Infrared Spectroscopy

  

Infrared Spectroscopy- Chemical Composition and Identification of Polymers and Organic Compounds

   
             FT-IR, Fourier Transform Infrared Spectroscopy, is an exceptional means for the profiling and screening of sample compounds. FT Infrared Spectroscopy testing is used to identify the chemical compounds in a wide range of products, including coatings, foods, paints, pharmaceuticals, consumer products, and polymers, to name a few. FT Infrared Spectroscopy is a useful analytical device for the detection of functional groups and describing covalent bonding data.
          In addition, FT Infrared Spectroscopy testing is useful in the determination and identification of all kinds of inorganic and organic compounds, identification of compounds in mixtures, as well as chromatographic effluents, functional groups of organic materials, and the molecular makeup of surfaces. Other FT Infrared Spectroscopy testing applications include impurities screening, contamination identification, gas calibration, and both qualitative and quantitative scans. In other words, FT Infrared Spectroscopy is a robust real-time monitoring methodology for the quantification and detection of multiple compounds in a simultaneous manner.  
             Normally, FT Infrared Spectroscopy equipment and systems do not need to be calibrated. Calibration is not required due to the use of a standards library that includes calibrated infrared spectra stored on the hard disk drive of the system (or instrument) computer. Basically, the FT Infrared Spectroscopy testing system transmits an IR (infrared) beam of light through an area that is to be analyzed, then captures this beam after passing through the area and finally generates a full infrared spectrum of the light, resulting in the identification of the materials present and allows for the concentration to be identified.

Helium Mass Spectrometer Leak Detector

The VS PR02 is a portable Helium Mass Spectrometer Leak Detector with a fully integrated DS 42 rotary vane primary pump. This powerful instrument is extremely easy to use, without sacrificing valuable functionality.

Ø                  Features

Ø                  Totally automatic startup and tuning/calibration routine

Ø                  Touch screen with intuitive menu structure make it is easy to navigate

Ø                  High clarity, wide angle, TFT color display provides excellent visibility

Ø                  High Test Port Pressure allows short cycle times, and detection of large leaks

Ø                  High Sensitivity (5 x 1012 MDL) meets the most stringent test requirements

Ø                  High Helium Pumping Speed ensures fast response and cleanup

Ø                  New spectrometer optimizes sensitivity and mass separation

Ø                  Multiple language and units capability facilitates worldwide use

Ø                  Compact, lightweight design enables easy transporting of instrument

Ø                  Automatic test cycle sequencing with selectable roughing and test times

Ø                  3 leak rate set points, 1 pressure set point, and 1 audible leak rate alarm

Ø                  Set points w/ selectable greater than or less than settings

Ø                  Turbo High Vacuum Pump is totally maintenance free.

Ø                  Protection from air inrushes caused by power failures and possible operator errors.

Ø                  Split Flow function allows accurate testing of vacuum process systems

Ø                  Useful for sniffing and/or vacuum applications, to measure or locate leaks

Ø                  Specifications

Ø                  Primary pump DS 42, 2 m3/hr (34 l/m)

Ø                  Minimum Detectable Leak 5 x 10 12 mbar l/s, atm cc/sec, 5 x 1013 Pa m3/sec

Ø                  Maximum Test Pressure 13 mbar, 10 Torr, 1330 Pa

Ø                  He Pumping Speed (fine test) 1.8 l/s

Ø                  Calibration routine Automated or Manual, to Internal or External leak

Ø                  Background suppression Pushbutton initiated Auto Zero, and Auto Zero < Zero

Ø                  User Interface High Clarity, Color Display, TFT Touch Screen

Ø                  Selectable languages English, French, German, Japanese, Korean, Mandarin, Spanish

Ø                  Automated Cyclin Programmable Rough Time, Test Time, Reject Set points

Ø                  Set Points 5 Set points, N/O or N/C; 3 Leak Rate, 1 Pressure, 1 Audio

