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Thursday, 28 February 2019
Wednesday, 27 February 2019
How to save your time by preventing Gas leaks before running the Gas Chromatograph?
How to save your time by preventing Gas leaks before running the Gas Chromatograph?
The article on importance of gas leak detection discussed the need for checking gas leaks and adoption of recommended leak detection methods. The present article discusses the practices that should be adopted to avoid gas leaks and save your valuable time for carrying out Gas chromatographic analysis.
Leaks should be checked and eliminated before proceeding for column conditioning and start of analytical work on the Gas chromatograph. You should start leak checking at the gas source regulator and carefully monitor each fitting and connector leading to the GC. It is important to switch off the column oven before checking all column connections, adapters, unions and fittings inside the oven.
How to prevent gas leaks?
It is advisable to adopt simple practices that will eliminate gas leaks and increase your confidence and laboratory sample throughput.
Proper cutting of tubing and columns
It is a good practice to use a tube cutter to obtain a clean tube cut. Unevenly cut ends contribute to leakages. A burr or ridge can result during the cutting process. This must be removed to allow free gas flow and obtain a leak free connection. Always hold the tube open end facing downwards while using a deburring tool to prevent fragments from falling inside the tube.
Choice of ferrule size and material
Choose the right size of ferrule that is compatible with the outer diameter of the capillary tubing.
Graphite ferrules are useful for general and high-temperature applications (up to 400°C). However, graphite is not the ideal choice for columns packed with oxygen sensitive stationary phases or oxygen sensitive detectors such as ECD due to semi- permeable nature of graphite. Over tightened graphite tends to flake and extrude thereby contaminating the columns.
Polyimide ferrules have limited application as they tend to shrink when exposed to heat cycling thereby increasing the need to over tighten but the material does not fragment.
Metal ferrules have the advantage of inertness and freedom from fragmentation but have no flexibility.
Never over tighten fittings
Over tightening can result in leaks due to breakage of columns or damage to fitting threads.
Compression fittings provide gas tight, leak free connections without the use of PTFE tape or adhesives.. For 1/8” tubing hand tighten the nut and follow by 3/4 turn using the wrench. For ¼” tubing turn one and quarter turn past fingered tight position with the wrench. On tightening the back ferrule forces itself onto the front ferrule to form a leak free seal. A properly tightened compression fitting usually shows one thread from the back of the nut. Over tighten fittings show no thread and results in leakage.
It always pays to spend a few minutes before start of analysis to ensure freedom from leaks so that you can avoid loss of high purity gases and save several hours trying to get reproducibility of results.
Importance of Colour Coding for Gas Cylinders and Lines in Laboratories
Importance of Colour Coding for Gas Cylinders and Lines in Laboratories
Gases constitute an essential utility in modern-day laboratories. Examples of gases commonly used are compressed air, zero air, nitrogen, helium, argon, hydrogen, nitrous oxide and acetylene. Operation of laboratory instruments such as Gas Chromatographs, Atomic Absorption spectrometers, ICP’s and Mass spectrometers is unthinkable without provision of required gases.
Let us begin by imagining a scene where a laboratory makes use of several gases but colour practices are followed.In such a situation though the chemist and technicians may be trained and confident but there is always scope for human error and catastrophic situations may arise due to:
- Wrong gas supplies being connected to instruments
- Storage of hydrogen or other combustible gases in vicinity of oxidant gases or storage in poorly ventilated areas which can result in formation of combustible gas mixtures.
- Fixing of non-compatible gas regulators to the gas cylinders
- Unsafe gas handling like storing of non- compatible gases or allowing passage of such gases in lines in vicinity of each other
Such potential laboratory hazards can be prevented by using the prescribed colour coding for gas cylinders and gas lines. It should be mandatory for every laboratory to make use of colour coded gas supply tanks and gas lines.
How to handle gas chromatographic gases safely provided some useful tips for handling of gases in a gas chromatography laboratory.You will not have to worry about getting the gas cylinders painted on receipt to the required specifications at it as it is the responsibility of the gas manufacturer to distribute. only prescribed colour coded cylinders.
Colour coding is helpful in identification of gas cylinders and lines even by laymen provided they are familiarised with such colour codes. Almost all countries follow their own guidelines but efforts have been made to prescribe universal colour coding. British Compressed Gases Association introduced cylinder identification and colour coding scheme through BS EN 1089 – 3 which has been harmonised in the European Union. The colours used for medical gases are harmonised on the basis of ISO 32 standard
The colour coding is applied to the shoulder or the curved portion of the cylinder and it identifies the property of the gas inside the cylinder.
