Spotlight on Analytical Applications e-Zine - Volume 2

VOLUME 2

SPOTLIGHTON APPLICATIONS.FOR A BETTERTOMORROW.

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PerkinElmer

INTRODUCTION

PerkinElmer Spotlight on Applications e-Zine – Volume 2

PerkinElmer knows that the right training, methods, applications, reporting and support are as integral to getting answers as the instrumentation. That’s why PerkinElmer has developed a novel approach to meet the challenges that today’s labs face – that approach is called EcoAnalytix™, delivering to you complete solutions for your applications challenges.

In this effort, we are pleased to share with you our Spotlight on Applications e-zine, delivering a variety of topics that address the pressing issues and analysis challenges you may face in your application areas today.

Our Spotlight on Applications e-zine consists of a broad range of applications you’ll be able to access at your convenience. Each application in the table of contents includes an embedded link that will bring you directly to the appropriate page within the e-zine.

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CONTENTS

Energy• Biodiesel Blend Analysis by FT-IR (ASTM D7371 and EN 14078)

• Diamond ATR and Calibration Transfer for Biodiesel-Blend Analysis by ASTM D7371

• Simple Method of Measuring the Band Gap Energy Value of TiO2 in the Powder Form Using a UV/Vis/NIR Spectrometer

• Photovoltaic Silicon Impurity Analysis by ELAN DRC ICP-MS

Environmental• Analysis of Micronutrients in Soil Using AAnalyst 800 Atomic Absorption Spectrophotometer

• Determination of Oil and Grease in Water with a Mid-Infrared Spectrometer

• Characterization of Soil Pollution by TG-IR Analysis

• Ozone Precursor Analysis Using a TurboMatrix Thermal Desorption-GC System

Food & Beverage• Analysis of Organic Fertilizers for Nutrients with AAnalyst 800 Atomic Absorption Spectrophotometer

• Trace Elemental Characterization of Edible Oils with Graphite Furnace Atomic Absorption Spectrophotometer

• Determination of Nickel in Fats and Oils

• Analysis of Fish and Seafood with AAnalyst 800 Atomic Absorption Spectrophotometer for Trace Metals Contamination, in Accordance with AOAC Methods 999.10 and 999.11

Materials Characterization• Determining Protein Secondary Structure with Spectrum 100

• Study Rigid Amorphous Fraction in Polymer Nano-Composites by StepScan and HyperDSC

Pharmaceuticals• Evolved Gas Analysis: Residual Solvent Contamination Measured by Thermogravimetric

Analysis-Mass Spectrometry

• Evolved Gas Analysis: High Sensitivity Study of a Solvent of Recrystallization in a Pharmaceutical

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Introduction – FAME and FAME Blends

The increasing importance of sustainability in energy production has led to a global commitment to the use of fuels derived from renewable biological sources, such as biodiesel produced from plant crops. Biodiesel consists of fatty acid methyl esters (FAME) and is produced in a transesterification reaction as depicted in Figure 1. A range of feedstocks are used globally, including rapeseed, soy, sunflower, palm and jatropha.

FT-IR Spectroscopy

a p p l i c a t i o n n o t e

Authors

Ben Perston

Nick Harris

PerkinElmer, Inc. Seer Green, UK

Biodiesel Blend Analysis by FT-IR (ASTM D7371 and EN 14078)

Figure 1. Reaction scheme for the production of biodiesel.

Triglycerides from biological sourceR = C14–C18, 0–3 double bonds

MethanolBase Catalyst

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TSInfrared Spectroscopy

a p p l i c a t i o n n o t e

Authors

Ben Perston

Nick Harris

PerkinElmer, Inc. Seer Green, UK

Introduction

Biodiesel and Biodiesel-Blend Analysis

The need for sustainable fuel sources has led to an increasing global emphasis on fuels produced from renewable, biological sources. Biodiesel is one such fuel, and consists of fatty acid methyl esters (FAMEs) produced from vegetable oils or animal fats via a trans- esterification reaction. Biodiesel is seldom used neat (B100), typically being blended with fossil diesel at ratios from 5% v/v (B5) to 30%

v/v (B30). Verifying the FAME content of diesel-fuel blends is an important aspect of quality control and auditing of blending and distribution operations. Because FAME has a strong infrared absorption at 1745 cm-1 due to the ester carbonyl group, infrared spectroscopy is an excellent technique for this analysis, and there are EN and ASTM® standard test methods describing the procedure.1,2

