Analysis of moisture is becoming increasingly important to many different industries
Many of these reasons require not only a precise, but also accurate reading
For years, most moisture analyses have been conducted on a semi-quantitative or even qualitative level
This document outlines the five main steps for developing an analytical HPLC method: 1) selecting the initial HPLC method and conditions, 2) selecting the initial chromatographic conditions, 3) optimizing selectivity, 4) optimizing system parameters, and 5) validating the method. Key aspects of each step are discussed, including selecting the type of chromatography, column, detector, and mobile phase based on the analytes. The goal is to develop a validated method that provides adequate resolution and selectivity within a desired analysis time.
Gas chromatography is a technique used to separate and analyze volatile compounds. It works by injecting a sample into a column through which an inert gas flows, carrying the separated components out at different rates depending on their interactions with the stationary phase coating the column. The separated components are detected to produce a chromatogram showing peaks that can be analyzed to determine the identity and quantity of each component in the original sample.
Reference standards in Pharmaceutical Industriesbhavanavedantam
This presentation is brief introduction about reference standards that are using in pharmaceutical industries for calibration of different instruments, methods and pharmaceutical chemicals...
This document discusses HPLC columns, including:
1. Silica is commonly used as the surface for HPLC columns, with silanols bonding to the surface. Pore size and surface area impact analyte retention and loading capacity.
2. Column particle sizes have decreased over time from 100 μm to below 2 μm, increasing theoretical plate counts. Column dimensions and particle sizes are selected based on the application.
3. Pore size should be larger than analyte molecules to allow entry without hindrance. Pore sizes of 60-80Å or 95-300Å are recommended for small molecules or proteins, respectively.
The document discusses primary and secondary standards. A primary standard is a compound that is sufficiently pure such that a standard solution can be directly prepared by weighing and diluting the compound. It must be easy to obtain, purify, dry, store, and test for impurities. Sodium carbonate, sodium tetraborate, and benzoic acid are provided as examples of primary standards for acid-base, complex formation, and oxidation-reduction reactions respectively. A secondary standard is a substance whose concentration has been determined by comparison to a primary standard solution, rather than direct weighing. Hydrated salts generally do not make good standards due to drying difficulties, but some like sodium tetraborate do not effloresce and can
This document discusses various detectors used in gas chromatography including the flame ionization detector, thermal conductivity detector, flame photometric detector, photoionization detector, atomic emission detector, sulfur chemiluminescence detector, nitrogen chemiluminescence detector, and others. For each detector, it provides information on the basic principle of operation, components, applications, and limitations. The document focuses on explaining how each detector is able to detect and measure compounds eluting from the gas chromatography column based on their specific characteristics.
This document provides an overview of coulometry, which is an electroanalytical technique used for quantitative analysis. There are two forms of coulometry: controlled-potential coulometry and controlled-current coulometry. Both techniques involve completely oxidizing or reducing an analyte and measuring the total charge passed to determine the amount of analyte. Controlled-potential coulometry applies a constant potential while controlled-current coulometry applies a constant current. Factors like electrolysis time, electrode area, and stirring rate affect the analysis. Coulometry is used to quantify both inorganic and organic analytes.
This document outlines the five main steps for developing an analytical HPLC method: 1) selecting the initial HPLC method and conditions, 2) selecting the initial chromatographic conditions, 3) optimizing selectivity, 4) optimizing system parameters, and 5) validating the method. Key aspects of each step are discussed, including selecting the type of chromatography, column, detector, and mobile phase based on the analytes. The goal is to develop a validated method that provides adequate resolution and selectivity within a desired analysis time.
Gas chromatography is a technique used to separate and analyze volatile compounds. It works by injecting a sample into a column through which an inert gas flows, carrying the separated components out at different rates depending on their interactions with the stationary phase coating the column. The separated components are detected to produce a chromatogram showing peaks that can be analyzed to determine the identity and quantity of each component in the original sample.
Reference standards in Pharmaceutical Industriesbhavanavedantam
This presentation is brief introduction about reference standards that are using in pharmaceutical industries for calibration of different instruments, methods and pharmaceutical chemicals...
This document discusses HPLC columns, including:
1. Silica is commonly used as the surface for HPLC columns, with silanols bonding to the surface. Pore size and surface area impact analyte retention and loading capacity.
2. Column particle sizes have decreased over time from 100 μm to below 2 μm, increasing theoretical plate counts. Column dimensions and particle sizes are selected based on the application.
3. Pore size should be larger than analyte molecules to allow entry without hindrance. Pore sizes of 60-80Å or 95-300Å are recommended for small molecules or proteins, respectively.
The document discusses primary and secondary standards. A primary standard is a compound that is sufficiently pure such that a standard solution can be directly prepared by weighing and diluting the compound. It must be easy to obtain, purify, dry, store, and test for impurities. Sodium carbonate, sodium tetraborate, and benzoic acid are provided as examples of primary standards for acid-base, complex formation, and oxidation-reduction reactions respectively. A secondary standard is a substance whose concentration has been determined by comparison to a primary standard solution, rather than direct weighing. Hydrated salts generally do not make good standards due to drying difficulties, but some like sodium tetraborate do not effloresce and can
This document discusses various detectors used in gas chromatography including the flame ionization detector, thermal conductivity detector, flame photometric detector, photoionization detector, atomic emission detector, sulfur chemiluminescence detector, nitrogen chemiluminescence detector, and others. For each detector, it provides information on the basic principle of operation, components, applications, and limitations. The document focuses on explaining how each detector is able to detect and measure compounds eluting from the gas chromatography column based on their specific characteristics.