Ø                  Response time <0.5 sec

Ø                  Communications Interface RS 232 isolated@ 9600 baud (DB9)

Ø                  Conformance Standards UL/CSA, CE

Ø                  Weight 38 kg (83 lbs)

Ø                  Size, mm (in) 567 (22.3) L, 396 (15.6) W, 441 (17.4) H

Ø                  Power Requirements 100 VAC, 50 Hz, or 115 VAC, 60 Hz, 20 A

Ø                  Max. Branch Circuit Breaker: 20A w/ motorrated delay

Chemical Testing to Know Exactly What You Have

Let the chemical testing services at Laboratory Testing Inc. determine the composition or elemental make-up of your metals and other materials. Our chemists analyze metals, powdered metals, ores, ferroalloys, composites, ceramics, aerospace and nuclear materials and more using chemical testing services by instrumental methods and classical wet chemistry.

Our chemical testing equipment performs carbon, sulfur, nitrogen, oxygen and hydrogen determination and provides Atomic Emission Spectroscopy (AES), ICP-AES, ICP-MS and Energy Dispersive X-ray Spectrometry (EDS) capabilities. Trace elemental analysis is performed using ICP spectrometers with detection limits in the "parts per million" range for many metals. Our chemical testing lab has the capability to process work with limited sample weight or specialized requirements.

Laboratory Testing Inc. also performs chemical testing services on metals to determine susceptibility to corrosion using methods such as passivation, humidity, salt spray and salt fog corrosion testing. RoHS Compliance Testing is provided to meet the restrictions against hazardous substances sold or used in the European Union.

 

A history of mass spectrometry in IOCB

·              A history of mass spectrometry at IOCB started in the early sixties of the last century when the first mass spectrometer was purchased. Two mass spectrometers MX-1303 were imported from the Soviet Union due to Prof. František Šorm, a former director of IOCB. Both instruments were initially located in the Institute of Physical Chemistry, Czechoslovak Academy of Sciences in Praha - Vinohrady. One instrument was operated by Dr. Vladimír Hanuš, the second one by

·              Dr. Ladislav Dolejš from IOCB. In 1967 one MX-1303 has been moved to IOCB in Praha-Dejvice. Under Dr. Dolejš supervision mass spectra of many compounds of natural as well as synthetic origin were measured. The MX-1303 had a heated-reservoir inlet designed for the analysis of petroleum products; the upper mass limit was ~600 Da with the resolution of 450. The mass spectra were recorded using a strip-chart recorder. The scanning was slow and analyses were sometimes difficult to reproduce, however, mass spectrometry has proven competent for structure elucidation of organic substances. Numerous quality and so far cited publications focused on mass spectrometry of naturally occurring compounds, particularly alkaloids, were published at that time.

·              A new mass spectrometer MS902 (Associated Electric Industry) was purchased in 1969. At that time it was probably the best mass spectrometer on the market. This high-resolution double focusing instrument had a maximum resolution of 70 000 and was capable to measure ion masses with accuracy below to 3 ppm. The instrument equipped for electron ionization possessed an inlet for gas chromatograph, though only with packed columns at that time. The GC/MS instrumentation enabled expansion of pheromone chemistry and identification of volatile compounds from plants and insect.

·              The mass spectra were plotted on UV-sensitive paper at three different sensitivities. To make nice-looking spectra for publications, the peak intensities were manually measured using a ruler and processed by one of the first computers in IOCB. MS902 was located in the basement of the IOCB main building, room 3.

Spectrophotometer Components

How the NMR Spectrometer works
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Wholesale JK VS 722N Visible
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PM-IRRAS Method for Infrared Spectrometry

1          There are several methods used in the process of infrared spectrometry. They are typically used for analyzing single continuous layers of molecules that are suspended on liquid or reflective substance.