The PerkinElmer® EcoAnalytix™ Biodiesel IR FAME Analyzer3 consists of a Spectrum™ 100 FT-IR spectrometer with an attenuated total reflection (ATR) accessory featuring either a diamond or zinc selenide (ZnSe) crystal. In addition to the Spectrum Express™ or Spectrum 10 software, which includes a dedicated biodiesel-analysis module and detailed standard operating procedures (SOPs), the system is provided with a “starter calibration”, covering the full range from 0% to 100% FAME. This application note describes how the supplied calibration can be optimized to give peak performance in a particular installation, without resorting to a full recalibration.

Diamond ATR and Calibration Transfer for Biodiesel-Blend Analysis by ASTM D7371

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Introduction

The measurement of the band gap of materials is important in the semi-conductor, nanomaterial

and solar industries. This note demonstrates how the band gap of a material can be determined from its UV absorption spectrum.

The term “band gap” refers to the energy difference between the top of the valence band to the bottom of the conduction band (See Figure 1); electrons are able to jump from one band to another. In order for an electron to jump from a valence band to a conduction band, it requires a specific minimum amount of energy for the transition, the band gap energy1,2. A diagram illustrating the bandgap is shown in Figure 1.

Measuring the band gap is important in the semiconductor and nanomaterial industries. The band gap energy of insulators is large (> 4eV), but lower for semiconductors (< 3eV). The band gap properties of a semiconductor can be controlled by using different semiconductor alloys such as GaAlAs, InGaAs, and InAlAs. A table of materials and bandgaps is given in Reference 1.

UV/Vis/NIR Spectrometer

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AuthorJayant Dharma PerkinElmer Technical Center

Aniruddha Pisal Global Application Laboratory PerkinElmer, Inc. Shelton, CT USA

Simple Method of Measuring the Band Gap Energy Value of TiO2 in the Powder Form Using a UV/Vis/NIR Spectrometer

Figure 1. Explanation of band gap.

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Photovoltaic Silicon Impurity Analysis by ELAN DRC ICP-MS

Rising energy and oil prices in light of the economic slowdown, and a heightened awareness of the environment, have led to an increase in global incentives for the diversification of energy sources and greater utilization of renewable energy segments.

With the increased interest in renewable energy, there are growing opportunities for photovoltaics (PV). According to market research, PV is expected to account for over 50% of the world’s total electricity generated by renewable energy sources by 2070. The PV market overall has grown to $19 billion globally and is predicted to continue over the next decade at over 30% per year. Wafers are the principal raw material used to produce solar cells, which are devices capable of converting sunlight into electricity. Today approximately 90% of the world-wide PV installations use mono- or multi-crystalline silicon wafers in the solar cells and silicon wafers represent half or more of the cost of silicon solar cells.

Case study

ICP-Mass Spectrometry

Jiabin Du, Huanhuan Pan Technology Center, LDK Solar Co., Ltd. Economic Development Zone Xinyu, Jiangxi 338032, China

Jianmin Chen and Wilson You Global Application Laboratory PerkinElmer, Inc. 710 Bridgeport Avenue, Shelton, CT USA

For more information about this story, please visit LDK Solar Limited at: http://www.ldksolar.com/index.html

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Introduction

Soil is used in agriculture, where it serves as the primary nutrient base for plants. Soil material is a critical component in the mining and construction industries. Soil serves as a foundation for most construction projects. Soil resources are critical to the environment, as well as to food and fiber production. Waste management often has a soil component. Land degradation is a human-induced or natural process which impairs the capacity of land to function. Soils are the critical

component in land degradation when it involves acidification, contamination etc. Soil contamination at low levels is often within soil capacity to treat and assimilate. Many waste treatment processes rely on this treatment capacity. Exceeding treatment capacity can damage soil biota and limit soil func-tion. Derelict soils occur where industrial contamination or other development activity damages the soil to such a degree that the land cannot be used safely or productively. The analysis of soils is an excellent measure of soil fertility. It is a very inexpensive way of maintaining good plant health and

Atomic Absorption

a p p l i c a t i o n n o t e

Author

Praveen Sarojam, Ph.D.

