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1 / 9 When things get rough you need new stuff William Lipps Analytical & Measuring Instrument Division July, 2015
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It’s out there
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All methods begin with an idea It’s coming to get you
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Are you ready?
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How will you detect it, and are your methods fast enough?
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MALDI-TOF Mass Spectrometry can identify sub-species in under 2 minutes
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Red lines indicating a spectrum match
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Algae is toxic and it Kills
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LCMSMS Analysis of Microcystins
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Polar pesticides and herbicides are difficult by GC
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Analyze pesticides and herbicides by LCMSMS, with very little sample prep
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We can analyze hundreds more pesticides with high selectivity and sensitivity by GCMSMS
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Methods can retain full scan capability and add MRM for greater selectivity and sensitivity Scan Chromatogram MRM Chromatogram 13.5013.7514.0014.25 0.25 0.50 0.75 1.00 (x10,000) 279.00>204.90 279.00>222.90 050100150200250300350400 0 25 50 75 100 % 97 223 162 65 279 117 251 173 59 135 203 259 341 397 365305 Qualification Quantification
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Analysis of solid waste for metals requires acid digestion and instrumental analysis,
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Or,
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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) PbCd Cr Al Pb Cr Cd 23.110 kev 10.552 keV 5.412 keV 1.487 keV Al Cr Pb Cd – cps/uA Fluorescent X-rays Detector Analysis sample
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20 / 9 20 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% Al 2 O 3 % SO 3 % CaO XRF1.753.9521.969.6 CRM1.933.8822.467.9
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Just place liquids, slurry samples, and emulsions in a sample cell Sample cell, film, and 5 mL oil
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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
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Foreign Matter Adhering to a Plastic Extruded Part — Fe Kb — Ni Ka — Cr Ka — Cr Ka Mn Kb — Ti Ka — Ti Kb — Ni Kb — Zn Ka — Zn Kb — Mo Ka Foreign matter Normal position Overlaid Profiles of Foreign Matter (Red) and Normal Position (Blue) — Fe Ka Sample Appearance Red circle: Foreign matter Blue circle: Normal position
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Let’s reduce toxic chemicals
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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) 10.80.94 2<0.10.05 3<0.10.24 40.660.68 511.811.6 60.780.79 72.43.11
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Should we continue with the Kjeldahl Method for TKN?
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Or use HTCO methods and obtain near equal results with TKN
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Technology is advancing faster than the methods
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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
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Thank You, for more information contact me wclipps@shimadzu.com
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