2          Most methods for this process are highly sensitive and very precise in terms of the surface they cover to make necessary measurements in an upright condition. Certain devices used for some methods are comprised of technological angular configuration that enables simple adjustments to different angles and a setup time that is more efficient.
3          The first FT-IR method for infrared spectrometry is the PM-IRRAS or Polarization Modulation-Infrared Reflection-Adsorption Spectroscopy which is highly specific on surfaces and has the ability to detect chemical compositions of films from a surface forming two bodies of common boundary down to single molecular films of thick quality. This kind of technique enables a better detection on measurements from the air water boundary as well as detecting substrates. When the indications of PM-IRRAS position and intensity changes, it can then be utilized to gather molecular absorption and desorption kinetics and behavior, shifting of phase, molecular coating, hydrogen bonds, hydration, and the different reactions of the surface in a thin film.

FTIR Spectrum

 
Situation:

Polyamide pellets were mixed with a UV inhibitor for manufacturing purposes. After a while, the surface of the pellets began to produce a thin white residue. Presumably, it was the UV inhibitor that has “blossomed” to the pellet’s exterior, but to further analyze the matter and make a precise conclusion regarding the condition of the pellets and the cause of the white residue, an FTIR Spectrum analysis has to be taken.

In order to further comprehend on the given situation, the people behind the analysis need to determine important factors—the kind of technique they would need to conduct and the polymers and chemicals involved.

The pellets producing the white residue as well as the polyamide pellets and UV inhibitor were placed on a test by means of FTIR Spectrum. It seems to show that the thin white residue is an Amine stabilizer that was stuck. The pellets were also observed using a microscope, its surface also showed the same residue and was later found out that both residues are similar in characteristics. It was identified to be a hindered Amine UV stabilizer.

It appears from the FTIR spectrum that the UV stabilizer was unsuccessfully   mixed together with the polymer material, thus, it drifted to the pellet’s surface and same thing happened when it was formed in to the final result of the mixture. The cause improper result is either the poor blending of the additives to the polymer or it might be that the wrong UV stabilizer was used.

Conclusion: Through this analysis, the client determined that it was the poor process of mixing the UV stabilizer to the polymer that has caused the result. By means of analyzing the FTIR Spectrum, they found out that they need to be more meticulous and detailed when using the polymer additives in order to avoid problems like this.

infrared radiation in IR Spectrometry

 

In IR Spectrometry, light of longer wavelengths which is usually invisible to human eye is used to recognize and name the elements that a certain material is comprised of. In some cases, especially on a crime scene investigation, this method is uses to determine a specific composition of a certain material found by knowing how it responds when there is interaction with light, or the light it produces when exposed to radiation or when it is burned.

In Physics, the universe is filled with small band in the electromagnetic radiation spectrum that results to visible light.The higher end of the spectrum that is used in methods of IR Spectrometry in microwaves is 1mm and down to about 800 nanometers. The molecules have the ability to absorb enough amounts of IR radiation with different wavelengths depending on the type of the material. This process is possible because molecules have the natural capacity of to be intact as it moves even when energy is applied to the sample material.

To further analyze the absorption pattern that is taking place, spectrometers can recognize the compounds and elements that are present in the specified sample of material and can even lead to a conclusion of the whole material. One should be familiar in organic chemistry to operate any instruments for this process as well as to further understand any information that is shown in the result. Organic Chemistry courses in numerous universities incorporates a portion of spectrometry particularly IR spectrometry.

For some laboratory testing, particularly with Innova Tech Labs, their website shows in a simple tutorial and some practical details  how Fourier Transformation IR spectrometry process goes, how useful the process is identifying materials that are unknown, residues, fibers, measurement of oxidation levels, curing process of a polymer, and etc.