This document provides an overview of coulometry, which is an electroanalytical technique used for quantitative analysis. There are two forms of coulometry: controlled-potential coulometry and controlled-current coulometry. Both techniques involve completely oxidizing or reducing an analyte and measuring the total charge passed to determine the amount of analyte. Controlled-potential coulometry applies a constant potential while controlled-current coulometry applies a constant current. Factors like electrolysis time, electrode area, and stirring rate affect the analysis. Coulometry is used to quantify both inorganic and organic analytes.
Karl Fischer titration is a technique used to determine the water content in a sample. It works based on a reaction between water, sulfur dioxide, iodine, and an alcohol solvent. The endpoint is detected electrometrically. Some advantages are its high accuracy, ability to measure small amounts of water, and suitability for automation. It has a variety of applications in industries like plastics, pharmaceuticals, chemicals and more.
1. The document discusses troubleshooting strategies and common problems in HPLC.
2. It outlines a 5-step troubleshooting strategy of identifying the problem, determining the cause, isolating the exact cause, rectifying the problem if possible, and returning the system to use.
3. Common problems discussed include issues with the mobile phase, pump, injector, detector, and peaks/baseline, along with potential causes and solutions for each.
Introduction to gas Chromatography
,Principle of gas chromatography
Instrumentation of gas Chromatography
Type of detectors of gas chromatography
Advantages of gas chromatography
Disadvantages of gas chromatography
Applications of gas chromatography
The document discusses Karl Fischer titration (KFT) techniques for determining water content. It describes two common methods - volumetric KFT, which uses a burette to dispense Karl Fischer reagent, and coulometric titration, which generates iodine electrochemically. The key reaction involves iodine oxidizing an intermediate alkylsulfite to alkylsulfate, consuming water. Factors like solvent choice, water content, pH, and kinetics are discussed. The document also outlines how volumetric and coulometric titrators function and how the endpoint is detected.
This document discusses the importance of instrumental analysis methods in conjunction with traditional analytical techniques. It provides an overview of fundamental principles of instrumental measurements and how they can be applied to specific chemical analyses. Key aspects covered include the differences between analytical techniques and methods, important terms, developing a method of analysis by defining the problem, sampling, sample preparation, performing measurements, and comparing results to standards. The overall message is that instrumental methods provide modern solutions to analytical problems when used appropriately alongside traditional methods.
Analytical method development and validation of tapentadol hcl by rp hplcShweta Tiwari
This document summarizes the development and validation of an analytical method using reverse phase high performance liquid chromatography (RP-HPLC) to analyze tapentadol hydrochloride in tablet dosage forms. The method utilized a C18 column with a mobile phase of methanol and water, detected the analyte at 272 nm. Validation of the method showed good linearity, precision, accuracy, specificity. The developed and validated method can be used for quality control of tapentadol hydrochloride tablet formulations.
The document discusses the flame ionization detector (FID). It explains that the FID is one of the most sensitive and reliable detectors for gas analysis. It works by ionizing solutes in a flame, with electrons emitted attracted to a positive electrode to produce a current. The FID is responsive only to organic compounds with carbon atoms, making it useful for analyzing volatile solutes in water without pretreatment. It also lists key characteristics of the FID like being rugged, sensitive, having a wide dynamic range, and being destructive. Example applications mentioned include analyzing purge gases and impurities in gas supplies for various industrial processes.
Moisture content determination by karl fischer titrationDaman Pandey
Karl Fischer titration is a method for determining water content. It works by titrating a sample with Karl Fischer reagent, which contains iodine, sulfur dioxide, and a base, causing a reaction where water and iodine are consumed in a 1:1 ratio. There are two main types - volumetric titration for higher water content samples, and coulometric titration for very low water content samples, which generates iodine via electrolysis. Factors like sample pH, impurities, and atmospheric moisture can affect the results. The method is accurate, specific to water, and suitable for solids, liquids, and gases.
The document discusses bioanalytical sample preparation. It begins with an introduction to sample preparation as an essential step in the bioanalytical process. Sample preparation techniques discussed include protein precipitation, liquid-liquid extraction, and solid phase extraction. Protein precipitation involves denaturing proteins to isolate analytes. Liquid-liquid extraction uses differential solubility to separate analytes between immiscible liquid phases. Solid phase extraction selectively retains analytes on a solid sorbent under specific conditions. The document provides details on each technique's principles, steps involved, advantages, and disadvantages.
General considerations and method development in ce,ChowdaryPavani
This document provides an overview of capillary electrophoresis (CE). It defines CE, describes its principle and instrumentation. CE involves separating components of a sample based on their differential rate of migration in an applied electric field. Key points covered include electrophoretic mobility, electroosmotic flow, sample introduction techniques, and common applications such as protein, DNA and pharmaceutical analysis. CE provides high resolution separations due to its small capillary diameter and long separation length.
This document provides an overview of HPLC methodology and validation requirements. It discusses the key components of an HPLC test procedure including system suitability testing, relative response factors, and the validation parameters of specificity, linearity, accuracy, precision, LOD/LOQ, and robustness. Validation requirements depend on whether the method is compendial or non-compendial, with full validation needed for non-compendial methods. System suitability criteria and validation acceptance limits are outlined for various analytical techniques like assay, impurities testing, and dissolution.
The document discusses hyphenated techniques, specifically liquid chromatography-nuclear magnetic resonance (LC-NMR). It begins by introducing hyphenated techniques as the combination of two analytical methods, usually a separation technique coupled with a spectroscopic technique. It then describes LC-NMR in more detail, explaining how it works to separate components with liquid chromatography and then uses NMR for identification. Key aspects covered include instrumentation, modes of data acquisition (continuous flow, stopped flow, time sliced), and advantages such as automation, reproducibility, and simultaneous separation and quantification.
