std. Dey.

RSD

Recov,

Std.Dey.

RSD

We have always specially treated our Massachusetts

1. nonane (C9)

86.4

9.11

10.5

TPH SPE cartrid ges (cat.# 26065) to ensure mini. 2. decane

(t:.1QL

84.7

7.17

8.5

mum backgrou nd extra ctables and maximum sili

3. naphthalene

82.3

6.09

7.4

4. dodecane C12

83.8

8.33

9.9

ca activity. Now, a new process has allowed us to

5. 2-methylnaphthalene

89.1

5.50

6.2

reduce extractables even furth er, and assure greater

2-fluorobiphenyl (surrog.}

92.1

6.70

7.3

reliability of fractionation. Larger uniform lots of

6. tetradecane (C14)

90.7

6.29

6.9

silica will redu ce the frequency with which a lab

7. acenaphthylene

91.6

7.63

8.3

2-bromonaphthalene (surro .

84.9

6.82

8.0

will need to verify fractionation results. New pack

8. acenaphthene

93.4

6.32

6.8

aging ensures reduced levels of coextractables and

9. fluorene

92.4

6.19

6.7

better protection from environmental humidity.

10. hexadecane (Cl6)

90.9

4.37

4.8

11. phenanthrene

90.4

5.55

6.1

Figure IC shows the background of a typical previ

12. octadecane (C18)

94.9

3.45

3.6

ous lot of cartridges, compared to the significantly

l L .anthracene

91.5

5.29

5.8

lower background from the new product, in Figure

14. nonadecane (Cl9)

91.1

3.63

4.0

o-terphenyl int. std.

96.4

3.43

3.6

l B. All cartridges were extracted with 15mL of

15. eicosane C20

89.8

2.64

2.9

hexane, with no prior conditioning. The hexane

1&:

fluoranthene

93.4

3.16

3.4

was evapora ted, o-terphenyl and l -chlorooctade

1-chlorooctadecane (int. std.)

83.1

5.02

6.0

-~~-~----

cane were added, and sampleswere reconstitut ed to

1L.Pyrene

95.1

3.84

4.0

18. docosane C22

85.2

3.97

4.7

ImL for analysis by GC-FID. Fraction ation, extrac

19. tetracosane (C24)

85.0

3.23

3.8

tion efficiency, and reproducibility also are excel

20.

benzo(a~'!!hLasene

91.2

2.38

2.6

lent, as shown by the summary in Table

Details of

21. chrysene

90.9

2.56

2.8

the extraction method, based on the Massachusetts

12. hexacosane

(<:.~)

85.8

2.97

3.5

procedure, also are presented in Table

23. octacosane (C28)

85.7

2.51

2.9

24. benzo(b)fluorantheQ.?

91.3

2.23

2.4

If you are cond ucting Massachusetts EPH analyses,

l.~jJ~lgQl~)pyrene

91.0

2.67

2.9

or similar analyses, and have been concerned about

25. benzo(k)fluoranthene

90.8

2.10

2.3

27. triacontane 0 0

86.0

2.49

2.9

the quality and uniformity of the SPE cartridges

._-~-~-

28. dibenzo(a,h)anthracene

90.9

1.78

2.0

you have been using, we think you will be as

29. indeno(l, 2,3-cd)pyrene

91.4

1.48

1.6

impressed as we are with the quality of our new

30. benzo(ghi)perylene

90.7

2.21

2.4

31. hexatriacontaneJ C36)___

_ _J8 .6

3.95

5.0

product.

n=4 (2 analyses on eachof 2 lots of SPEcartridges)

Massachusetts TPH SPE Cartridges

Analytical Conditions

Column:

Rtx"-S30m, 0.32mm!D, 0.2S/lm(cat. # 10224)

20mL, 5g, 20-pk.

26065

Sample:

SO/lL Mass EPH SurrogateSpike Mix (cat.# 31479) dilutedto

400/lg/mL

l mLMAFractionationCheckMix (cat.# 31481), 2S/lg/mLin hexane

l mLMAFractionationSurrogate Spike Mix(cat.# 31480), dilutedto

40/lg/mL

in hexane

Rtx<!l-S Column(fusedsilica)

Inj.:

O.S/lL splitless (holdO.7Smin.), Precision™split inlet liner withwool (cat.# 21027)

(Crossbond"

5%diphenyl/ 95%dimethyl polysiloxane)

Inj.temp.:

290°C

Inj. press. prog.: pressurepulseto

SOcm/sec.

-0.71min.

df (,um)

temp. limits

length

cat.

pressureto35cm/sec.

0.8 min.

0.32mm 0.25 -60 to 330/350°C

10,,,,,-

3D-Meter

,"" 224,--~

Carrier gas:

helium

Linear velocity:

3Scm/ sec., constant velocity

Oventemp.:

40°C(hold1 min.) to310°C

lSoCimin.

MA EPH Surrogate Spike Mix

Del.:

PerkinElmer AutoSYSTMGC'F!D

330°C

1-chlorooctadecane

o-terphenyl

SPEMethod

4,OOO/lg/ mL

each in acetone, 1mL/ ampul

Tube:

MassachusettsTPH20mL/Sg, cat.# 2606S

cat. # 31479

(ea.)

Tube conditioning: 30mLhexane; donot allow topfrit or bed to dry.

Sample:

Addl mLEPH samplein hexane.

Elution# 1:

Using gravity or verylowvacuum, pass18mLhexane throughtube*

MA Fractionation Check Mix

Do not allowtopfrit or bed to dry; collectthisaliphaticfractionina cleansample container.

Reduce eluate tol mLunder gentle nitrogen purge orother concentration technique.

(31 components)

Do not concentrate to lessthanl mLor allow eluate to dry before analysis.

25/l g/ mLeach in hexane, 1mL/ampul

Elution #2:

Usinggravity or low vacuum, pass20mLmethylene chloride throughtube.

Do not allowtopfrit or bedto dry; colectthis aromatic fractionina clean sample container.

cat. # 31481 (ea.)

Reducetol mL(seeabove) andanalyze.

*Note that the volume ofhexanewill vary, and shouldbeverifiedineach laboratory.

For detailsconcerningtheSPEmethod, refer to the original methodin Reference

MA Fractionation Surrogate Spike Mix

2-bromonaphthalene

2-fluorobiphenyl

References

4,OOO/lg/ mLeach in hexane, 1mL/ ampul

1 Methodfor theDetermination of ExtractablePetroleumHydrocarbons(EPH) Massachusetts Department of

cat.

31480 (ea.)

Environmental Protection, Divisionof Environmental Analysis, Ofice of Research andStandards, Bureau of

WasteSiteCleanup,Revision

1.1,

May 2004.

2 Total PetroleumHydrocarbons,TNRCCMethod100S, Revision 03(June1, 2001); Draft TNRCCMethod1006

(May 2000)Texas NaturalResourceConservationCommission.

2006

vol. 1

• 5 •

Website :

www.chromtech.net.au

E-mail :

info@chromatech.net.au

TelNo : 03 9762 2034 . . . in AUSTRALIA