The first scanning mass spectrometer

                   Thomson was, however, dissatisfied with his photographic method of recording the parabolas. The problem was that lightweight species penetrated the film deeply, causing a disproportionate amount of blackening, compared to heavier ions, and thus quantitative estimations of beam intensities were impossible. 
             He eventually solved this problem by constructing a slit in the tube where the photographic film would normally sit. Behind this slit was a Faraday cup that collected any ion charge. The intensity of the charge was estimated by noting the time it took for a charged electroscope to discharge. By slowly changing the magnetic field, the ion beams could be positioned, one at a time, on the slit, and their intensities noted. From his results he plotted intensity against relative mass: Thomson had invented the world's first scanning mass spectrometer. ⁸   

          Leaving his protégé, Francis William Aston, to concentrate on determining the isotopic constitution of any elements he had to hand, Thomson decided to record the mass spectra of some chemical compounds, including slightly impure CO, HCl and carbonyl chloride (COCl₂). The first of these is shown in  Fig 1. ⁸  Note the abundant peak of the undissociated molecule, together with the smaller peaks at 12 (carbon) and 16 (oxygen) - an astonishingly good match with today's bar-graph version (see Fig 2).  The spectra of these species represented the conclusion of Thomson's work with positive rays and mass spectrometry. Administration (as master of Trinity College, Cambridge, from 1918) took the place of bench-work.                     
        However, he published, initially in 1913, his thoughts on the potential of his technique to chemical analysis. ⁹  These he amplified in his 1921 book  Rays of positive electricity and their application to chemical analyses. 

           We can, by measuring the parabolas, determine the masses of all the particles in the [discharge] tube, and thuidentify the contents of the tube as far as this can be done by a knowledge of the atomic and molecular weights of all its constituents. When we find a new line we know at once the atomic or molecular weight of the particle that produced it.
           [In conventional forms of spectroscopy] the presence of one gas is apt to swamp the spectrum of another.This is not the case to anything like the same extent with the positive rays; the presence of other gases is a matter of comparatively little importance.  
          The method is more sensitive than that of [other forms of] spectrum analysis. With. [my] apparatus the helium in 1 cm³ of air [ie, about 3 x 10^-6 cm³] could be detected with great ease.

Mass Spectrometry

·        What is the most common reagent you find in all types of laboratories?

You got the answer right! Water.

Water can be found in every type of laboratory, be it medical, pharmaceutical, chemistry, and microbiological. These laboratories need different levels of water purity for the different levels of sensitivity of their analysis and experiments.
Water Purification Process

·        The whole water purification process is long and involves many steps. The most common purification processes used to decontaminate water of its impurities are the following:

·        Distillation – Water is heated and the condensed vapor is trapped and collected. However, there are still impurities found in distilled water such as silica, ammonia, and other organic compounds. Storage of distilled water is also important to keep it from contamination.
2. Reverse osmosis – Osmosis is the movement of water from higher concentration to lower concentration as caused by the osmotic pressure. In reverse osmosis, water is passed through a filter using a higher pressure than the osmotic pressure to separate the impurities.
3. Ion exchange – This process removes various metals particularly heavy metals present in water however ion exchange will retain microorganisms.
4. Activated carbon – Also known as adsorption media and works effectively removing chlorine in water by “a catalytic mechanism and dissolved organics by adsorption”.
5. Ultraviolet disinfection – It uses ultraviolet light which is a powerful sterilizing agent to kill bacteria and other microorganisms.
6. Filtration – Filtration of water using different pore sizes ensure that other impurities which are of various sizes are also trapped and the water is uncontaminated.

·        These are just some of the water purification methods used and their progressions differ from system to system as well.

There are also different types of water according to their use in the laboratory. This is dependent on the purification process and more importantly on the quality of water that results after the long and careful methods of purification.

Types of Laboratory-grade Water

According to the Genetic Engineering and Biotechnology News, there are three main types of laboratory-grade water:

o Type 1. This is the ultrapure water which has very low levels of ions (resistivity 18.2), organic molecules, bacteria, and particles. It is commonly manufactured by combining purification technologies such as activated carbon, reverse osmosis, ion-exchange resins, ultraviolet photo-oxidation, filtration processes, and electrodeionization. It is used for analytical methods such as high-pressure liquid chromatography (HPLC), gas chromatography, and inductively-coupled plasma mass spectrometry (ICP-MS). However, it is very important for reagent as well as equipment preparation for molecular biology and cell culture.