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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

Thank You, for more information contact me

wclipps@shimadzu.com