Solid Phase Extraction Issues

TRC September 2007

Solid Phase Extraction (SPE)

 Provides a means for preconcentrating water

phase organics to allow lower detection limits
without logistically intimidating sample sizes
(~20L equivalent per analyte type- PCBs,
PAHs, etc)
 May show some artifacts of incomplete
recovery, depending on a number of factors,
e.g. DOC, sample size, collection speed
RMP Collection Methodology

 100L sample, pumped at 1.5L/min by Infiltrex

300 through wound glass filter (nominal 1um
pore) and columns (2x70g) of XAD2 resin.
 Most recent cruise increased volume pumped
through filter to increase PBDE signal relative
to blanks (no change in pumping speed)
Infiltrex vs Whole Water
2003 PCB 100L vs 4L

 4L whole water 12

sample vs 100L 10
BG30

Infiltrex

4 L results (pg/L)
8

particulate (filter) 6

+ dissolved 4
y = 1.5875x + 0.046
R2 = 0.9916
(XAD2) 2

0
0 2 4 6 8 10 12
100 L results (pg/L)
2004
2004 PCB 100L vs 4L

70
SB026W
60 SPB010W

50
4L results (pg/L)

y = 1.1164x - 0.615
40
R2 = 0.9309
30
y = 0.5856x + 0.432
20
R2 = 0.9754
10

0
0 10 20 30 40 50 60 70
100L results (pg/L)
2005
2005 PCB 100L vs 4L

50

45 SB036W
40 CB015W

35
4 L results (pg/L)

y = 1.2096x + 0.0227
30 2
R = 0.9891
25

20

15

10 y = 0.7442x + 0.1428
5 R2 = 0.9925

0
0 10 20 30 40 50
100 L results (pg/L)
Bias Trend?

max
PCB
site year (100L) slope SS DOC
BG30 2003 6 1.59 23.5 1606
CB015 2005 10 1.21 3.8 1014
SPB010 2004 22 1.12 34.5 1650
SB036 2005 40 0.74 9.0 2463
SB026 2004 65 0.59 18.0 1870
Bias Trend?

 Does not track TSS (SSC)

 4L (liquid-liquid) solvent extraction recovery
high for low organics (=totPCBs)
– 100L short contact time = lower recovery?
 100L solid phase extraction high(er) for high
organics samples
– 4L solvent volume = limited equilibrium?
Alternatives

 Switch to liquid-liquid extraction

– Likely accurate for low organics
– Underestimate for high concentrations
– PCB/PBDE, PAH, OCP, OPP, backup = 4L x 5
bottles/site x 22 sites = 110 bottles, 440L to ship
 Status quo 100L SPE- (preferred?)
– Maintain awareness of tendencies
– Considered minimum concentrations
– More accurate for high concentration samples