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Fresh - vol 6 2009

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009 INDIA ANALYTICAL SCIENCES It is our immense pleasure that we are receiving your feed backs and suggestions through this FRESH communications. We are trying our level best to incorporate different products and applications related to its usage in various industries and market segments. Our efforts are towards to keep you updated about the solutions available from The newer techniques of analysis to get the precise and accurate results through the methodology used by experts and users worldwide are being synopsized for your quick glance. Your particular interest in products or solutions can be directed to us by email any time. We shall be pleased to interact with you for any techno commercial assistance possible from our end.
- High resolution measurement of optical filters in NIR Team Marketing-India - Analysis of tartarates in wine using FTNIR spectrometer - Automated Thermal Desorber and GCMS for the - PerkinElmer Optima ICP 7000 a solution to pharmaceutical sample analysis for inorganic element

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES Gaining high resolution measurements of optical filters in the NIR range with the LAMBDA 1050 UV/Vis/NIR Christopher Lynch PerkinElmer Life andAnalytical Sciences 710 Bridgeport AvenueShelton, CT 06484 USA The most common measurement for Author Christopher Lynch PerkinElmer the analysis, a polarizer should be optical filter quality testing is done in Life and Analytical Sciences 710 added to allow the specific angle of transmission mode with the results Bridgeport Avenue Shelton, CT 06484 polarization to be measured. This typically displayed in %T. The USA. All modern high performance could range from S to P polarization or measurement may be performed at spectrophotometers use reflective any angle between.
any angle of incidence required by the gratings to disperse the source energy filter design. The angle of incidence into specific wavelengths. This process Optical filter types and design light used can range from normal to will create strongly polarized light requirements vary widely from simple greater than 60° with 45° being one of which will be used for sample neutral density filters to the most the most common requirements. analysis.For this reason, to achieve the complex multi layer bandpass designs. When measurements are to be truest results a depolarizer should be All have specific design requirements performed at angles other than used at angles higher than 8° to and all require spectroscopic analysis normal, typically considered to be measure a sample under random to validate designs and for quality between 5°- 8°, polarization affects polarization conditions. If specific control in manufacturing. need to be considered.
angles of polarization are required by

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES Typical design requirements of several common types of filters are shown in Figures 1 and 2 Figure 1. Typical filter design requirements.
Figure 2. Typical bandpass filter response characteristics.
Optical filters have many functions, nm: A gridless PMT for detec- tion in Key to a successful analysis is including color correction, used to the UV/Vis, a high sensitivity Peltier translating the specifica- tion improve color balance in many optical cooled InGaAs detector for use in the requirements into the method setup systems, to neutral density filters that 800-2600 nm region and a Peltier parameter used by the produce specific reduction in the level cooled PbS detector for the range from spectrophotometer. Choosing high of transmitted light. Thin film filters 2500-3300 nm. This offers the best resolution and a very small data used in laser based systems have more combination of scanning speed and interval for a filter type which has no demanding requirements typically photodynamic range that can be spectral features will simply waste requiring very narrow bandpass and achieved on a given sample type.
valuable time. In general the resolution very high out-of-band blocking. The needs to be 4-10 times smaller than characterization of these diverse optical In determining the best method for the the bandpass of a given component to filter types is critical from design analysis of a specific filter several provide sufficient data to validate a through manufacturing, providing factors need to be considered. The validation of a specific design and the design specification will provide the necessary means to perform QC/QA of majority of the information necessary Photodynamic range is another finished products. for a spectroscopic analysis. important consideration. The level of Wavelength range, bandpass, absorbance of a given material will The LAMBDA™ 1050 utilizes three transmission and out of band blocking impact how a method is developed detectors for optimum energy will all be defined and need to be and how fast a sample can be scanned. detection across the entire wavelength taken into consideration.
A notch filter with very high absorbing range of the instrument, 175-3300 re- quirements may require reference

