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OmniTek brings you current developments in molecular analysis: Low Resolution IR and Electron Spin Resonance
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E-mail: info@omnitek.nl
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Subjects in this information bulletin
 
1.       Low Resolution Infrared (IR) Spectroscopy
1.1.   Low Res IR can be superior over FTIR
1.2.   Biodiesel analysis


2.       Examples of instruments
2.1.   Wilks IR Filtometers
2.2.   Spectro Inc Oil Condition Monitor


3.       Electron Spin Resonance
3.1.   Original study on engine lubricant
3.2.   Marine oil investigation
3.3.   Experimental application: Oxidation in ester-based oils
3.4    Instruments by Active Spectrum
New intuitive touch screen display on Wilks InfraCal 2:

· High sensitivity, performance
· Touch screen display
· Multiple calibrations
· Up to 4 wavelengths
· Internal data logging
· Alarm functions
· Security/password protection
· Data transfer capabilities

1.       Low Resolution Infrared Spectroscopy

1.1.    Low Res IR can be superior over FTIR
Resolution is often used as a yardstick of instrument performance in Infrared Spectroscopy. This is especially true when the measurements are energy limited as they are in the mid-infrared.
For example, in both the European and ASTM standards - EN14078 and ASTM D7371 - for the determination of biodiesel in diesel fuel, a 4 cm-1 resolution is specified which is a relatively high resolution. Resolution is important to qualitatively examine specific components and attributes of a sample, but quantitative analysis does not always benefit from higher resolution. In fact, as has been pointed out in the past by Hart and Griffiths, a lower resolution instrument will actually perform better for quantitative measurements where absorbance peaks are well defined and not overlapping. This can be demonstrated with the following example of biodiesel in diesel.

1.2.    Biodiesel analysis


The data shown seems to contradict the spectra shown in picture above, since the high resolution spectra had a more visibly intense and clearly defined peak. When using high resolution, however, there is a trade off in the signal-to-noise ratio. Typically, instruments operating at a lower resolution will have a higher signal to noise ratio. Figure below shows the noise level of the FT-IR used in this study at both the 4 cm-1 and 16 cm-1 resolution. It is clear that the noise level is significantly lower when the instrument is operating at low resolution. This lower noise level results in a higher degree of precision in the spectra, which translates to a better performing calibration.

2.       Examples of instruments
 
Several OEM's have realized that Low-res Mid-IR can perform specific tasks on a (mobile or remote) quality control lab. We would like to introduce a few to you.
 
2.1.   Wilks IR Filtometers
  • ATR cell
  • Flow trough cell
  • Transmission cells based instruments

Fixed Filter based
The InfraCal Filtometer can be customized for in-/out house process monitoring

 
Variable filter
The InfraSpec VFA-IR Spectrometer can be customized for your specific analysis

 
Typical Applications
- Single component analysis
- Total Oil & Grease (TOG) & Total Petroleum Hydrocarbon (TPH) Levels in Water & Soil (Fracking)
- Ethanol in Gasoline and Water in Ethanol
- Measuring Soot in Diesel Engine Oil
- Fats, Oils and Grease (FOG) in Wastewater
- Measuring Antioxidant Inhibitor in Transformer Oil
- Measuring Nylon, EVA or EVOH in a Multilayer Film
- Determining Unsulfonated Matter (UM) in Surfactant
- Checking Cleaning Efficiency of Metal Parts
- Resin Coatings on Metal Substrates

- D2O in H2O and H2O in D2O
Typical Applications
- Multiple component analysis
- Biofuel blend analysis
- Free Fatty Acids (FFAs) Analysis in Biodiesel
- Feedstock and Edible Oils
- Alcohol Measurements in Beverages
- Trans-fatty Acid Analysis
- Flexible film analysis
- Raw materials verification
- Solvents in water
- Oil in Vertrel
-  Isocyanates
 

 
Recently Wilks IR has announced InfraCal 2. The lack of moving parts, a rugged metal case, and optional internal battery pack make the InfraCal 2 fixed filter infrared analyzer ideal for the range of conditions typically found in a field environment - at a price significantly lower than an FTIR spectrometer. Most analyses require minimal or no consumables reducing the cost per test. InfraCal 2 requires no scheduled maintenance or recalibation. The touch screen display allows a simple set up for quick operation along with an easy calibration wizard.
2.2.   Spectro Inc
  • FluidScan Oil Condition Monitor
  • FluidScan combo with SpectroVisc Q3000
  • Combo with Q3000 and Q5200 Trivector Mini-Lab
 
Spectro FluidScan FLSC 1000 / 1100 Oil Condition Monitor
 
Quantitative and qualitative infrared analysis wherever you need it. Spectro’s patented Direct Infrared (DIR) approach provides direct quantitative measurement of a lubricant’s condition. The Fluidscan Q1000 immediately detects lubrication contamination, degradation and cross contamination in mineral and synthetic engines, including gear, hydraulic, turbine and transmission oils as well as biodiesel and diesel blends.