PerkinElmer Global Application Center Mumbai, India

Analysis of Micronutrients in Soil by Using AA 800 Atomic Absorption Spectrophotometer

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Introduction

The concentration of dispersed oil and grease (OG) is an important parameter for water quality and safety. OG in water can cause surface films and shoreline deposits leading to environmental degradation, and can induce human health risks when discharged in surface or ground waters. Additionally, OG may interfere with aerobic

and anaerobic biological processes and lead to decreased wastewater treatment efficiency. Regulatory bodies worldwide set limits in order to control the amount of OG entering natural bodies of water or reservoirs through industrial discharges, and also to limit the amount present in drinking water.

OG in water is commonly determined by extraction into a non-polar, hydrocarbon- free solvent followed by measurement of the infrared absorption spectrum of the extract. The absorption between 3000 and 2900 cm-1 by C-H groups in the OG is correlated to the concentration of OG. There are several standard test protocols based around this methodology,1–4 most commonly using 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113) or tetrachloromethane. However, these solvents are known ozone-depleting compounds, and under the Montreal Protocol, the use of CFC-113 was phased out by 1996 and the use of tetrachloromethane will become illegal in 2010.

Infrared Spectroscopy

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Author

Aniruddha Pisal

PerkinElmer, Inc. Shelton, CT 06484 USA

Determination of Oil and Grease in Water with a Mid-Infrared Spectrometer

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There are many scenarios in which soil can become contaminated by hydrocarbon products. Leakage from fuel storage tanks or transfer lines as well as storm water runoff from vehicle washing areas are just two examples. In environmental monitoring or land reclamation, therefore, it is important to test soil for contamination. Total petroleum hydrocarbon (TPH) testing by solvent extraction and infrared spectroscopy is a sensitive method, but has a considerable burden of sample preparation. A gas chromatographic analysis of the extract can provide even greater sensitivity and more detailed compositional information, but further increases the time required for the analysis.

Thermogravimetric analysis coupled to infrared spectroscopy (TG-IR) can provide detailed information about the amount and nature of the pollution, while requiring no sample preparation at all. This application note illustrates the kind of data that can be obtained with a modern TG-IR system.

Experimental

A soil sample was obtained and mixed with diesel fuel at a concentration of about 10% m/m. 17 mg of the soil was transferred to the crucible of a PerkinElmer® TGA 4000, coupled to a PerkinElmer Spectrum™ 100 infrared spectrometer by the TL 8000 transfer line with a 10-cm gas cell. The transfer line and gas cell were heated to 280 °C to avoid any risk of condensation of heavier organic compounds. The purge gas through the TGA was nitrogen at flow rate of 20 mL/min with a balance purge of 40 mL/min. This combined rate of 60 mL/min was kept constant through the transfer line and cell. The temperature was increased from 30 to 800 °C at a constant rate of 20 °C/min. Infrared spectra over the range 4000–600 cm-1 were collected every 12 s at 8 cm-1 resolution (co-adding four interferometer scans for each spectrum). Pyris™ software was used to control the TGA, while TimeBase™ was used for collection and analysis of the time-resolved IR data.

Characterization of Soil Pollution by TG-IR Analysis

Thermogravimetric Analysis – Infrared Spectroscopy

a p p l i c a t i o n n o t e

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Whitepaper Gas Chromatography

Authors

Graham Broadway

Andrew Tipler

PerkinElmer, Inc. Shelton, CT USA

In the United States, the Clean Air Act of 1970 gave the U.S. Environmental Protection Agency (EPA) responsibility for maintaining clean air for health and welfare. Six parameters are measured routinely in ambient air: SOx, NOx, PM10 (particulate matter less than 10 microns), Pb, CO and ozone. In the 1990 Clean Air Act Amendments, Title 1 expanded the measurements in air to include volatile organic compounds (VOCs) that contribute to the formation of ground-level ozone. These parameters are measured in urban areas that do not meet the attainment goals for ozone, as shown in Figure 1. These measurements are implemented through a program known as Photochemical Assessment Monitoring Stations (PAMS).

