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When things get rough you need new stuff William Lipps Analytical & Measuring Instrument Division July, 2015
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It’s out there
All methods begin with an idea
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
(x1,000,000) 4.0
3.0
2.0
Scan Chromatogram
1.0
11.0
11.5
100 % 75 50 25 0 0 12.0
12.5
13.0
13.5
14.0
97 59 50 65 223 162 100 117 135 150 173 203 200 Qualification 251 259 279 250 305 300 341 365 397 350 400
MRM Chromatogram
14.5
15.0
15.5
16.0
16.5
17.0
(x10,000) 1.00
279.00>222.90
279.00>204.90
0.75
0.50
0.25
13.50
13.75
14.00
14.25
Quantification 17.5
Analysis of solid waste for metals requires acid digestion and instrumental analysis,
Or,
And create new methods that use XRF
Primary X-rays Analysis sample Al Cr Pb Cd Vertical axis: X-ray intensity (cps/uA) = Concentration (ppm) – cps/uA – cps/uA – cps/uA – cps/uA Fluorescent X-rays Al Cr Pb X-ray tube Cd Al Cr Cd Pb Detector 1.487
keV 5.412
keV 10.552
keV 23.110
kev Horizontal axis: Energy (keV) = Type of element
An example of a whole rock quantitative analysis of cement
Na-S K-Zn Sr
XRF CRM
Peak Profile of Cement Standard Substance
% MgO 1.75
1.93
% Al 2 O 3 3.95
3.88
% SO 3 21.9
22.4
% CaO 69.6
67.9
Sample Appearance (Press-formed at 250 kN for 30 sec)
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) Blank Sample Overlaid Profiles of Heavy Elements in Waste Oil 10 ppm 30 ppm 50 ppm
Foreign Matter Adhering to a Plastic Extruded Part
Sample Appearance Red circle: Foreign matter Blue circle: Normal position Foreign matter Normal position Overlaid Profiles of Foreign Matter (Red) and Normal Position (Blue)
Let’s reduce toxic chemicals
Replace toxic cadmium with reductase for NOx Sample # Commercial Laboratory Results, Analysis Method EPA 335.2 (mg NO 3 +NO 2 -N/L) Analysis by Reductase (mg NO 3 +NO 2 -N/L) 1 2 3 4 5 6 7 0.8
<0.1
<0.1
0.66
11.8
0.78
2.4
0.94
0.05
0.24
0.68
11.6
0.79
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
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MALDI TOF – New, faster way to confirm bacteria
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LCMSMS – Emerging Contaminants not visible before
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GCMSMS – more sensitive, higher throughput
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XRF – no digestions, higher throughput
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NOx – safer, non toxic reagents
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TN – safer and higher throughput than TKN
Thank You, for more information contact me