GB2466802A - Measuring low levels of contaminants in fuels using Fourier Transform Infra red spectroscopy with dynamic reference analysis - Google Patents
Measuring low levels of contaminants in fuels using Fourier Transform Infra red spectroscopy with dynamic reference analysis Download PDFInfo
- Publication number
- GB2466802A GB2466802A GB0900195A GB0900195A GB2466802A GB 2466802 A GB2466802 A GB 2466802A GB 0900195 A GB0900195 A GB 0900195A GB 0900195 A GB0900195 A GB 0900195A GB 2466802 A GB2466802 A GB 2466802A
- Authority
- GB
- United Kingdom
- Prior art keywords
- sample
- additives
- components
- infra red
- contaminants
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000356 contaminant Substances 0.000 title abstract description 18
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 title abstract description 14
- 239000000446 fuel Substances 0.000 title abstract description 9
- 238000004458 analytical method Methods 0.000 title description 4
- 238000001228 spectrum Methods 0.000 abstract description 28
- 239000000654 additive Substances 0.000 abstract description 25
- 230000000996 additive effect Effects 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 238000005259 measurement Methods 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000002594 sorbent Substances 0.000 abstract description 8
- 230000009977 dual effect Effects 0.000 abstract description 4
- 239000012530 fluid Substances 0.000 abstract description 4
- 235000019387 fatty acid methyl ester Nutrition 0.000 abstract description 3
- 239000007790 solid phase Substances 0.000 abstract description 3
- 208000016444 Benign adult familial myoclonic epilepsy Diseases 0.000 abstract description 2
- 239000003225 biodiesel Substances 0.000 abstract description 2
- 238000010828 elution Methods 0.000 abstract description 2
- 208000016427 familial adult myoclonic epilepsy Diseases 0.000 abstract description 2
- ZGNITFSDLCMLGI-UHFFFAOYSA-N flubendiamide Chemical compound CC1=CC(C(F)(C(F)(F)F)C(F)(F)F)=CC=C1NC(=O)C1=CC=CC(I)=C1C(=O)NC(C)(C)CS(C)(=O)=O ZGNITFSDLCMLGI-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000383 hazardous chemical Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 25
- 238000011109 contamination Methods 0.000 description 3
- 239000013074 reference sample Substances 0.000 description 3
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Abstract
A process, and a sample handling system, used in conjunction with a mid infra red Fourier Transform Infra red (FTIR) spectrometer with a single or dual through flow cell, to enable the accurate measurement of specific contaminants and additives/components in fluids. The system creates its own continuous reference spectra after pumping the sample through a solid phase sorbent selected to absorb the contaminant or additive/component to be measured. The output of the sorbent is initially free of specific contaminants and/or additives/components. This output changes if specific contaminants and/or additives/components breakthrough the sorbent. The continuous dynamic reference spectra are compared with the spectrum from the sample thus enabling the required measurement to be made. The process eliminates the requirement for solvent washing or solvent elution, thus simplifying the process and avoiding the use of potentially hazardous chemicals. The process and system have particular application in measuring trace amounts of biodiesel (FAME), in aviation turbine fuels to high precision using an apparatus that can easily be used by non specialist staff at many points in the supply chain.
Description
Sampling apparatus and process for measuring low levels of contaminants, or additives/components, in fuels using FTIR with dynamic reference analysis
Description
In many industries, such as petroleum and especially when fuels are involved, there is often a requirement to quickly and frequently measure the presence of a known contaminant, an additive or component.
These fuels are made to strict specifications but on the way to their end use they pass through various multiproduct pipelines, storage containers and filtration systems. Allowed additives and/or components may be added initially or later in the supply chain. Finally the fuel may be commingled with other fuels of the same specification but from a different manufacturer or batch.
There are many analytical techniques available to make these measurements, however these are very costly, can be time consuming and require a trained chemist, thus making tests at a terminal, pipeline, fuel farm or depot not reasonably possible.
One technique, using the Fourier Transform lnfra red (FTIR) spectrometer, is easy to use and can provide a quick chemical fingerprint(spectrum) of a sample being analysed. The sample test is non-destructive and only requires a small sample. Unknown substances such as contaminants or additives/components are identified by comparison of the spectrum with reference spectra. Bespoke software presents the result of the analysis to the operator.