- Yellow – toxic
- Red – flammable
- Light blue – oxidising
- Bright Green – inert
A gas cylinder having two concentric colour bands indicates a combination of properties. The body of the cylinder can be of any colour of manufacturer’s choice but it should not lead to confusion regarding risk associated with the gas as indicated by the shoulder colour.
For the purpose of easy identification and the shoulder colours can refer to the gas inside the cylinder. Some typical examples are:
- Maroon – acetylene
- Grey – carbon dioxide
- Brown-helium
- Red – hydrogen
- Blue – Nitrous oxide
- Black – nitrogen
- White – oxidant.
In addition to the colour coding it is helpful if a label is a fixed which bears the name of the gas inside the cylinder.
It is important for all laboratories to prominently display colour code charts in workplace as well as in gas storage space so as to familiarise the workers with associated hazards of gases and their potential hazards..
Peak Height or Peak Area? – Which is the right choice for quantitative chromatographic calculations
Peak Height or Peak Area? – Which is the right choice for quantitative chromatographic calculations
A typical chromatogram comprises of several peaks varying in size. The height of each peak is in proportion to the amount of the particular component present in the sample mixture injected into the chromatograph.
The chromatogram shown above is an ideal one showing symmetrical shaped peaks rising above a stable horizontal baseline. It can be seen that the peaks are well separated from one another and there are no overlap or shoulder bands. In such situations it is immaterial whether you use peak height or peak area in quantitative calculations.
Real-life sample chromatograms may not be that simple and will more than often show deviations resulting in non-Gaussian peaks due to several factors some of which are listed below:
- Presence of interfering compounds or impurities in the sample mixture
- Changes in operational parameters such as column temperature, flow rate of carrier stream, injection volume, etc.
- Leakages due to septum coring or worn out ferrules, O-rings or joint fittings.
- Detector response variation due to nature of compound
- Residual impurities present from earlier analysis.
Due to such reasons the chromatograms can deviate from ideal peak shapes and distortions in chromatograms become apparent as shown below
In such cases complications arise due to unsymmetrical peak responses and unstable baselines which are not uniformly flat. Peak height based calculations will lead to errors in quantitative estimations. Closely appearing peaks cannot be integrated in a reproducible manner because neighbouring peaks or overlaps influence peak height and area integration.The same is true for peaks arising from sloping or noisy baselines.
Peak integration is a mathematical operation performed by the chromatographic software to measure the area under a peak. The area measurement is based on integration which hypothetically divides the region below the peak into several rectangles which are summed up to give the total area under the peak. In order to define this area the software permits either manual or automatic marking of the start and end points of the peak. The baseline is then drawn between the start and end points to define the area calculation. It is important that same algorithm is used for area calculation of standard as well as sample peaks
Asymmetrical peaks often result due to peak tailing. It is difficult to reproducibly mark the endpoint of such peaks. This leads to errors in reporting of areas resulting in lowering of precision and accuracy of quantitative measurements.
Peak areas are used for most quantitative chromatographic estimations. Peak heights can vary due to distortion of the shapes such as the broadening or fronting and tailing. However, in such situations areas are not affected and show high reproducibility. On the other hand for very small peaks resulting from trace amounts of impurities peak height calculations may be a better option as errors in small variations in making start and end point of peaks become negligible.
The answer to the choice is based on your judgement of the quality of the chromatogram. However, in a majority of situations it would be advisable to make use of peak area measurements to get the highest levels of accuracy and precision.
How to prevent damage to Capillary GC columns
How to prevent damage to Capillary GC columns
Capillary GC columns are capable of producing highly reproducible chromatograms provided right operational conditions are maintained and steps are taken from time to time to prevent damage and performance degradation.
The factors which can result in deterioration are discussed in the present article and preventive measures are suggested:
- Accidental breakage
- High-temperature damage
- Oxygen damage
- Chemical attack
- Contamination
- Accidental damage
Accidental Breakage
Columns appear to be very delicate but the outer polyimide coating on fused silica tubing contributes to their physical stability. However, repeated heating – cooling cycles, vibrations produced by the cooling fan and careless mounting on the cage can lead to breakages. Sudden breakages are not common but over the use weak spots develop which can result in cracks or breakages.
The remedy is installation of unions to join the broken ends but multiple unions can contribute to dead volume which results in complications like peak tailing.
High-Temperature Damage
Every column has a specification on upper temperature operation. Exceeding the limit accelerates the degradation of the stationary phase. However, significant damage like loss of resolution or peak tailing becomes apparent over prolonged operation at temperatures above prescribed limit. Overheating a column with leaks result is in exposure to oxygen which can cause irreversible damage.