It analyzes for TAN, TBN, oxidation, nitration, sulfation, additive depletion and incorrect (or mixup) lubricant within water content, soot and glycerin in addition to FAME in biodiesels.

Oil analysis, when you need it and where you need it, gives you the power to make immediate decisions. Spectro Inc.’s FluidScan® Q1000 and SpectroVisc Q3000 provide oil condition data including viscosity, acidity, oxidation and water or coolant contamination, in just a few minutes. Benefits include:

  • Convenience of on-site analyses
  • Immediate feedback on critical properties
  • Ease of use and no chemicals needed
  • Actionable information with pre-set alarm limits

Learn how the US Armed Forces use portable tools to keep their high-value assets running and download the case study and ROI analysis of the kits used for shipboard maintenance.
 
 
Spectro FluidScan 1000 (the yellow one) is a stand-alone performing instrument. Aside there is FluidScan 1100 (blue one) for use in combination with Spectro Q5200 Trivector MiniLab. The latter is also known as Emerson CSI 5200.
 
FluidScan 1100
Oil Condition Monitor
Combo-kit FluidScan 1000 + SpectroVisc 3000 Spectro Q5200 Trivector MiniLab (Microscope available)

3.       Electron Spin Resonance
 
OmniTek introduces brand new technology:
Micro
Electron Spin Resonance - Unlocking Free Radicals

Free radicals are highly reactive chemical species that govern many fundamental chemical processes in nature, most notably combustion and oxidation. Until now, direct measurement of the composition and concentration of free radicals has represented a challenge for chemists due to the complexity and expense of the necessary equipment. A new innovation in sensor design, the Micro Electron Spin Resonance spectrometer (Micro-ESR™), offers the exciting potential of measuring free radicals with an extremely compact, low cost and ruggedized device.
Micro-ESR™ enables new low-cost applications such as on-line measurement of lubricant breakdown in engines and machinery, on-line airborne particulates monitoring in diesel engine exhaust and even spin immunoassay medical diagnostics.
 
3.1.            Original study on engine lubricant
 
A study of engine oil from a Honda gasoline engine was performed with ESR. As the antioxidant package in the oil is depleted by oxidation, the intensity of the peroxy radical (RO2•) signal increases steadily from zero. This is the induction period. Also, the g-factor of the peroxy radical signal increase slightly as the hydrocarbon chains are broken down. When the oil is approaching the end of its useful life, the intensity of the peroxy radical signal rises dramatically and failure is imminent as shown in figure below.

 


3.2.            Marine oil investigation
 
A number of test have been performed on marine fuel to see time based changes in magnetic response. Typical changes are formation of Soot and presence of Vanadyl and Asphaltenes. The latter 2 are typical for fuel dilution.




3.3.           Experimental application: Oxidation in ester-based oils
 
Oxidation in used oils is predominantly monitored via FTIR according ASTM E2412. But in ester based oils this peak falls in same region as the ester peak itself. Hence analysis of oxidation is a troublesome task. ESR may give an answer to this tedious problem. As oxidation is promoted by free radicals ESR may pick up the signal yielding crisp graphics without signal blocking by other (dark) substances, as is usually the case with used engine oils.
 
Two images below show magnetic response as a function of oxidation in ester based oils. Top image is base oil, where only a few radicals are present. But after long exposure oxide radicals give a huge sharp peak.







3.4.   Instruments by Active Spectrum

ESR instruments are available for laboratory investigation as well for continuous production control. Most likely applications are:

•    Crude oil analysis:
      Asphaltene and vanadium content
•     Lubricants analysis:
      Oxidation of engine oil, hydraulic oil and turbine oil
•     Spin-trapping (PBN, TEMPOL, DMPO)
•     Shelf life of food products (vegetable oil, beer, wine)
•     Biodiesel oxidative stability
•     Detection of raw fuel dilution in marine engines
•     Thermal coking
•     Soot
•     Catalyst coking


Active Spectrum has ESR models available as Desktop model for the laboratory or Flow Through for continuous analysis.
Your application not listed here?
  Please contact us for discussing your products and applications.  
  • Low Resolution applications from Wilks IR
  • Oil Condition monitoring from Spectro Inc
  • Oil / Chemical analysis through Electron Spin Resonance from Active Spectrum
Former newsletters:

- #9: July 2013 - OmniTek U-VIsc series : Automated ASTM D445 Kinematic Viscometers
Other instruments from OmniTek
 
Physical properties Brands Systems
Kinematic Viscometers OmniTek Houillon , Ubbelohde
Rotational Viscometers ATS Rheosystems Black Pearl
Infra-Red Spectrometers Wilks IR
Spectro
ATR IR
Oil Condition spectrometer
Elemental Spectrometers Spectro Fuel: Spectroil M 
Oil: Spectro Q100
Particle Analyzers Spectro
V4L
LNF Q200
Filter Patch Scan
ED-XRF Spectrometers Xenemetrix Portable
Benchtop
Secondary target
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