This program has been in place in the U.S. for a number of years, and in 2008 the National Ambient Air Quality Standards (NAAQS) for Ground-Level Ozone was reduced to 0.075 ppm for an 8-hour period.1 The U.S. EPA predicts that a large number of counties will violate the 2008 stan-dard2 (Figure 1). Similar recommendations have also been made in Europe. Following the 1992 Ozone Directive and United Nations Economic Commission for Europe’s protocol on controlling VOC emissions, a European ozone precursor priority list was established by Kotzias et al.3 and subse-quently modified by the EC 2002/3/CE directive.

Ozone Precursor Analysis Using a Thermal Desorption-GC System

Figure 1. Areas expected to violate the 2008 Ozone Standard.

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Introduction

The fertilizer industry helps to ensure that farmers have the nutrients they need to grow enough crops to meet the world's requirements for food, feed, fiber and energy. Nutrients in manufactured fertilizers are in the form that can be absorbed readily by the plants. All of these nutrients exist in nature, but the quantities are not sufficient to meet the needs of our growing, urbanized population. Soils may be naturally low in nutrients, or they may become deficient due to nutrient removal by crops over the years without replenishment – or when

high-yielding varieties are grown that have higher nutrient requirements than do local varieties. All of the essential nutrients are important but in varying quantities. Macronutrients (N, P, K, Ca, Mg, etc.) are needed by plants in large quantities. The “primary nutrients” are nitrogen, phosphorus and potas-sium. Today, sulphur is also considered a key macronutrient. Macronutrients include both primary and secondary nutrients. Micronutrients (or “trace elements”) (Fe, Mn, Zn, Cu, Ni, etc.) are required in very small amounts for correct plant growth. They need to be added in small quantities when they are not provided by the soil. Every plant nutrient, whether required in large or small amounts, has a specific role in plant growth and food production. One nutrient cannot be substituted for another. For example, potassium activates more than 60 enzymes (the chemical substances that govern life and play a vital part in carbohydrate and protein synthesis). It improves a plant's water regime and increases tolerance to drought, frost and salinity. Plants that are well supplied with potassium are less affected by disease. Magnesium is the central constituent of chlorophyll, the green pigment in leaves that functions as an acceptor of the energy supplied by the sun: 15-20% of the magnesium in a plant is found in the green

Atomic Absorption

a p p l i c a t i o n n o t e

Author

Praveen Sarojam, Ph.D.

PerkinElmer Global Application Center Mumbai, India

Analysis of Organic Fertilizers for Nutrients with AAnalyst 800 Atomic Absorption Spectrophotometer

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Introduction

The determination of the inorganic profile of oils is important because of the metabolic role of some elements in the human organism. On the one hand, there is knowledge of the food's nutritional value, which refers to major and minor elements. On the other hand, there is the concern to verify that the food does not contain some minerals in quantities toxic for the health of the consumers, regardless whether this presence of minerals is naturally occurring or is due to contamination during the

production processes. Oil characterization is the basis for further nutritional and food technological investigations such as adulteration detection1. The most common adulteration is an addition of a cheaper vegetable oil to expensive oil. Authenticity is a very important quality criterion for edible oils and fats, because there is a big difference in prices of different types of oil and fat products. Adulteration detection is possible by determining the ratio of the contents of some chemical constituents and assuming these ratios as constant for particular oil. In regard to adulteration detection, approaches based on atomic spectroscopy can be attractive2. The quality of edible oils with regard to freshness, storability and toxicity can be evaluated by the determination of metals. Trace levels of metals like Fe, Cu, Ca, Mg, Co, Ni and Mn are known to increase the rate of oil oxidation. Metals like As, Cd, Cr, Se etc. are known for their toxicities. The development of rapid and accurate analytical methods for trace elements determination in edible oil has been a challenge in quality control and food analysis. However, sample pretreatment procedures are required in order to eliminate the organic matrix. These include wet, dry or microwave digestion, dilution with organic solvent and extraction methods3. The content of metals and their species (chemical forms) in edible seed oils depends on several factors. The metals can be incorporated into the oil from the soil or be introduced during the production process. Hydrogenation of edible seed oils and fats has been

Atomic Absorption

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Author

Praveen Sarojam Ph.D.