This document discusses supercritical fluid chromatography (SFC). SFC uses supercritical fluids like carbon dioxide as the mobile phase. Carbon dioxide is most widely used as it is non-toxic, inexpensive, and has a critical temperature and pressure that are easily reached. SFC works on the principles of adsorption and partition chromatography. It can be used to analyze and purify low to moderate weight compounds, including chiral separations. SFC instrumentation includes pumps to deliver the mobile phase, an oven for temperature control, various injectors, columns, a backpressure regulator, and detectors. SFC finds applications in fields like pharmaceuticals and has advantages over HPLC like using less toxic solvents.
This document discusses regulatory perspectives on metabolite identification and safety testing. It notes that metabolite toxicity profiles may differ from parent drugs, so safety testing is necessary. Metabolites of concern are those that are unique to or disproportionately present in humans. Safety testing should be conducted early in development to avoid delays. The guidance recommends identifying differences between species' metabolism early. If safety testing is warranted, studies should be completed before large clinical trials. The document reviews safety evaluation approaches and timelines to consider for metabolite testing throughout the drug development process.
Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized without decomposition. The sample is injected into a heated injector port and carried by an inert gas through a long column containing a stationary liquid or solid phase. Components of the sample partition between the stationary and mobile phases and elute from the column at different retention times, allowing for separation. Common detectors measure properties like conductivity or combustion byproducts to identify separated components. GC is useful for analyzing volatile organic compounds like natural products, foods, drugs, and more.
This document summarizes a webinar about oxygen analysis using the rapid OXY cube. It discusses the advantages of high temperature oxygen determination at 1500°C compared to lower temperature methods. The rapid OXY cube allows matrix-independent oxygen analysis using glassy carbon tubes. It also features backflush chromatography to remove interfering gases and ensure accurate results. Examples are given showing the instrument's use for coal, fuels, liquids and other samples.
Karl Fischer titration is a technique used to determine the water content in a sample. It works based on a reaction between water, sulfur dioxide, iodine, and an alcohol solvent. The endpoint is detected electrometrically. Some advantages are its high accuracy, ability to measure small amounts of water, and suitability for automation. It has a variety of applications in industries like plastics, pharmaceuticals, chemicals and more.
1. The document discusses troubleshooting strategies and common problems in HPLC.
2. It outlines a 5-step troubleshooting strategy of identifying the problem, determining the cause, isolating the exact cause, rectifying the problem if possible, and returning the system to use.
3. Common problems discussed include issues with the mobile phase, pump, injector, detector, and peaks/baseline, along with potential causes and solutions for each.
Introduction to gas Chromatography
,Principle of gas chromatography
Instrumentation of gas Chromatography
Type of detectors of gas chromatography
Advantages of gas chromatography
Disadvantages of gas chromatography
Applications of gas chromatography
The document discusses Karl Fischer titration (KFT) techniques for determining water content. It describes two common methods - volumetric KFT, which uses a burette to dispense Karl Fischer reagent, and coulometric titration, which generates iodine electrochemically. The key reaction involves iodine oxidizing an intermediate alkylsulfite to alkylsulfate, consuming water. Factors like solvent choice, water content, pH, and kinetics are discussed. The document also outlines how volumetric and coulometric titrators function and how the endpoint is detected.
This document discusses the importance of instrumental analysis methods in conjunction with traditional analytical techniques. It provides an overview of fundamental principles of instrumental measurements and how they can be applied to specific chemical analyses. Key aspects covered include the differences between analytical techniques and methods, important terms, developing a method of analysis by defining the problem, sampling, sample preparation, performing measurements, and comparing results to standards. The overall message is that instrumental methods provide modern solutions to analytical problems when used appropriately alongside traditional methods.
Analytical method development and validation of tapentadol hcl by rp hplcShweta Tiwari
This document summarizes the development and validation of an analytical method using reverse phase high performance liquid chromatography (RP-HPLC) to analyze tapentadol hydrochloride in tablet dosage forms. The method utilized a C18 column with a mobile phase of methanol and water, detected the analyte at 272 nm. Validation of the method showed good linearity, precision, accuracy, specificity. The developed and validated method can be used for quality control of tapentadol hydrochloride tablet formulations.
The document discusses the flame ionization detector (FID). It explains that the FID is one of the most sensitive and reliable detectors for gas analysis. It works by ionizing solutes in a flame, with electrons emitted attracted to a positive electrode to produce a current. The FID is responsive only to organic compounds with carbon atoms, making it useful for analyzing volatile solutes in water without pretreatment. It also lists key characteristics of the FID like being rugged, sensitive, having a wide dynamic range, and being destructive. Example applications mentioned include analyzing purge gases and impurities in gas supplies for various industrial processes.
Moisture content determination by karl fischer titrationDaman Pandey
Karl Fischer titration is a method for determining water content. It works by titrating a sample with Karl Fischer reagent, which contains iodine, sulfur dioxide, and a base, causing a reaction where water and iodine are consumed in a 1:1 ratio. There are two main types - volumetric titration for higher water content samples, and coulometric titration for very low water content samples, which generates iodine via electrolysis. Factors like sample pH, impurities, and atmospheric moisture can affect the results. The method is accurate, specific to water, and suitable for solids, liquids, and gases.
The document discusses bioanalytical sample preparation. It begins with an introduction to sample preparation as an essential step in the bioanalytical process. Sample preparation techniques discussed include protein precipitation, liquid-liquid extraction, and solid phase extraction. Protein precipitation involves denaturing proteins to isolate analytes. Liquid-liquid extraction uses differential solubility to separate analytes between immiscible liquid phases. Solid phase extraction selectively retains analytes on a solid sorbent under specific conditions. The document provides details on each technique's principles, steps involved, advantages, and disadvantages.