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES beam attenuation to be used to requirement. A filter of this type will achieve accurate data on the true require slit resolution of 0.25 nm to performance of a filter. Simply achieve sufficient resolution to determine its characteristics. The knowing the design goal of the LAMBDA 1050 using an InGaAs component will determine the detector in the NIR region allows both method details for a successful high resolution and wider analysis to be performed.
photodynamic range improving both signal- to-noise and speed of analysis over a conventional PbS detector. With the proper selection of operating Figure 3. 1 nm Laser line filter measured with parameters completed and baseline 0.25 nm resolution on a LAMBDA 1050 using data acquired, sample measurement an InGaAs detector can now be performed. Figure 3 shows the typical response of a laser line filter. Excellent signal-to-noise is seen in the spectra even at very high resolution.
Figure 4 shows the same filter measured on a typical spectrophotometer using a PbS (Lead Measuring a laser bandpass filter with a Sulfide) detector in the NIR region. Poor center wave- length of 1064 nm and a signal-to-noise is due to low sensitivity Figure 4. 1 nm Laser line filter measured with bandpass of 1 nm is a common of the detector at very high resolution.
0.25 nm resolution on a LAMBDA 950 using a PbS detector.

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES Tartrates are used extensively in the Type 1 sample spectra (based on wine industry to clear the 'muddiness' calcium tartrate) are shown in Figure or sediment before bottling (materials 1. The spectra are similar; the variation used in this process are called in baseline indicating a difference in '?nings'). This application example particle size distribution between the describes the use of NIR to discrimi- two samples which can be removed by nate between two typical samples, converting to a second derivative as based on calcium tartrate and shown in Figure 2. It is also easier to potassium bitartrate. see the bands due to the calcium tartrate itself in the second derivative Figure 1: Sample spectra based on calcium tartrate.
Why choose NIR for this application? rather than the water bands which There are many different types of dominate Figure 1. ?nings used in the beer, cider and Type 2 samples (based on a potassium wine making industries. These range bitartrate/calcium tartrate mixture) are from aluminosilicates to gelatin, egg shown in Figure 3. Note the strong white, ?sh glue and polyvinyl- band at around 4700 cm-1 indicative polypyrrolidone or polyclar. Since many of the ?nings are the bi-products of other processes, they are often of Figure 2: Second derivative of sample spectra based on calcium tartrate.
extremely variable quality. For It is a simple task to create a short example, particle size distribu- tion COMPARE™ library and use it to verify varied widely from sample to sample. the identi?cation of test samples. This NIR re?ectance is an ideal method for was done for the ?nings samples, see ?nings analysis since no sample table 1. The results for a test sample of preparation is involved (other than type 1 (batch 5412) and type 2 (batch transferring a few grams of sample to 5431) indicate that the task of a glass vial), and both chemical and separating type 1 and type 2 samples Figure 3: Sample spectra based on potassium bitartrate/calcium tartrate.
physical property information is is easily accom- plished. Resolution, intensity, noise and water blanking Compare – 5412.SP
COMPARE ?lters were switched on to Correlation Factor minimize unwanted spectral and sample Four samples were provided for analysis. Two of type 1 (calcium tartrate based) and two of type 2 (potassium bitartrate/calcium tartrate mixture). The samples were prepared for analysis by placing a few grams of sample into a glass vial. NIR spectra of Compare – 5431.SP
the four samples were generated using a PerkinElmer FT-NIR System equipped with in-board Re?ection Accessory. Typical scan conditions:– 11000-3800 cm , 8 cm resolution, 16 scans. Spectrum 400 FTIR/FTNIR

