Lab Standard Operating Procedure:
PFAS analysis
Title of Procedure: Analysis of poly- and per-fluoroalkyl substances in different environmental
and biological samples
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PI: Elsie Sunderland
Room & Building: ESL305
Department: SEAS
Research Group: Sunderland
Date: 07/16/2015
Pertains to Lab Protocol: PFAS analysis
Prepared by: Xianming Zhang
DESCRIPTION
Sample preparation for the determination of selected perfluoroalkyl substances (PFASs) in environmental (e.g. water),
animal and plant tissues (e.g. fish fillet) using liquid chromatography/tandem mass spectrometry (LC/MS/MS)
PROCEDURE (See documented method for details)
~1 g wet-weight equivalent homogenized tissue is fortified with isotope labeled internal standards. The analytes are subjected to ionpairing extraction using methyl-tert-butyl ether (MTBE). The extract is then concentrated to dryness with nitrogen and then adjusted to a
0.5-mL methanol solution. The solution is filtered with non-syringe polypropylene filter. A 20-µL injection is made into an Agilent 6460
LC-MS/MS system
x
x
x
x
x
x
Irritant
Other Comments:
x
x
x
x
x
x
x
Unstable
Carcinogen
Shock-Sensitive
Water-Reactive
Pyrophoric
Acutely Toxic
Biological Toxin
Teratogen
Mutagen
Sensitizer
Corrosive
Principal Materials Used
Methanol
Methyl-tert-butyl ether
Ammonium hydroxide
Tetra-butyl ammonia
bisulfate
Sodium carbonate
Acetonitrile
PFAS standards
Flammable
POTENTIAL HAZARDS
x
x
x
Notes: PFAS standards come as solutions in organic solvents such as methanol, isopropanol and
nonane. Although the maximum concentration is 50 µg/ml, that is 0.005% (w/v), these compounds
must be considered toxic and should be handled accordingly.As with all of our products, due care
should be exercised to prevent human contact and ingestion. The absence of a toxicity warning for
any of our products must not be interpreted as an indication that there is no possible health hazard.
These materials should only be used by personnel trained in the handling of hazardous chemicals.
All procedures should be performed in a fume hood and suitable gloves, eye protection and clothing
should be worn at all times.
Despite methyl-tert-butyl-ether is less likely to form explosive peroxide compared to other ethers, ,
prolonged exposure to light and air should be avoided
Lab SOP
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ENGINEERING/VENTILATION CONTROLS
_Handle organic solvent in vented fume hood Collect waste in tightly sealed container. Store away
from non- compatibles in a cool, well ventilated, flammable liquid storage area for disposal in
accordance with Harvard regulation
REQUIRED PERSONAL PROTECTIVE EQUIPMENT
(Refer to your lab’s PPE Assessment Report, supplemented with information here)
The level of skin and eye protection should be selected based on the potential for splashing and other forms of
exposure.
Minimum potential for splash & exposure:
! Chemical splash goggles
! Single pair of neoprene rubber gloves recommended (however, may be bulky)
• Double nitrile gloves acceptable, but note that there is a shorter breakthrough time.
o Double-gloving is recommended, given the diversity of chemical hazards and
highly corrosive chemicals involved. Consider a different color and chemistry
with each layer.
o Immediately replace with new gloves when splash occurs.
! Protective clothing (e.g. impervious lab coat, sleeves, closed-toed footwear)
When using or transferring large quantities, or for spill clean-up:
! Chemical splash goggles
! Heavier gloves made of polyvinyl alcohol (PVA), or double neoprene rubber gloves
• Double-gloving is recommended, given the diversity of chemical hazards and highly
corrosive chemicals involved. Each layer may be a different color and chemistry.
• Immediately replace with new gloves when splash occurs.
! Chemical resistant, impervious apron/smock/lab coat (PE, PVC, natural rubber, neoprene, or
Silver ShieldTM) that ties from behind.
• Avoid using the traditional cotton-polyester white lab coat, which readily
collects/absorbs compounds.
! Protective clothing (e.g. sleeves, impervious boots or PVC disposable shoe coverings, closedtoed footwear)
ADDITIONAL PRECAUTIONS
Handling: with caution
Storage: Cabinet for flammables
Permits:
Mgmt. Approval:
Training: Chemical safety training, procedure demonstration
Medical Surveillance:
Other:
Lab SOP
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SAFETY REFERENCES
Additional chemical safety information, including MSDSs and other information, is available
electronically as tools at ehs.harvard.edu/programs/safe-chemical-work-practices.
WASTE DISPOSAL
Refer to the Laboratory Waste Guide posted at ehs.harvard.edu/node/7699.
EMERGENCY PROCEDURES
(Refer to the Emergency Response Guide posted in your lab, supplemented with information here)
•
Fire/Evacuation: In the event of fire, evacuate and bar further entry. Activate fire alarm
and leave the building
•
Chemical Spill:
For small spills, follow chemical spill response guidelines above. Don protective clothing,
extinguish all ignition sources, and carefully apply vermiculite or other appropriate spill
absorbent material to the spill. Place in a durable and sealable container for disposal.
For spill clean-ups, use polyvinyl alcohol (PVA) gloves (chemical breakthrough time > 8 hrs).
Do not wear nitrile gloves (with a breakthrough time of a few minutes), due to the risk of
direct or prolonged contact when cleaning up a spill.
Respiratory protection may be necessary in the event of a large spill or release in a confined
area.
For a large spill, vacate the lab, deny further entry, and call the University Operations Center
at 5-5560 for assistance
•
Medical Emergency: University Health Services (UHS), 617-495-5711
•
Personal Exposure: Emergency:911; non-emergency: 617-495-5711
Reference(s):
a. Sunderland Group Analytical Method. Determination of selected perfluorinated alkyl substances
in tissue sample via ion-pairing extraction and liquid chromatography / tandem mass
spectrometry (LC/MS/MS), 2015 prepared by Xianming Zhang
b. Determination of selected perfluorinated alkyl acids in drinking water by solid phase extraction
and liquid chromatography/tandem mass spectrometry (LC/MS/MS). 2009, EPA Document #:
EPA/600/R-08/092.
c. [author(s), document 1 title, publisher, year]
Lab SOP
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