General considerations and method development in ce,ChowdaryPavani
This document provides an overview of capillary electrophoresis (CE). It defines CE, describes its principle and instrumentation. CE involves separating components of a sample based on their differential rate of migration in an applied electric field. Key points covered include electrophoretic mobility, electroosmotic flow, sample introduction techniques, and common applications such as protein, DNA and pharmaceutical analysis. CE provides high resolution separations due to its small capillary diameter and long separation length.
This document provides an overview of HPLC methodology and validation requirements. It discusses the key components of an HPLC test procedure including system suitability testing, relative response factors, and the validation parameters of specificity, linearity, accuracy, precision, LOD/LOQ, and robustness. Validation requirements depend on whether the method is compendial or non-compendial, with full validation needed for non-compendial methods. System suitability criteria and validation acceptance limits are outlined for various analytical techniques like assay, impurities testing, and dissolution.
The document discusses hyphenated techniques, specifically liquid chromatography-nuclear magnetic resonance (LC-NMR). It begins by introducing hyphenated techniques as the combination of two analytical methods, usually a separation technique coupled with a spectroscopic technique. It then describes LC-NMR in more detail, explaining how it works to separate components with liquid chromatography and then uses NMR for identification. Key aspects covered include instrumentation, modes of data acquisition (continuous flow, stopped flow, time sliced), and advantages such as automation, reproducibility, and simultaneous separation and quantification.
This document discusses supercritical fluid chromatography (SFC). SFC uses supercritical fluids like carbon dioxide as the mobile phase. Carbon dioxide is most widely used as it is non-toxic, inexpensive, and has a critical temperature and pressure that are easily reached. SFC works on the principles of adsorption and partition chromatography. It can be used to analyze and purify low to moderate weight compounds, including chiral separations. SFC instrumentation includes pumps to deliver the mobile phase, an oven for temperature control, various injectors, columns, a backpressure regulator, and detectors. SFC finds applications in fields like pharmaceuticals and has advantages over HPLC like using less toxic solvents.
This document discusses regulatory perspectives on metabolite identification and safety testing. It notes that metabolite toxicity profiles may differ from parent drugs, so safety testing is necessary. Metabolites of concern are those that are unique to or disproportionately present in humans. Safety testing should be conducted early in development to avoid delays. The guidance recommends identifying differences between species' metabolism early. If safety testing is warranted, studies should be completed before large clinical trials. The document reviews safety evaluation approaches and timelines to consider for metabolite testing throughout the drug development process.
Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized without decomposition. The sample is injected into a heated injector port and carried by an inert gas through a long column containing a stationary liquid or solid phase. Components of the sample partition between the stationary and mobile phases and elute from the column at different retention times, allowing for separation. Common detectors measure properties like conductivity or combustion byproducts to identify separated components. GC is useful for analyzing volatile organic compounds like natural products, foods, drugs, and more.
This document summarizes a webinar about oxygen analysis using the rapid OXY cube. It discusses the advantages of high temperature oxygen determination at 1500°C compared to lower temperature methods. The rapid OXY cube allows matrix-independent oxygen analysis using glassy carbon tubes. It also features backflush chromatography to remove interfering gases and ensure accurate results. Examples are given showing the instrument's use for coal, fuels, liquids and other samples.
This document provides an introduction and overview of gas liquid chromatography (GLC) and high performance liquid chromatography (HPLC). It defines chromatography as a technique that separates components of a mixture based on differences in affinity for a stationary and mobile phase. GLC uses an inert gas as the mobile phase and a liquid stationary phase, while HPLC uses high pressure to push a liquid mobile phase through a column. The document describes the basic instrumentation, principles, and applications of these techniques.
Gas chromatography is a common type of chromatography used in analytical chemistry for separating and analyzing compounds that can be vaporized without decomposition.
methods for continues emission gas monitoringwaleedElazab
This document discusses factors to consider when choosing a continuous emission gas monitoring (CEM) system. It covers compliance with legislation, suitable analytical methods like in-situ, dilution probe, and extractive, appropriate analytical techniques for different gases, correct system design including sample extraction, transport, conditioning, and calibration. Key aspects of CEM system design include sample probe, heated transfer line, moisture measurement, water and acid removal, and calibration with certified gases. The goal is to select a reliable, cost-effective system that provides accurate emission measurements compliant with regulations.
Gas testing is required to ensure work areas are safe. There are three main types of gas tests - flammable, toxic/harmful, and oxygen content. Proper gas detection equipment must be calibrated and functional, with the tester knowledgeable about safe gas levels. Locations must be carefully checked, as gases can accumulate at different levels, and frequent testing may be needed when work is occurring.
This document provides an overview of gas chromatography. It discusses the basic principles and components of gas chromatography including the stationary and mobile phases, how samples are injected and separated in the column based on their partitioning properties. Key components like the carrier gas, temperature control, detectors, and columns are described. The document outlines some parameters used to evaluate chromatography performance and lists common applications of gas chromatography in fields like pharmaceutical analysis, food testing, and environmental analysis.
Chromatographic Analysis of Natural Gas Liquids, sherry petrochemicalsherrylabs
The document discusses chromatographic analysis of natural gas liquids performed by Sherry Laboratories. Sherry Laboratories is an industry leader in independent third-party testing with 10 laboratories providing accredited analytical testing and technical expertise. The document focuses on Sherry's hydrocarbon laboratory and reference standards division, describing the analytical methods, sampling, transportation, and chromatographic analysis used to test natural gas and liquid hydrocarbon mixtures.