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES Analysis of Volatile Organic Compounds by ATD-GCMS Automated thermal desorber (ATD) has been widely used for air quality monitoring in a confined places and for outdoor. Volatile organic compounds (VOC) are common Desorber, Clarus Gas Chromatograph compounds analyzed using ATD and Clarus Mass Spectrometer (MS), hyphenated with gas chromatograph the system provides outstanding (GC) and gas chromatograph-mass analytical performance as well as spectrometer (GCMS). This brief paper several unique features to simplify and outlines the conditions of the VOC speed analysis. Thermal desorbers with analysis with ATD. TurboMatrix PPC incorporate a powerful dry-purge Thermal Desorbers can solve problems technique that allows for analysis and provide answers for difficult under extreme levels of applications in many industries. humidity/moisture, while a unique Thermal desorption is instrumental for capability of the Clarus GC/MS offers monitoring environmental levels of the benefits of both full scan and organic pollutants and simplifies many single ion monitoring simultaneously routine determinations of volatiles in within a single analytical run. products such as disc drives and wafers in semiconductor manufacture, polymers, pharmaceuticals, foods and Instrument used was Clarus 600 GCMS with direct injection with Helium as carrier from ATD model Air toxics analysis
Turbomatrix 650 with cold trap and The PerkinElmer Air Toxics Analyzer NIOSH 2549 mix bed tube. integrates several analytical techniques Chromatograms in sequence of time into a single, unified system solution, performing tube-based sampling in accordance with established methodologies such as U.S. EPA ATD and GCMS were demonstrated to Method TO-17. Tube-based sampling be capable of analyzing volatile offers greater convenience as well as organic substances for environmental some analytical advantages over emission, occupational hazardous traditional canister-based analysis. chemical exposure and indoor air Comprised of a TurboMatrix Thermal quality monitoring.

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES Determination of metal impurities in pharmaceuticalsamples by Inductive Coupled Plasma Optical Emission Spectrometer (ICP-OES) Application Specialist (Atomic Spectroscopy), PerkinElmer Technical Centre, Mumbai (India) infestations. The suitable method for the analysis of these samples was defined by the PerkinElmer Optima 7000 ICP spectrometer. The sample preparation involved digestion procedure. The convention method of digestion was causing the loss of elements due to open vessel. PerkinElmer Multiwave 3000 microwave digestion enabled the faster digestion without loss of element in matrix. The study carried out to find out impurities in some of the Standard and sample preparation: pharmaceutical samples The samples 1.Standard solutions are prepared in selected for the analysis are: 2% Nitric Acid solution. 2.Sample preparation: Samples were Fig. 2 Multiave 3000 digested by using Microwave digestion used for short-term treatment of system (Multiwave 3000) as per the active duodenal ulcer in adults.
method mentioned in table 1. The multiwave represents a microwave based sample preparation system treatment of dyspepsia, peptic ulcer allows the rapid and complete wet- disease (PUD), gastroesophageal reflux chemical decomposition of organic disease (GORD/GERD) and Zollinger- and inorganic sample materials in Ellison syndrome. Esomeprazole closed TFM or quartz glass tube provides improved efficacy, in terms of reaction vessels at high pressure and stomach acid control, over racemic high temperature. Weight taken Reagents used 3. Sevelamer Hydrochloride: Sevelamer Hydrochloride is indicated After digestion program is complete, for the control of hyperphosphataemia Esomeprazole 0.0853 g clear solutions obtained were in adult patients receiving transferred in standard volumetric haemodialysis or peritoneal dialysis.
flasks, volume was made up to 25 ml and analysis was carried out.
Albendazole is a member of the benzimidazole compounds used as a drug indicated for the treatment of a variety of worm

HUMAN HEALTH ENVIRONMENTAL HEALTH VOLUME 6 June 2009INDIA ANALYTICAL SCIENCES Recovery study: 0.5 mg/l of mix 1. Complete digestion of pharmaceutical samples can be carried by Multiwave standard solution spiked in a 0.10 gm digestion system without any loss of elements. It is programmable, safe and easy to of Albendazole sample and results found are showing following recovery. 2. From the observed results it is concluded that the analysis of pharmaceutical sample can be carried out by the ICP-OES for most of the metals at very low level Omeprazole Esomeprazole

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