Impact of New Analytical Technologies on Environmental LaboratoriesCharles Carter, Ph.D.Vice President

October 11, 2011©2011, TestAmerica Laboratories, Inc. All rights reserved.TestAmerica & Design ™ are trademarks of TestAmerica Laboratories, Inc.

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Topics

• A few new technologies• Impact on laboratories• Improvements to old technologies• Impact on laboratories• Unintended consequences

Solid phase microextraction

UPLC/MS/MS

How a UPLC/MS/MS Works

• Compounds bound then eluted from a reverse phase LC column using an Ultra Performance LC

• Solvent is removed and then ions are produced• Ions travel through the first quadrupole where selected

product masses pass through and other masses and interferences are filtered

• Ions travel through the second quadrupole/collision cell where they are fragmented into daughter ions

• Daughter ions travel through the third quadrupole where selected daughter masses pass through and other masses and interferences are filtered

• Compounds are identified based on parent>daughter transition masses

Massive list of supported analytes

Perfluorobutanoic acid (PFBA) 2 ng/LPerfluoropentanoic acid (PFPeA) 2 ng/LPerfluorohexanoic acid (PFHxA) 2 ng/LPerfluoroheptanoic acid (PFHpA) 2 ng/LPerfluorononanoic acid (PFNA) 2 ng/LPerfluorodecanoic acid (PFDA) 2 ng/LPerfluoroundecanoic acid (PFUnA) 2 ng/LPerfluorododecanoic acid (PFDoA) 2 ng/LPerfluorotridecanoic acid (PFTriA) 2 ng/LPerfluorotetradecanoic acid (PFTeA) 2 ng/LPerfluorobutane sulfonate (PFBS) 2 ng/LPerfluorohexane sulfonate (PFHxS) 2 ng/LPerfluorodecane sulfonate (PFDS) 2 ng/LPerfluorooctane sulfonamide (PFOSA) 2 ng/LPerfluoro-n-hexadecanoic acid (PFHxDA) 2 ng/LPerfluoro-n-octandecanoic acid (PFODA) 2 ng/LPerfluoro-1-heptanesulfonate (PFHpS) 2 ng/LPerfluoro-1-octanesulfonamidoacetic acid (FOSAA) 2 ng/LPerfluorooctanoic Acid (PFOA) 2 ng/LPerfluorooctanesulfonic acid (PFOS) 2 ng/L

UCMR analytes

Compound RL UnitsAcetochlor ESA 1 ug/LAcetochlor OA 2 ug/LAlachlor ESA 1 ug/LAlachlor OA 2 ug/LMetolachlor ESA 1 ug/LMetolachlor OA 2 ug/L

Chemical Warfare Degradates

Compound RL UnitsDIMP 10 ug/LDMMP 10 ug/LEMPA 10 ug/LIMPA 20 ug/LMPA 100 ug/LThiodiglycol 10 ug/L

Explosives

Compound RL Units2-Amino-4,6-dinitrotoluene 0.1 ug/L4-Amino-2,6-dinitrotoluene 0.1 ug/LBromacil 0.1 ug/LDiethanolamine 0.1 ug/L1,3-Dinitrobenzene 0.1 ug/L2,4-Dinitrotoluene 0.1 ug/L2,6-Dinitrotoluene 0.1 ug/LDiuron 0.1 ug/LHMX 0.1 ug/LN-Nitrosodiethanolamine 0.1 ug/LNitrobenzene 0.1 ug/LNitroglycerin 10 ug/L3-Nitrotoluene 0.1 ug/L4-Nitrotoluene 0.1 ug/L2-Nitrotoluene 0.1 ug/LPETN 10 ug/LRDX 0.1 ug/LTetryl 0.1 ug/L1,3,5-Trinitrobenzene 0.1 ug/L2,4,6-Trinitrotoluene 0.1 ug/L

Surfactants, hexachlorophene, perchlorate

Compound RL Units4-Chlorobenzene Sulfonic Acid 1 ug/L4-Bromobenzene Sulfonic Acid

Compound RL UnitsPerchlorate 0.5 ug/L

Compound RL UnitsHexachlorophene Who cares? ug/L Footnote 1

1. Put on the Appendix IX list in the mid 1980's.It has never been detected, even once, at any concentration, in any laboratory, in any sample.

Pharmaceuticals and Personal Care Products

CompoundAndrostenedioneAndrosterone17a-DihydroequilinEquileninEquilin17a-Estradiol17b-EstradiolEstriolEstrone17a-Ethynyl EstradiolProgesteroneTestosterone

CompoundAcetaminophenAzithromycinCaffeineCarbamazepineCotinineDiltiazemFluoxetineGemfibrozilIbuprofenIopromideLincomycinNaproxenSulfamethoxazoleTrimethoprimTylosinTriclocarbanTriclosan

Impact on laboratories

• New and interesting technologies• Advancing state of the art• Exploring new environmental issues• Essential capability for certain projects• 0.5% of annual revenue

One of the greatest advances in the history of the environmental

laboratory business

Data processing speed

• Metals data package today~ A few minutes

• Metals data package 20 years ago~ Hours of processor time

• Press any key to continue

• Press any key to continue

Instrumentation advances, what has changed

• Replacement of atomic absorption• ICPMS• Pressure programming in GC• Advances in capillary chromatography• VOA autosamplers• Automated general chemistry systems• Some automation in sample preparation• Large volume injectors• Fast autosamplers for ICP and ICPMS• Significantly improved reliability of new generation instruments• Simpler instrument operation and resulting decrease in learning

curve

What has not changed

• Analyte lists~ Priority pollutants, appendix 1, 2, and 9, PAHs, pesticides

and PCBs that have been banned for one to three decades

• Underlying analytical technology~ ICPAES~ GC/MS, GC/ECD, GC/FID

Advances in ICP-AES

• Sample introduction and torch largely unchanged• Significant changes in optics and light detection• Vastly increased flexibility – no fixed optical bench• Interelement interference correction with old technology

Old Detector Technology

20-40 photomultiplier tubes (PMT) lined up in order by wavelength

Each fixed in place for one element

One-dimensional detector array

Spectral overlap can only come from an adjacent λ

3-D Spectral Display andNew Kind of Spectral Overlap

Pb and Si have emission lines geometrically close,but not sequential, i.e., non-adjacent λs

Spot due to 40 ppm Si at 220.570 nm

Window for Pb at 220.350 nm

Full Frame View of ICP Camera Chip

Technology has advanced, methods need to catch up

• Vastly increased possibility of both positive and negative interferences

• Existing method QC checks entirely adequate for old technology

• Existing method QC checks have no chance of detecting new interferences in current generation of optical chip based instruments

• Significantly more rigorous procedures required to avoid interferences

• Unintended consequence of an advancement in technology

Conclusion

• Same old stuff• Industry survivors are a lot faster• Emerging and advanced areas have always been slow

to develop~ Explosives~ Perchlorate~ Congener specific PCBs~ PBDEs

• True of current emerging areas as well• Sometimes new technology and existing method criteria

are not entirely compatible