This document discusses gas chromatography apparatus and applications. It describes the key components of a GC system including the carrier gas supply, sample injection system, column, column thermostating, and detectors such as thermal conductivity and flame ionization. It also discusses stationary phases, qualitative and quantitative analysis applications, calibration with standards, and internal standard methods. Quantitative GC analysis is based on comparing analyte peak heights or areas to calibration standards to obtain concentration.
Gas chromatography is a technique used to separate and analyze mixtures of substances. It works by vaporizing the sample and carrying it by an inert gas through a column coated with a stationary liquid or solid phase. Components in the sample partition between the mobile and stationary phases and exit the column at different retention times, producing separated peaks that can be analyzed. Key aspects of gas chromatography include the carrier gas, injection system, columns, temperature control, detectors, and data recording systems. Common detectors include the thermal conductivity detector, flame ionization detector, and electron capture detector. Gas chromatography is useful for analyzing volatile and thermally stable compounds.
Karl fischer titration is an analytic system to determine the trace amount of water in solid, gases and liquids. It is a very efficient and accurate technique. In this presentation we go deeper about this titration system.
1. Gas chromatography and liquid chromatography techniques such as HPLC are commonly used to characterize and study protein pharmaceuticals. HPLC methods like reverse phase HPLC can separate proteins based on hydrophobic interactions.
2. Other analytical techniques used include spectroscopy, electrophoresis, and mass spectrometry which provide information on protein structure, purity, quantity and degradation.
3. The selection of technique depends on the desired information and factors like resolution, sensitivity, sample requirements and throughput. Together these analytical approaches support protein quality control and characterization.
Gas chromatography (GC) is a technique used to separate and analyze compounds that can be vaporized without decomposition. It works by carrying a gas sample mixture through a column via an inert carrier gas, separating the compounds based on their interactions with the column's stationary phase. The separated compounds then exit the column and are detected, allowing for qualitative and quantitative analysis. Key components of a GC system include an injection port, column housed in an oven, detector, and recorder. Common applications are separation of lipids, drugs, pollutants, and more.
NATURAL CONVECTIVE HEAT TRANSFER BY Al2O3 &PbO NANOFLUIDSAlagappapandian M
In this presentation related about natural convective heat transfer incresed by using different nano particles. in this fluid is called nanofluids. Nanofluids improve the heat transfer rate of base fluid.
Gas chromatography is an analytical technique used to separate and analyze chemical compounds. It involves vaporizing a sample and injecting it into a column with a gaseous mobile phase. Components are separated based on how they partition between the mobile and stationary phases. The separated components exit the column and are detected, producing a chromatogram. Key advantages are its speed, sensitivity, and ability to analyze volatile organic and inorganic compounds. Common detectors include the flame ionization detector and thermal conductivity detector. Gas chromatography has many applications in fields like drug analysis, food testing, and environmental analysis.
Instrumentation of column and gas chromatographySadaqat Ali
This document provides an overview of column chromatography and gas chromatography instrumentation. Column chromatography separates components based on their differing rates of movement through a stationary phase packed in a column. Gas chromatography uses a mobile gas phase to carry vaporized sample components through a column coated with a liquid or solid stationary phase. Both techniques use instrumentation that includes columns, carrier gas systems, temperature control, sample injection ports, and detectors to separate and analyze sample components as they elute from the columns.
Detection Method for Low Level of Potent ToxinsShreyas Patel
This document discusses various analytical methods for detecting low levels of potent toxins and impurities. It describes gas chromatography, high-performance liquid chromatography, and thin-layer chromatography techniques. For GC, it outlines instrumentation components like injectors, detectors, and sample introduction methods. For HPLC, it discusses separation modes, detectors, and instrumentation. TLC is described as using capillary action to separate components based on their affinity for the stationary phase. Various compounds are listed along with example separation and detection methods used for their analysis in different matrices.
This document provides an overview of gas chromatography. It discusses the basic components and principles of GC, including the mobile and stationary phases, instrumentation, and applications. The key points are:
- GC separates components in a sample using an inert gas mobile phase and either a solid or liquid stationary phase in the column.
- Common instrumentation includes the carrier gas, flow regulators, sample injector, temperature-controlled column oven, detectors, and recorders.
- Separation is based on how strongly components partition between the mobile and stationary phases.
- GC has wide applications in fields like pharmaceutical analysis, environmental analysis, forensics, and industrial quality control.
- Advantages are strong separation power,
Similar to Handling Difficult Samples in Karl Fischer Analysis (20)
The use of Nauplii and metanauplii artemia in aquaculture (brine shrimp).pptxMAGOTI ERNEST
Although Artemia has been known to man for centuries, its use as a food for the culture of larval organisms apparently began only in the 1930s, when several investigators found that it made an excellent food for newly hatched fish larvae (Litvinenko et al., 2023). As aquaculture developed in the 1960s and ‘70s, the use of Artemia also became more widespread, due both to its convenience and to its nutritional value for larval organisms (Arenas-Pardo et al., 2024). The fact that Artemia dormant cysts can be stored for long periods in cans, and then used as an off-the-shelf food requiring only 24 h of incubation makes them the most convenient, least labor-intensive, live food available for aquaculture (Sorgeloos & Roubach, 2021). The nutritional value of Artemia, especially for marine organisms, is not constant, but varies both geographically and temporally. During the last decade, however, both the causes of Artemia nutritional variability and methods to improve poorquality Artemia have been identified (Loufi et al., 2024).
Brine shrimp (Artemia spp.) are used in marine aquaculture worldwide. Annually, more than 2,000 metric tons of dry cysts are used for cultivation of fish, crustacean, and shellfish larva. Brine shrimp are important to aquaculture because newly hatched brine shrimp nauplii (larvae) provide a food source for many fish fry (Mozanzadeh et al., 2021). Culture and harvesting of brine shrimp eggs represents another aspect of the aquaculture industry. Nauplii and metanauplii of Artemia, commonly known as brine shrimp, play a crucial role in aquaculture due to their nutritional value and suitability as live feed for many aquatic species, particularly in larval stages (Sorgeloos & Roubach, 2021).