PerkinElmer, Inc. Global Application Center Mumbai

Trace Elemental Characterization of Edible Oils with Graphite Furnace Atomic Absorption Spectrophotometer

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Scope

Triglyceride-based vegetable fats and oils can be trans-formed through partial or complete hydrogenation to fats and oils of greater molecular weight. The hydro- genation process involves sparging the oil at high temperature and pressure with hydrogen in the presence of a catalyst, typically a powdered nickel compound. Atomic Absorption Spectrometry is commonly used to estimate the amount of nickel left in the vegetable oils.

Typical Analytical Procedure

Materials and Methods

The following reagents and equipment are used for the measurement:

• Atomicabsorptionspectrometer

• Nickelmetal

• Conc.nitricacid

• Conc.hydrochloricacid

• Doubledistilledwater

Atomic Absorption

a p p l i c a t i o n B R i E F

Determination of Nickel in Fats and Oils

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Introduction

Increased knowledge about the nutrient content of biological organisms is essential for a thorough understanding of ecological stoichiometry and nutrient transport in and among ecosystems. As a result of water pollution in coastal area, many problems in food safety like heavy metal accumulation have been recog-nized in farmed fish, which is one of the important fish-ery food resources. The heavy metals accumulated in fish not only have a bad influence on fish but they also affect the health of human beings through the food chain. It is pointed out that remarkable heavy metals were contained in fish meals that are used as major raw materials for aquaculture feeds. The Itai-itai disease of the Toyama Jintsu River area in Japan was the documented case of mass cadmium poisoning. Itai-itai disease is known as one of the Four Big Pollution Diseases of Japan.

Atomic Absorption

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Author

Praveen Sarojam, Ph.D.

PerkinElmer, Inc. Shelton, CT 06484 USA

Analysis of Fish and Seafoods with AAnalyst 800 Atomic Absorption Spectrophotometer for Trace Metal Contamination, in Accordance with AOAC Methods 999.10 and 999.11

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Although crystallography and NMR are the primary tools for determining geometrical protein structures there are significant limitations in the range of

proteins that these techniques can address. FT-IR gives less detailed information but it has some important advantages. It can be applied to any protein, it requires a relatively small sample, and the measurements can be made in solution. The applications for FT-IR include determining secondary structure of novel proteins, identifying conformations in formulations, measuring the kinetics of conformational changes with temperature or other perturbations, and investigating protein-ligand interactions.

The information about secondary structure is contained in the shape of the amide-1 band in the IR spectrum. This requires careful measurement as it overlaps with the water band at 1640cm-1 and water vapor absorptions. Both transmission and ATR techniques can be used, but adsorption of the protein on to the crystal surface is a potential problem with ATR. For transmission measurements pathlengths between 6 and 10μm are generally used.

The secondary structure is analyzed as a mixture of different amounts of various sub-structures such as α-helix and β-sheet, each of which has characteristic absorptions. In curve-fitting and deconvolution approaches the amide-1 band is analyzed explicitly as the superposition of such bands. Chemometric approaches use a library of spectra from proteins of known secondary structure.

Determining Protein Secondary Structure with Spectrum™ 100

FT-IR Spectroscopy

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Author

Richard SpraggPerkinElmer, Inc.Chalfont RoadSeer GreenBeaconsfieldBuckinghamshire, UK

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Introduction

It is known that there is a rigid amorphous fraction (RAF) in semicrystalline polymers. The RAF exists at the interface of crystal and amorphous phase as a result of the immo-bilization of a polymer chain due to the crystal. There is debate on whether the crystal melts first and then RAF devitrifies or the RAF devitrifies before the crystal melts. It can

not be answered easily because these two things often happen in the same temperature range. Also, the RAF fraction sometimes exists at the surface of silica nanoparticles in the polymer silica nanocom-posites material. However, unlike semi-crystalline polymers, the silica nanoparticle does not undergo any transition at the temperature when RAF devitrifies. So polymer silica nanocomposites offer a good opportunity to study the devitrification of RAF1.