The ultimate performance of the FTIR in measuring the amount of contamination or additive present is therefore limited by knowledge of the unadulterated sample. In some industries, such as the petroleum industry, fluids are manufactured to a specification but will have a different spectrum, manufacturer to manufacturer or even batch to batch. For the detection of large levels of contaminants or additives a "typical" reference spectrum may be adequate, however accurate measurements, from low percentages down to ppm or mg/kg levels, need much better reference spectra. At point of use it will not be possible to have accurate reference spectra due to the use of multiproduct pipelines, commingling, use of additives and/or components, transport and storage practices.
Solid phase extraction is a technique used to concentrate contaminants or additives/components of interest up to a level that is required for further processing or measurements. The sample passed through a sorbant is usually discarded, and a solvent with more affinity to this contaminant or additive/component is used to recover the contaminant or additive/component of interest from the sorbant. This contaminant or additive/components, and often other additives with a similar spectrum, are then measured using an FTIR spectrometer by comparing the spectrum of the contaminant or additive/component with the solvent used. The disadvantage with this concept is the complexity of the sample handling system, the health and safety aspects of use and evaporation of solvents and the possibility of including interferences, such as the additives, in the measurement.
The invention eliminates the need for solvents and creates dynamic reference spectra for comparison against the sample spectrum thus allowing identification and level of the contaminant, additive/component to be measured.
An FTIR with a single or dual through flow cell is used in conjunction with a sample handling system and software to compare the sample and reference spectra, and make the required measurements. The use of a dual through flow cell allows spectra comparisons in parallel as against in series for the single through flow cell. For the single cell the spectrum of the sample is measured before the reference, although the reverse order is feasible.
The invention is a process and sample handling system to enable the accurate measurement of specific contaminants and additives/components in fluids. It uses an FTIR to compare the sample's spectrum with the spectrum of the fluid after it is pumped through a solid phase sorbent during the test cycle. It essentially creates a dynamic reference spectrum for the sample being tested, by selectively (and temporarily for some additives) removing the contamination and/or additive/component using a solid phase sorbent (from 100% absorbance to breakthrough during the test cycle) and comparing the resulting dynamically changing FTIR spectrum with the spectrum of the sample, in realtime, using a single or dual through flow FTIR cell. The real time processing of the sample during the test cycle allows the selective identification of additives and their elimination as potential interferences if required. The invention also encompasses a process that has eliminated the requirement for solvent washing or solvent elution, thus simplifying the process and avoiding the use of potentially hazardous chemicals.
The invention results from the requirement to measure trace amounts of biodiesel (FAME Fatty Acid Methyl Esters) in aviation turbine fuels to high precision at levels down to 30 mg/kg or ppm using an apparatus that could easily be used at many points in the supply chain.
Operational sequence for measuring a contaminant i) The sample is pumped or drawn from the sample container through the FTIR flow cell to flush and clean the pipework and the through flow cell.
ii) The sample is pumped or drawn from the sample container through the FTIR flow cell, the flow of the sample is stopped and its FTIR spectrum measured and recorded.
iii) The sample is pumped or drawn from the sample container through a cartridge containing a specifically selected sorbent. The output from the cartridge (reference sample) is passed through the FTIR flow cell. The flow of the reference sample is stopped at predetermined intervals so that a set of spectra from the FTIR can be recorded.
iv) The spectra change as the reference sample replaces the sample in the flow cell and as some known interferences (additives and components) breakthrough the sorbent v) The set of dynamic reference spectra are compared with the sample spectra.
vi) A reference spectrum is then chosen when interferences are judged to have broken through the sorbent and are part of the spectrum, but before the contaminant(or additive/component) to be measured breaks through.