ANAMOLOUS SECONDARY GROWTH IN DICOT ROOTS.pptxRASHMI M G
Abnormal or anomalous secondary growth in plants. It defines secondary growth as an increase in plant girth due to vascular cambium or cork cambium. Anomalous secondary growth does not follow the normal pattern of a single vascular cambium producing xylem internally and phloem externally.
Comparing Evolved Extractive Text Summary Scores of Bidirectional Encoder Rep...University of Maribor
Slides from:
11th International Conference on Electrical, Electronics and Computer Engineering (IcETRAN), Niš, 3-6 June 2024
Track: Artificial Intelligence
https://www.etran.rs/2024/en/home-english/
hematic appreciation test is a psychological assessment tool used to measure an individual's appreciation and understanding of specific themes or topics. This test helps to evaluate an individual's ability to connect different ideas and concepts within a given theme, as well as their overall comprehension and interpretation skills. The results of the test can provide valuable insights into an individual's cognitive abilities, creativity, and critical thinking skills
Nucleophilic Addition of carbonyl compounds.pptxSSR02
Nucleophilic addition is the most important reaction of carbonyls. Not just aldehydes and ketones, but also carboxylic acid derivatives in general.
Carbonyls undergo addition reactions with a large range of nucleophiles.
Comparing the relative basicity of the nucleophile and the product is extremely helpful in determining how reversible the addition reaction is. Reactions with Grignards and hydrides are irreversible. Reactions with weak bases like halides and carboxylates generally don’t happen.
Electronic effects (inductive effects, electron donation) have a large impact on reactivity.
Large groups adjacent to the carbonyl will slow the rate of reaction.
Neutral nucleophiles can also add to carbonyls, although their additions are generally slower and more reversible. Acid catalysis is sometimes employed to increase the rate of addition.
BREEDING METHODS FOR DISEASE RESISTANCE.pptxRASHMI M G
Plant breeding for disease resistance is a strategy to reduce crop losses caused by disease. Plants have an innate immune system that allows them to recognize pathogens and provide resistance. However, breeding for long-lasting resistance often involves combining multiple resistance genes
ESPP presentation to EU Waste Water Network, 4th June 2024 “EU policies driving nutrient removal and recycling
and the revised UWWTD (Urban Waste Water Treatment Directive)”
EWOCS-I: The catalog of X-ray sources in Westerlund 1 from the Extended Weste...Sérgio Sacani
Context. With a mass exceeding several 104 M⊙ and a rich and dense population of massive stars, supermassive young star clusters
represent the most massive star-forming environment that is dominated by the feedback from massive stars and gravitational interactions
among stars.
Aims. In this paper we present the Extended Westerlund 1 and 2 Open Clusters Survey (EWOCS) project, which aims to investigate
the influence of the starburst environment on the formation of stars and planets, and on the evolution of both low and high mass stars.
The primary targets of this project are Westerlund 1 and 2, the closest supermassive star clusters to the Sun.
Methods. The project is based primarily on recent observations conducted with the Chandra and JWST observatories. Specifically,
the Chandra survey of Westerlund 1 consists of 36 new ACIS-I observations, nearly co-pointed, for a total exposure time of 1 Msec.
Additionally, we included 8 archival Chandra/ACIS-S observations. This paper presents the resulting catalog of X-ray sources within
and around Westerlund 1. Sources were detected by combining various existing methods, and photon extraction and source validation
were carried out using the ACIS-Extract software.
Results. The EWOCS X-ray catalog comprises 5963 validated sources out of the 9420 initially provided to ACIS-Extract, reaching a
photon flux threshold of approximately 2 × 10−8 photons cm−2
s
−1
. The X-ray sources exhibit a highly concentrated spatial distribution,
with 1075 sources located within the central 1 arcmin. We have successfully detected X-ray emissions from 126 out of the 166 known
massive stars of the cluster, and we have collected over 71 000 photons from the magnetar CXO J164710.20-455217.
The binding of cosmological structures by massless topological defectsSérgio Sacani
Assuming spherical symmetry and weak field, it is shown that if one solves the Poisson equation or the Einstein field
equations sourced by a topological defect, i.e. a singularity of a very specific form, the result is a localized gravitational
field capable of driving flat rotation (i.e. Keplerian circular orbits at a constant speed for all radii) of test masses on a thin
spherical shell without any underlying mass. Moreover, a large-scale structure which exploits this solution by assembling
concentrically a number of such topological defects can establish a flat stellar or galactic rotation curve, and can also deflect
light in the same manner as an equipotential (isothermal) sphere. Thus, the need for dark matter or modified gravity theory is
mitigated, at least in part.
Travis Hills' Endeavors in Minnesota: Fostering Environmental and Economic Pr...Travis Hills MN
Travis Hills of Minnesota developed a method to convert waste into high-value dry fertilizer, significantly enriching soil quality. By providing farmers with a valuable resource derived from waste, Travis Hills helps enhance farm profitability while promoting environmental stewardship. Travis Hills' sustainable practices lead to cost savings and increased revenue for farmers by improving resource efficiency and reducing waste.