Some studies have indicated a second glass transition from RAF in dynamic measurements. To the author’s best knowledge, there is no evidence of a second Tg in polymer nanocomposites from DSC experi-ments. In order to identify RAF in DSC, absolute heat capacity measurement is very important. A formula has been well established for the determination of RAF in semicrystalline polymers based on accurate heat capacity measurement as described by Wunderlich, see2 for a review.

Here, heat capacity measurement has been performed in order to detect a possible second Tg on nanocom-posites of polymethyl methacrylate (PMMA) with silicon oxide nanoparticles of different shape. StepScan™ DSC was used for determination of precise heat capacity and HyperDSC® to prevent degradation and identify devitrification of the RAF at elevated temperatures.

Differential Scanning Calorimetry

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Author

Christoph SchickUniversity of RostockInst. of PhysicsUniversitätsplatz 3, 18051 Rostock, Germany

Study Rigid Amorphous Fraction in Polymer Nano-Composites by StepScan and HyperDSC

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Introduction

Thermogravimetric analysis (TGA) of mate-rials is commonly used to measure weight loss from a sample as it is heated or held isothermally. In the pharmaceutical industry, many materials show weight losses associated with the loss of solvent/ water, desolvation or decomposition of the sample. This information is then used to assess the purity and stability of the material and its suitability for use. The TGA gives a quantitative measure of mass lost from the sample, but it does not provide information on the nature of the products that are lost from the sample, and this information is often required for complete characterization.

Coupling a mass spectrometer (MS) to a TGA allows evolved gases to be analyzed and identified, delivering this additional valuable information.

Thermogravimetric Analysis – Mass Spectrometry

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Evolved Gas Analysis: Residual Solvent Contamination Measured by Thermogravimetric Analysis-Mass Spectrometry

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Introduction

Thermogravimetric analysis (TGA) of materials is commonly used to measure weight loss as a sample is heated or held isothermally. In the pharmaceutical industry, materials often show weight losses associated with the loss of solvent/water, desolvation or decomposition of the sample. This information is then used to assess the purity and stability of the material and its suitability for use. The TGA gives a quantitative measure of mass lost from the sample, but it does not provide information on the nature of the products that are lost from the sample, and this information is often required for complete characterization.

Coupling a mass spectrometer (MS) to a TGA allows evolved gases to be analyzed and identified giving this additional valuable information.

Thermogravimetric Analysis – Mass Spectrometry

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Evolved Gas Analysis: a High Sensitivity Study of a Solvent of Recrystallization in a Pharmaceutical

Instrumental Setup

All of the TGA systems supplied by PerkinElmer (Pyris™ 1 TGA, STA 6000 and TGA 4000) can be easily interfaced to MS systems. PerkinElmer can supply systems with either the PerkinElmer Clarus® MS or with a Hiden Analytical MS. In this study, a Pyris 1 TGA interfaced to a Hiden Analytical HPR-20 MS was used.

Figure 1. Pyris 1 TGA is shown interfaced to a HPR-20 MS (left) and a Clarus 600 MS (right).

Typical applications of TG-MS include:

• Detectionofmoisture/solventlossfromasample(e.g.lossondryingordehydrationofapharmaceutical)

• Thermalstability(degradation)processes

• Studyreactions(e.g.polymerizations)

• Analysisoftracevolatilesinasample(e.g.volatileorganiccompound(VOC)testing)

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• Atomic Absorption (AA)• Elemental Analysis• Gas Chromatography (GC)• GC Mass Spectrometry (GC/MS)• Hyphenated Technology• ICP Mass Spectrometry (ICP-MS)• Inductively Coupled Plasma (ICP-OES & ICP-AES)• Infrared Spectroscopy (FT-IR & IR)• LIMS & Data Handling• Liquid Chromatography (HPLC & UHPLC)• Mass Spectrometry• Raman Spectroscopy• Thermal Analysis• UV/Vis & UV/Vis/NIR