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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
 4L whole water
sample vs 100L
Infiltrex
particulate (filter)
+ dissolved
(XAD2)
2003 PCB 100L vs 4L
y = 1.5875x + 0.046
R2
= 0.9916
0
2
4
6
8
10
12
0 2 4 6 8 10 12
100 L results (pg/L)
4
L
results
(pg/L)
BG30
2004
2004 PCB 100L vs 4L
y = 1.1164x - 0.615
R2
= 0.9309
y = 0.5856x + 0.432
R2
= 0.9754
0
10
20
30
40
50
60
70
0 10 20 30 40 50 60 70
100L results (pg/L)
4L
results
(pg/L)
SB026W
SPB010W
2005
2005 PCB 100L vs 4L
y = 1.2096x + 0.0227
R
2
= 0.9891
y = 0.7442x + 0.1428
R2
= 0.9925
0
5
10
15
20
25
30
35
40
45
50
0 10 20 30 40 50
100 L results (pg/L)
4
L
results
(pg/L)
SB036W
CB015W
Bias Trend?
site year
max
PCB
(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

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8_Solid_Phase_Extraction_Issues_2 (1).ppt

  • 1. Solid Phase Extraction Issues TRC September 2007
  • 2. 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
  • 3. 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)
  • 4. Infiltrex vs Whole Water  4L whole water sample vs 100L Infiltrex particulate (filter) + dissolved (XAD2) 2003 PCB 100L vs 4L y = 1.5875x + 0.046 R2 = 0.9916 0 2 4 6 8 10 12 0 2 4 6 8 10 12 100 L results (pg/L) 4 L results (pg/L) BG30
  • 5. 2004 2004 PCB 100L vs 4L y = 1.1164x - 0.615 R2 = 0.9309 y = 0.5856x + 0.432 R2 = 0.9754 0 10 20 30 40 50 60 70 0 10 20 30 40 50 60 70 100L results (pg/L) 4L results (pg/L) SB026W SPB010W
  • 6. 2005 2005 PCB 100L vs 4L y = 1.2096x + 0.0227 R 2 = 0.9891 y = 0.7442x + 0.1428 R2 = 0.9925 0 5 10 15 20 25 30 35 40 45 50 0 10 20 30 40 50 100 L results (pg/L) 4 L results (pg/L) SB036W CB015W
  • 7. Bias Trend? site year max PCB (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
  • 8. 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?
  • 9. 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