The debris of the ‘last major merger’ is dynamically youngSérgio Sacani
The Milky Way’s (MW) inner stellar halo contains an [Fe/H]-rich component with highly eccentric orbits, often referred to as the
‘last major merger.’ Hypotheses for the origin of this component include Gaia-Sausage/Enceladus (GSE), where the progenitor
collided with the MW proto-disc 8–11 Gyr ago, and the Virgo Radial Merger (VRM), where the progenitor collided with the
MW disc within the last 3 Gyr. These two scenarios make different predictions about observable structure in local phase space,
because the morphology of debris depends on how long it has had to phase mix. The recently identified phase-space folds in Gaia
DR3 have positive caustic velocities, making them fundamentally different than the phase-mixed chevrons found in simulations
at late times. Roughly 20 per cent of the stars in the prograde local stellar halo are associated with the observed caustics. Based
on a simple phase-mixing model, the observed number of caustics are consistent with a merger that occurred 1–2 Gyr ago.
We also compare the observed phase-space distribution to FIRE-2 Latte simulations of GSE-like mergers, using a quantitative
measurement of phase mixing (2D causticality). The observed local phase-space distribution best matches the simulated data
1–2 Gyr after collision, and certainly not later than 3 Gyr. This is further evidence that the progenitor of the ‘last major merger’
did not collide with the MW proto-disc at early times, as is thought for the GSE, but instead collided with the MW disc within
the last few Gyr, consistent with the body of work surrounding the VRM.
The ability to recreate computational results with minimal effort and actionable metrics provides a solid foundation for scientific research and software development. When people can replicate an analysis at the touch of a button using open-source software, open data, and methods to assess and compare proposals, it significantly eases verification of results, engagement with a diverse range of contributors, and progress. However, we have yet to fully achieve this; there are still many sociotechnical frictions.
Inspired by David Donoho's vision, this talk aims to revisit the three crucial pillars of frictionless reproducibility (data sharing, code sharing, and competitive challenges) with the perspective of deep software variability.
Our observation is that multiple layers — hardware, operating systems, third-party libraries, software versions, input data, compile-time options, and parameters — are subject to variability that exacerbates frictions but is also essential for achieving robust, generalizable results and fostering innovation. I will first review the literature, providing evidence of how the complex variability interactions across these layers affect qualitative and quantitative software properties, thereby complicating the reproduction and replication of scientific studies in various fields.
I will then present some software engineering and AI techniques that can support the strategic exploration of variability spaces. These include the use of abstractions and models (e.g., feature models), sampling strategies (e.g., uniform, random), cost-effective measurements (e.g., incremental build of software configurations), and dimensionality reduction methods (e.g., transfer learning, feature selection, software debloating).
I will finally argue that deep variability is both the problem and solution of frictionless reproducibility, calling the software science community to develop new methods and tools to manage variability and foster reproducibility in software systems.
Exposé invité Journées Nationales du GDR GPL 2024
2. Background
• Analysis of moisture is becoming
increasingly important to many different
industries
• Many of these reasons require not only a
precise, but also accurate reading
• For years, most moisture analyses have
been conducted on a semi-quantitative
or even qualitative level
3. Questions about how much water?
Karl Fischer analysis is the answer.
• Karl Fischer (KF) titrations have been the gold standard for
water analysis since 1935
• The KF titration provides a reliable and robust way to directly
analyze for water in a sample
• Many other techniques exist for indirect analysis of water in a
sample, but KF titration is the best way to calibrate this other
methodology
• KF is rapid, well characterized, and the recognized standard
for water analysis in many solids, liquids and semi-solids
CH3OH + SO2 + RN → (RNH)SO3CH3
H2O + I2 + (RNH)SO3CH3 + 2 RN → (RNH)SO4CH3 + 2 (RNH)I
4.
5. Measurement range
% range ppm range
Volumetric KF titration Coulometric KF titration
16. How do we mitigate side reactions,
poor water release and gaseous
samples?
• Adjust pH with buffers
• Use specialized reagents for aldehydes
and ketones
• Use different sample preparation
17. What if my sample comes in a
container that looks like this?
18. KF Gas Analyzer
• For determining water in:
• Propane
• Propene
• LPG
• LNG
• Butane
• Butene
• Butadiene
• Dimethyl ether
• Ethylene oxide
• Methylene chloride
• Ethylene chloride
• Vinyl chloride
• Chlorofluorocarbons
• Analyzes gases and liquefied
gases from sample cylinders!
19. Mass Flow
↙ Controller
← Oil Filter
Heater →
Precision
← Control
Valve
↙ Coulometer
Sample
Inlet→
Nitrogen
Inlet→
KF Gas Analyzer
20. Reproducibility
Results of 360 measurements of LPG (3 g per measurement) within 84 h, mean value: 26,5
µg/g ± 0,8 µg/g
y = -0,005x + 27,389
0
5
10
15
20
25
30
35
0 50 100 150 200 250 300 350
number of measurements
watercontent[µg/g]
80°C / constant sample flow
50°C / constant
sample flow
50°C / fluctuating sample flow
21. What if my sample is solid or liquid
and needs a lot of preparation?
22.
23. Gas extraction
1. Samples
soluble in KF
reagent
2. Samples that
release water
in KF
compatible
solubility
promoters
direct titration gas extraction
1. Samples that
are not
soluble in KF
reagent
2. Samples that
cause side
reactions
liquid extraction
1. Samples that
release water
in organic
liquids
24. Principle of the Metrohm oven
technique
Dry carrier gas is used to
transport evaporated humidity
into titration vessel
Universal to nearly all samples
25. Principle of the Metrohm oven
technique
Metrohm developed the orginal
headspace analysis for Karl Fischer
titration
26. Advantages of using a KF Oven
• Nearly all KF analyses can utilize oven
• Very economical
• Much smaller reagent use
• Much more effective use of time
• Efficient
• Automation to handle many samples without human
interaction
• No need to clean vessel after just a few analyses
• Wide variety of applications
• Nearly all KF samples can be adapted to oven
technique
27. Gas extraction (oven method)
• Step 1: (use empty vial)
- Heat up KF oven
- Start gas flow
- Titrate cell to dryness
• Step 2: (use empty vial)
- Determine blank value
• Step 3:
- Put sample vial into the oven
- Heat up sample and transfer released water with carrier
gas to KF cell
28. Gas extraction (oven method)
Sample: Motor oil
• Oven, 160°C, N2
Content: ~ 390 ppm
• Direct measurement
Content: ~ 960 ppm
long determination time
curve with side reaction
29. Headspace KF analysis
• Wonderful technique for most sample types
• Until recently, Metrohm sample changers would
only accommodate a 6 mL headspace vial
• Now Metrohm can adapt our 874 USB KF Oven
Sample Processor to fit many of the most common
vials
30. How do you adapt a sample to KF
Ovens?
