100
8
80
6
60
4
40
2
20
0
0.0003
0.0006
0.0009
0.0012
0.0015
0.020
0
0.005
0.010
0.015
White Phosphorus Concentration (g/g) by Solvent Extraction
WP Concentration (g/g) by Solvent Extraction
a. Data within linear range of detector.
b. Same data as a, showing results at lowest concentra-
tions detected.
Figure 5. Mass of white phosphorus detected by headspace SPME and concentration found in same sediment sample
following solvent extraction.
Water
Sediment/ Soil
(25 mL)
(40 g plus water to form slurry)
Headspace Solid Phase
Micro-Extraction (SPME) (5 min)
Headspace Solid Phase
and
Micro-Extraction (SPME) (5 min)
Thermal Desorption in Gas Chromatograph
and
Nitrogen Phosphorus Detector (NPD)
Thermal Desorption in Gas Chromatograph
Nitrogen Phosphorus Detector (NPD)
No
White Phosphorus Detected by SPME?
Stop
No
Stop
White Phosphorus Detected by SPME?
Yes
Estimate White Phosphorus
Yes
Avoid Solvent
Concentration Based on Matrix
Yes
Extraction?
Calibration Standards
Extract Sediment/Soil with 10 mL Isooctane
No
Extract 500 mL Water with 50 mL Diethyl Ether
Analyze Extracts by Gas Chromatography
Nitrogen Phosphorus Detector
Collect Ether Extract
Reduce Volume of Ether Extract to 1.0 mL
Calculate White Phosphorus Concentration
by Mixing with Reagent Water
Based on Calibration Standards in Isooctane
a. Sediment/soil method.
Analyze Extracts by Gas Chromatography
Nitrogen Phosphorus Detector
Figure 6. Flow chart of analytical methods for white
b. Water method.
Calculate White Phosphorus Concentration
phosphorus with headspace SPME used to screen
Based on Calibration Standards in Ether
samples for white phosphorus.
Ma. Wa
MaW 0
10
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