Thermal damage can be reversed to an extent by removal of a segment of the detector end of the column. Heating for about 8– 10 hours at its isothermal temperature limit and removing about 10 cm length from the detector end. Re-install and condition as prescribed before reusing.
Oxygen Damage
Continuous use of a leaking column at high-temperature leads to fast deterioration of the stationary phase due to oxygen damage. The damage is lower for stationary phases with polar characteristics.
The leaks can result from gas lines or injector fittings. Early symptoms of oxygen damage are excessive column bleed, loss of resolution, peak tailing, etc. It is best to ensure leak free operation to prevent onset of oxygen damage. This can be achieved by regular leak checking of gas lines and regulators, periodic septa changes and use of high purity grades of gases and installation of oxygen traps in gas lines. Remember to always replace gas cylinders before they run out of supplies completely.
Chemical Attack
Chemical attack is less serious than oxygen attack. Nonvolatile compounds have greater potential of damage to the stationary phase. The influence of nonvolatile compounds can be reversed to an extent by solvent rinsing.
Apart from non-volatile compounds mineral acids or alkalis can attack severely the stationary phases. Organic acids such as perfluoro acids can also result in column damage. Fortunately the damage is confined to around the front end of the column and removal of the front-end (say,1 – 2 m) can improve the column performance.
Contamination
Column contamination can result from introduction of semi-volatile or non-volatile impurities present in the sample matrices. While semi-volatile impurities are easily eluted over a period of time non-volatile impurities impair stationary phase performance and may or may not elute out of the column even on prolonged use. In addition to sample induced contamination such contamination can also result from foreign solid micro particles from gas lines or traps, septa and ferrules, etc.
Freedom of such contamination can be achieved by proper prior treatment of samples and frequent changes of ferrules and septas. Use of guard columns can also reduce problems arising from contamination. The column performance can be reversed by removal of a length of the front end of the column and using the other section and baking the column at its isothermal temperature limit for about 1 to 2 hours.
Among the other performance recovery solutions solvent rinsing technique is popular. Inject a few ml of solvent to dissolve soluble residues and remove them. However, this approach works with bonded or cross-linked phases and on the contrary can result in severe damage to non-bonded stationary phases.
Column Storage
On removal columns should be stored in their original boxes. Septas should be affixed to the open ends to prevent entry of any debris. At time of reuse around 2 – 4 cm of end tubing should be removed to prevent entry of septa debris, if any.
It should be remembered to keep carrier gas flow on if column is left inside a heated GC oven. Without the carrier gas flow damage can occur to the heated stationary phase.
Sampling of Gases for analysis by Gas Chromatography
Sampling of Gases for analysis by Gas Chromatography
Gas chromatography is an ideal tool for analysis of gases. The versatility of the technique extends its capability to analyse samples such as dissolved solids, liquids and gases. The scope of applications extends from pharmaceuticals, foods, environmental monitoring, petroleum refining, and workplace environment monitoring for safety of workers. Gas samples require special handling as gases have different physical and chemical properties in comparison with solids and liquids.
Types of Gas Sampling
Spot Sampling
Spot sampling is adopted when compositional details of a sample are required at any given point of time.It is commonly applied to observe the composition of a gas stream in industrial manufacturing processes. A tube similar Pitot tube,used for measuring flow velocities of fluids is inserted into the process pipeline and the representative sample is collected in the sampling cylinder for analysis in the laboratory.
Continuous Sampling
Continuous sampling has gained popularity in recent years and is mainly applied in process stream monitoring. The sample is withdrawn continuously and led to the detector for real-time analysis. The method provides real-time changes in the composition and helps in taking instantaneous quality control measures for consistent quality of product. The only disadvantage of this approach is that you have to place reliance on the accurate response of the instrument to changes in composition of the gas stream.
Three approaches are commonly used for collection of gas samples. One requires a direct collection for analysis in a laboratory and the other involving liquid displacement and another using adsorption or absorption on a solid support followed by desorption. In the present article direct collection is covered in some detail.
Grab Sampling
Several devices are used for grab sampling such as evacuated flasks, metal cylinders, plastic bags, etc.
Evacuated glass bulbs with varying capacities have one heat sealed and the open and drawn to a tip and sealed. The sealed tip is broken in the required environment and the allowed air is filled inside the bulb. On resealing the container is submitted for analysis to the laboratory. The sample is drawn using a gas tight syringe by penetrating the butyl rubber septum on the bulb.