• Choose a temperature
• Classic method
• Multiple samples with different temperatures
• Choose best temperature for most stable and
reproducible moisture evolution
• Optimize for speed
• Gradient Method
• One sample over a range of temperatures
• Choose a carrier gas
• Choose air, nitrogen or argon depending on the
thermal stability and combustibility of the
sample
31. Example data: method development
Classic method of temperature determination
• Steroidal compound
Temp. Air source Extraction Time Water
Content
Decomposition
?
1 150 Air 300 0.04% Yes
2 160 Air 300 4.44% Yes
3 170 Air 300 6.60% Yes
4 200 Air 300 6.91% Yes
5 150 N2 300 0.14% Yes
6 155 N2 300 0.98% Yes
7 135 N2 1800 0.04% No
8 140 N2 900 0.06% No
32. Temperature gradient
• What oven temperature is optimal for an unknown
sample?
• Find the ideal temperature running a temperature
gradient with the KF OVen
• Looking for a temperature that will accelerate
water extraction but not pyrolyze the sample
• Pyrolysis or combustion leads to erroneously high results
33. Example data from temperature
gradient analysis
• Sample of mixed sugars and buffers
• Lyophilized Sample
• Ran 50 – 180ºC in 30 minutes
34. Example data from temperature
gradient analysis
• Chose temperature of 95 degrees
• Analysis was slightly more than 7
minutes
• This only took 1 gradient sample and one
sample to confirm
• Without gradient, this takes up to 7
samples
35. Example data: method development
Gas determination
• Steroidal compound
Air carrier gas at high
temperature
Evidence of
decomposition
Nitrogen carrier gas at
low temperature
Stable extraction
36. Headspace Karl Fischer moisture
analysis in your vial
• The 874 uses Metrohm’s
exclusive KF Oven
technology for unsurpassed
moisture results
• The 874 is perfect for your
lyophilized samples because
Metrohm USA will customize
the 874 to fit your sample
vial!
• Because only water vapor is
analyzed, reagent costs are
greatly reduced
• Holds up to 36 samples
depending on rack
configuration
41. Why NIR for moisture analysis
• Requires no sample preparation
• Non-destructive
• Fast, accurate and precise
• Multi component analysis
• No solvent procurement or disposal
• Low-cost analysis
• Easy to use and maintain
• Remote sampling via fiber optics
Secondary technique: requires primary
method for calibration development
43. • Based on absorption
in the Near Infrared
region of the
spectrum
• It provides both
chemical and
physical information
• Primarily sensitive to
organic compounds
• O-H, C-H, N-H bonds
absorb strongly in
NIR
NIR spectroscopy
48. Run Samples as
Standards in NIR
Analyze
Samples by
Primary
Method
Calibration
and
Validation
Routine
Analysis by
NIR
Right Sampling Module
Sample Presentation
Collection Parameter
Accuracy of
Primary method
influences NIR
Method
Chemometric
Software
Method
Maintenance
Quantitative Moisture analysis
53. Moisture in polymer pellets
The water content of expandable
polystyrene is determined
according to Karl Fischer
The sample is first dissolved in
p-xylene to extract the water
Then methanol is added to
precipitate the sample
The water is determined in the
supernatant solution by
coulometric titration
60. Moisture in solvent mixture
PLS: Factor 3
Correlation: 0.9998
SEC: 0.1939
• Save Time & Money
• NIR can be off-line, at-
line, or on-line
• NIR can measure Solvent
components and moisture
in single run
61. Inline Process NIR
granulator drying analysis
• Single-pot
granulator dryer
• Probe in contact
with powder
• Provides real-time
process analysis
and control
62. Granulator drying analysis
• Blend of lactose and starch granulated with
1.5% water and 8% methanol
• Granulation was dried with heat and
vacuum
• NIR probe monitored drying in-process
• NIR prediction models developed for water
and methanol
77. Experimental design
• Lyophilized product
• Contained in ~ 30 mL serum vials
• Average cake weight is 1.6 g
• Acceptable moisture limit is NMT 2 %
• Calibration sample set
• 46 samples used to prepare training and test sets
• Near-IR analysis
• Spectra of calibration samples collected in triplicate
• Primary analyses
• Regression equations developed using data from
volumetric Karl Fischer titration
81. Conclusion
• NIR is well suited for analysis of residual moisture in
lyophilized products
• Samples can be easily altered to provide calibration sets
with varying amounts of moisture
• Regression equations should be optimized for the
specific moisture range of interest
• The speed of the technique allows large sample sets to
be analyzed, enabling NIR to be used either as a
diagnostic or inspection tool
• Combined KF Thermoprep with NIR allows the quick
calibration and validation
82. Summary
• Combined Titration and NIR
• Calibration and Validation
• Routine application
• Accuracy and calibration stability
• Methods from lab to process
• Flexible and customized sampling accessories
• Rugged instrumentation
• Continual technical and application support