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When things get rough you need new stuffWilliam LippsAnalytical & Measuring Instrument DivisionJuly, 2015
It’s out there
All methods begin with an idea
It’s
co
min
g to
get yo
u
Are you ready?
How will you detect it, and are your methods fast enough?
MALDI-TOF Mass Spectrometry can identify sub-species in under 2 minutes
Red lines indicating a spectrum match
Algae is toxic and it Kills
LCMSMS Analysis of Microcystins
Polar pesticides and herbicides are difficult by GC
Analyze pesticides and herbicides by LCMSMS, with very little sample prep
Analyze pesticides and herbicides by LCMSMS, with very little sample prep
We can analyze hundreds more pesticides with high selectivity and sensitivity by GCMSMS
Methods can retain full scan capability and add MRM for greater selectivity and sensitivity
11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 16.0 16.5 17.0 17.5
1.0
2.0
3.0
4.0
(x1,000,000)
Scan Chromatogram
MRM Chromatogram
13.50 13.75 14.00 14.25
0.25
0.50
0.75
1.00
(x10,000)
279.00>204.90279.00>222.90
0 50 100 150 200 250 300 350 400
0
25
50
75
100
%
97
223
16265
27911725117359 135 203
259 341397
365305
Qualification Quantification
Analysis of solid waste for metals requires acid digestion and instrumental analysis,
Or,
And create new methods that use XRF
X-ray tube
Primary X-rays
Horizontal axis: Energy (keV) = Type of element
Vertical axis: X-ray intensity (cps/uA) = Concentration (ppm)
Pb Cd
CrAl
AlPb
CrCd
23.110kev
10.552keV
5.412keV
1.487keV
Al
Cr
Pb
Cd
– cps/uA
– cps/uA
– cps/uA
– cps/uA
Fluorescent X-rays
Detector
Analysis sample
20 / 920
An example of a whole rock quantitative analysis of cement
Na-S SrK-Zn
Peak Profile of Cement Standard Substance
Sample Appearance
(Press-formed at 250 kN for 30 sec)
% MgO % Al2O3 % SO3 % CaO
XRF 1.75 3.95 21.9 69.6
CRM 1.93 3.88 22.4 67.9
Just place liquids, slurry samples, and emulsions in a sample cell
Sample cell, film, and 5 mL oil
Elements in Waste Oil (0, 10, 30, and 50 ppm of each element)
Overlaid Profiles of Heavy Elements in Waste Oil
30 ppm
Blank Sample
50 ppm
10 ppm
Foreign Matter Adhering to a Plastic Extruded Part
— F
e K
b—
Ni K
a
— C
r K
a
— C
r K
a
Mn
Kb
— T
i Ka
— T
i Kb
— N
i Kb
— Z
n K
a
— Z
n K
b
— M
o K
a
Foreign matter
Normal position
Overlaid Profiles of Foreign Matter (Red) and Normal Position (Blue)
— F
e K
a
Sample Appearance
Red circle: Foreign matterBlue circle: Normal position
Let’s reduce toxic chemicals
Replace toxic cadmium with reductase for NOx
Sample # Commercial Laboratory
Results, Analysis Method EPA 335.2 (mg
NO3+NO2-N/L)
Analysis by Reductase (mg NO3+NO2-N/L)
1 0.8 0.942 <0.1 0.053 <0.1 0.244 0.66 0.685 11.8 11.66 0.78 0.797 2.4 3.11
Should we continue with the Kjeldahl Method for TKN?
Or use HTCO methods and obtain near equal results with TKN
Technology is advancing faster than the methods
It’s time for some new stuff
• MALDI TOF – New, faster way to confirm bacteria
• LCMSMS – Emerging Contaminants not visible before
• GCMSMS – more sensitive, higher throughput
• XRF – no digestions, higher throughput
• NOx – safer, non toxic reagents
• TN – safer and higher throughput than TKN