vii) The comparison between the sample and chosen reference spectrum is then used to measure and report the level of contamination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0900195A GB2466802B (en) | 2009-01-08 | 2009-01-08 | Sampling apparatus and process for measuring low levels of contaminants, or additives/components, in fuels using FTIR with dynamic reference analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0900195A GB2466802B (en) | 2009-01-08 | 2009-01-08 | Sampling apparatus and process for measuring low levels of contaminants, or additives/components, in fuels using FTIR with dynamic reference analysis |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB0900195D0 GB0900195D0 (en) | 2009-02-11 |
| GB2466802A true GB2466802A (en) | 2010-07-14 |
| GB2466802B GB2466802B (en) | 2013-03-13 |
Family
ID=40379262
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB0900195A Active GB2466802B (en) | 2009-01-08 | 2009-01-08 | Sampling apparatus and process for measuring low levels of contaminants, or additives/components, in fuels using FTIR with dynamic reference analysis |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2466802B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2485766A (en) * | 2010-11-18 | 2012-05-30 | Michael John Sherratt | Contaminant detection using permittivity measurement and creation of a reference sample |
| US9194858B2 (en) | 2012-05-11 | 2015-11-24 | Polaris Sensor Technologies, Inc. | System for measuring the concentration of an additive in a mixture |
| US20210239610A1 (en) * | 2020-01-31 | 2021-08-05 | eralytics GmbH | Contamination analyser |
| US11255779B2 (en) * | 2017-09-06 | 2022-02-22 | Quantared Technologies Gmbh | Process for quantitative determination of fatty acid esters in fuels |
| CN115372306A (en) * | 2022-07-26 | 2022-11-22 | 中国科学院理化技术研究所 | Oil pollution analysis method based on infrared absorption spectrum fingerprint characteristics |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5889683A (en) * | 1996-04-22 | 1999-03-30 | Ismail; Ashraf A. | Method and apparatus for continuous oil monitoring and treatment |
| US20060137432A1 (en) * | 2004-12-29 | 2006-06-29 | Industrial Technology Research Institue | Process for collecting and concentrating trace organics in a liquid sample |
| EP2009434A2 (en) * | 2007-06-29 | 2008-12-31 | Delphi Technologies, Inc. | System and Methods for Determining a Concentration of Biodiesel in a mixture of Biodiesel and Petrodiesel |
| EP2028475A1 (en) * | 2006-06-12 | 2009-02-25 | Nippon Telegraph and Telephone Corporation | Chip for optical analysis |
-
2009
- 2009-01-08 GB GB0900195A patent/GB2466802B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5889683A (en) * | 1996-04-22 | 1999-03-30 | Ismail; Ashraf A. | Method and apparatus for continuous oil monitoring and treatment |
| US20060137432A1 (en) * | 2004-12-29 | 2006-06-29 | Industrial Technology Research Institue | Process for collecting and concentrating trace organics in a liquid sample |
| EP2028475A1 (en) * | 2006-06-12 | 2009-02-25 | Nippon Telegraph and Telephone Corporation | Chip for optical analysis |
| EP2009434A2 (en) * | 2007-06-29 | 2008-12-31 | Delphi Technologies, Inc. | System and Methods for Determining a Concentration of Biodiesel in a mixture of Biodiesel and Petrodiesel |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2485766A (en) * | 2010-11-18 | 2012-05-30 | Michael John Sherratt | Contaminant detection using permittivity measurement and creation of a reference sample |
| US9194858B2 (en) | 2012-05-11 | 2015-11-24 | Polaris Sensor Technologies, Inc. | System for measuring the concentration of an additive in a mixture |
| US11255779B2 (en) * | 2017-09-06 | 2022-02-22 | Quantared Technologies Gmbh | Process for quantitative determination of fatty acid esters in fuels |
| US20210239610A1 (en) * | 2020-01-31 | 2021-08-05 | eralytics GmbH | Contamination analyser |
| AT523446A1 (en) * | 2020-01-31 | 2021-08-15 | eralytics GmbH | Contamination analyzer |
| AT523446B1 (en) * | 2020-01-31 | 2023-06-15 | eralytics GmbH | contamination analyzer |
| CN115372306A (en) * | 2022-07-26 | 2022-11-22 | 中国科学院理化技术研究所 | Oil pollution analysis method based on infrared absorption spectrum fingerprint characteristics |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2466802B (en) | 2013-03-13 |
| GB0900195D0 (en) | 2009-02-11 |
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