# Presentation: 046400

## Triclosan

**One Example of How Emerging Pollutants Come to Our Attention**
**Steven Reimer**
**EPA Region 10 Laboratory**

## 1997 – 1998 Region 10 Laboratory

- CRITFC Project: ~300 fish samples for broad spectrum of organics and metals
- First large scale survey of fish for consumption in area
- Lab participated in identifying target list
- Found “usual suspects”

## PCB Aroclor Analysis

- Extra peaks on ECD eluting after Aroclor 1260
- Present in bottom dwelling and older fish
- Did not match Aroclor 1268 or chlorinated terphenyl pattern
- Analysis on GC with Atomic Emission Detector showed bromine, not chlorine!

## Mystery Bromine Compounds

- Identified Brominated Diphenyl Ethers as probable
- No commercially available standard so homemade “Bromkal 70” generated to make a standard
- Able to report “total PBDE” from this analysis

## 2001 - 2002

- Standards available through Cambridge Isotopes
- Revisit same fish samples, this time with individual standards
- Check “homemade” standard vs “storebought”
- Look for sources in environment

## Potential Sources, based on Literature

- WWTP effluent – water and sludge
- Storm water runoff
- Industrial effluent

## Sampling of Possible Sources

- Five WWTP from Industrial (Tacoma) to agricultural (Yakima) to residential (Port Orchard)
- Sediments above and below the outfalls for each WWTP
- Biosolids end user

## Procedure

- Soxhlet Extraction
- Florisil treatment
- Acid treatment
- Sulfur removal
- GC/ECD analysis

## Frustration!

## “Maybe it isn’t sulfur”

- GC / Mass Spectrometer
- Clearly a chlorophenol “5-chloro-2-(2,4-dichlorophenoxy)phenol”
- Need a quick standard for comparison
- Toothpaste (Colgate) extract used 0.3% triclosan
- Standard ordered from Aldrich

## What was there?

|  |  |  | Triclosan    |  |  |  |
| --- | --- | --- | --- | --- | --- | --- |
| Site location | sample # | Matrix | results |  |  | bde 47 |
|  |  |  | ppb | qual |  | ppb |
| Rich.WWTP activ | 4117 | sludge | 620.00 |  |  | 1200.00 |
| Rich.WWTP digest | 4118 | sludge | 23000.00 |  |  | 760.00 |
| Prosser WWTP | 4131 | sludge | 3500.00 |  |  | 240.00 |
| Prosser WWTP | 4132 | sludge | 4200.00 |  |  | 200.00 |
| Prosser WWTP | 4133 | sed | 1.20 |  |  | 0.60 |
| Prosser WWTP | 4134 | sed | 1.40 |  |  | 0.50 |

## Slide 12

| hop field control | 4135 | soil | 0.04 | u |  | u |
| --- | --- | --- | --- | --- | --- | --- |
| hop field biosolids | 4136 | soil | 150.00 |  |  | 33.00 |
| hop field conc biosol | 4137 | soil | 29000.00 |  |  | 1300.00 |
| MD creek  | 4138 | sed | 4.50 |  |  | 0.50 |
| Yakima riv Zillah | 4140 | sed | 0.74 |  |  | 0.47 |
| Yakima WWTP | 4143 | sludge | 16000.00 |  |  | 1000.00 |
| Yakima WWTP | 4144 | sludge | 4100.00 |  |  | 950.00 |

## Why did this work?

- Time to work on extras
- Equipment, especially AED and MS to ID unknowns
- Able to find standards. PBDE standards were not available in ’97
- Picky analysts
- Luck!

## Credit where credit is due

- Bob Rieck – analysis, sample prep and cleanup, project direction
- Randy Cummings – analysis, deity of AED and user of Colgate
- Dave Terpening, Doc Thompson, and Jed Januch – sampling under trying circumstances