Title: Specific Identification of Organic Pollutants in the Catawba Watershed Wastewater Treatment Plant Effluents
1Specific Identification of Organic Pollutants in
the Catawba WatershedWastewater Treatment Plant
Effluents
- John Turner
- Faculty Mentor Dr. Pat Owens
- Faculty Committee Members Dr. Pat Owens,
- Dr. Cliff Calloway, Dr. Peter Phillips
2Threats posed by organics
- Many are toxic (harmful), carcinogenic
(cancer-causing), or mutagenic (capable of
altering genetic material) at very low levels - Many organics have been shown to be endocrine
disruptors capable of altering the sex of fishes
- May have the capability for bioaccumulation in
the fat cells and membranes
3From The Charlotte ObserverOctober 4th, 2004
4The Status Quo
- Presently there is no testing of organic levels
in WWTP effluents within the Catawba watershed - Furthermore, testing of drinking water and river
water for organics is not being done.
- Some organics such as 1,4-dioxane have been known
to travel as far as 200 kilometers from its point
of entry in a watershed. (Draper et al, 2000)
5Research Design and Methods
- Collection of WWTP samples
- Bottle washing procedure
- Glass bottles (approximately 600 mL) were used
with glass stoppers - 2 mL HPLC grade Methanol added to each bottle
- Stoppers returned to bottle and rolled and
flipped so that Methanol completely covered the
inside of the bottle - This was then repeated using reagent grade Ethyl
Acetate - Unstopped bottles were placed in a dry oven at
108oC for 24 hours
6Research Design and Methods
- Collection of WWTP samples
- Samples were collected from 2 WWTPs
- Samples were collected from Rock Hill (Manchester
Creek) and Fort Mill WWTPs. - The samples that were collected were composite
samples
7WWTP Locations
- Rock Hill WWTP (Manchester)
- Fort Mill WWTP
8Research Design and Methods
- Organic Extraction
- The Basic Apparatus
Glass Funnel Membrane Filter Vacuum
Hose Erlenmeyer Vacuum Flask
9Research Design and Methods
- Organic Extraction
- Empore C18 Membrane Filter Preparation
- An Empore C18 Membrane Filter was placed at the
bottom of the Glass Funnel on the screen. - 25 grams of Empore Filter Aid glass beads were
added to the funnel - The disk was washed with 20 mL of elution solvent
(methanol or ethyl acetate) and then allowed to
dry - 20 mL of methanol was used to condition the disk
10Research Design and Methods
- Organic Extraction
- Concentration of Organics onto the filter
- The sample was decanted into the glass funnel.
- The vacuum was then applied and the sample was
allowed to run through the disk. - The vacuum was allowed to continue to run for
5-20 minutes so that residual water was removed.
11Research Design and Methods
- Organic Extraction
- Organic Elution
- The organics were eluted from the disk into an
organic phase, and they were collected by placing
a Kuderna-Danish flask under the membrane filter.
- 10 mL of elution solvent was then added (either
methanol or ethyl acetate) so that it covered the
disk completely - The vacuum was used to pull the solvent that now
contains the organics into the Kuderna-Danish
flask.
12Research Design and Methods
- Organic Extraction
- Concentration of Elution
- Once the organics were concentrated into 10 mL of
solvent they were further concentrated for
analysis. - Two mL of elution solvent was removed.
- Then the remaining 8 mL of elution solvent was
evaporated down to approximately 1 mL. - This was done by blowing a gentle stream of
nitrogen that passed through an organic carbon
filter over the solvent.
13Research Design and Methods
- Organic Extraction
- Analytical Plan
500 mL of Water
10 mL of extract
1 µL analyzed
1/50th
1 mL of extract
1/500th
1 µL analyzed
14Research Design and Methods
- Run Gas Chromatography-Mass Spectrometry
- 1 µl of extract was injected into the GC column
- The extract contains a mixture of the organics
that were originally found in the wastewater but
have now been concentrated into an organic phase. - The GC column separated the analytes based upon
their polarity. - The MS measured the molecular weight of the
various ions and a chromatogram was produced.
15Results
- Siloxanes
- Phenol
- Phthalates
16Siloxanes D5
- Rock Hill WWTP
- 8.044 min with Ethyl Acetate
- 8.043 min with Methanol
17D5 (cyclopentasiloxane)
18Library Match for D5
19Siloxanes D6 (cyclohexasiloxane)
- Rock Hill WWTP
- 11.915 min with Ethyl Acetate
20Library Match for D6
Loss of 88
21Siloxanes D7(cycloheptasiloxante)
- Rock Hill WWTP
- 16.512 min with Ethyl Acetate
22Library Match for D7
23Siloxanes D8 (cyclooctasiloxane)
- Rock Hill WWTP
- 21.165 min with Ethyl Acetate
24Siloxanes D9 (cyclononasiloxane)
- Rock Hill WWTP
- 25.317 35.826 min with Ethyl Acetate
25Siloxanes D10 (cyclododecasiloxane)
- Rock Hill
- 29.171, 32.651, 38.769, 41.553, 44.177, 46.642,
48.208, and 49.746 min with Ethyl Acetate - 15.744 min with Methanol
- Fort Mill
- 37.174 and 42.471min with Ethyl Acetate
- 45.103 min with Methanol
26Library Match for D10
27Risks Associated with Siloxanes
- Bioaccumulation in tissues and organs
- Capable of inhibiting estrogen, leading to
reproductive problems
28Phenol
- Rock Hill WWTP
- 17.699 min with Ethyl Acetate
- 17.672 min with Methanol
29Library Match for Phenol
30Risks Associated with Phenol
- Most affects are related to the exposure to large
quantities over time - Probably not a major problem unless found in
substantial quantities
31Bis (2-ethylhexyl) phthalate
- Rock Hill WWTP
- 42.699 min with Methanol
- Fort Mill
- 42.726 min with Methanol
32Library Match for a Phthalate
33Risks Associated withBis (2-ethylhexyl) phthalate
- Has been shown to bioaccumulate in tissue
- Affects the abilities of males to father babies
34Conclusions
- GC-MS was shown to be an effective means of
identifying organics in wastewater - Within the organics identified, the siloxanes and
phthalates have serious health effects at very
low levels - This research established a basic understanding
of the use of GC-MS in identifying organics in
wastewater and has accumulated information to
fuel further research in this area in the future
at Winthrop