Sampling Bags
Plastic bags specially designed for the purpose are available in different capacities depending on applications in hand. These can be used successfully for sampling of both organic and inorganic gases. Such bags are made from materials like polyester, Teflon,Fluorocarbons,etc. The choice of material Is based on the absorption or reaction of the gas with the bag material. The bags are connected to a pump for drawing gas samples inside.
Tips to Reduce Sampling Errors
Like samples of liquids there are potential sources of errors with Gas sampling. Typically these errors can be minimised by:
- Running the sample pump for some time before start of sampling to optimise the representative sample collection
- The sampling bag material should be inert to the gases collected and before transfer samples to the laboratory the bulbs or bags should be sealed tightly with suitable caps and stoppers
- Samples should be stored under appropriate temperature conditions and protected from exposure to light to prevent decomposition
- Whenever possible the sample should be analysed at the earliest opportunity after collection to avoid any changes in composition during storage and transportation.
Standard calibration weights for Analytical Balances- Traceability, Handling and Care
Standard calibration weights for Analytical Balances- Traceability, Handling and Care
All of you would be familiar with standard weight boxes used for calibration of analytical balances from your school days. Such weights are supplied in wooden boxes and are placed in individual slots inside the box along with a pair of tweezers for handling purpose. The weights provided meet weighing requirements of most analytical laboratories and include following weights: 10mg(0.01gm),20mg(0.02gm),100mg(0.1gm),200mg(0.2gm), 500mg(0.5gm),0.10gm,0.20gm,0.50gm, 1.00gm, 2.00gm,5.00gm,10.00gm,20.00gm,50gm and 100gm.
The observed balance reading should be within +/- 0.1% of market value of standard weight as per USP 41 requirements. As per the mandatory requirements, a weighing balance should be calibrated on a daily, weekly and monthly basis.
Traceability of calibration weight standards
Calibration weight standards are accompanied by a certificate of traceability. Such certificates are issued by national or international laboratories accredited by global bodies such as NIST, ASTM or OIMIL. Such certificates contain information such as the type of weight, weight class, material density, limit of uncertainty and environmental controls at the time of calibration. The traceability reports also give acceptable tolerance and uncertainty limits. During regular use, the standard weights should be calibrated periodically at assigned intervals and should be sent to a national accredited calibration laboratory and the issued certifications should be preserved for records purpose.
Handling & care
All standard weights comprise of a single piece of metal or alloy with no air cavities or foreign adjusting materials for mass stability. However, the weight readings can vary over time due to mishandling and lack of care. The commonly observed changes are the appearance of scratches or corrosion at microscopic levels due to contact with humid air or fingerprint impressions. Persons handling standard weights should take precautions like wearing gloves to avoid contamination from hands or fingerprint impressions and hair net covers to prevent fall of hair and dandruff. Further weights should be lifted only with ivory-tipped forceps to prevent scratches. Wearing face masks also prevents disturbance due to breath air drafts.
It is also essential to keep standard weight boxes under controlled temperature and humidity even when not in use to preserve their certified characteristic parameters.
Tuesday, 26 February 2019
An increase in the average temperature of the Earth’s atmosphere and oceans Global temperature on both land and sea increased by 0.6 ± 0.2 °C over the past century Volume of atmospheric carbon dioxide increased from 280 parts per million in 1800 to 367 in 2000, a 31% increase over 200 years
Global Warming | ||||||||||||||
What is Global Warming? An increase in the average temperature of the Earth’s atmosphere and oceans Global temperature on both land and sea increased by 0.6 ± 0.2 °C over the past century Volume of atmospheric carbon dioxide increased from 280 parts per million in 1800 to 367 in 2000, a 31% increase over 200 years Our Changing Climate Global mean surface temperatures have increased 0.5-1.0°F since the late 19th century The snow cover in the Northern Hemisphere and floating ice in the Arctic Ocean have decreased Sea level has risen 4-8 inches over the past century Global surface temp. could rise 1-4.5°F (0.6-2.5°C) in the next fifty years, and 2.2-10°F (1.4-5.8°C) in the next century What causes it? Human Impacts- Atmospheric greenhouse gases trap some of the outgoing energy, retaining heat Natural Impacts- Change in sun’s energy output Volcanoes Water Vapor Clouds Greenhouse Gases - CO2 Methane Nitrous oxide Fluorinated compounds Since industrial revolution, atmospheric concentrations of carbon dioxide increased 30%, methane more than doubled, nitrous oxide risen by 15%. These increases have enhanced the heat-trapping capability of the earth’s atmosphere Greenhouse Gas Emissions
Greenhouse Gas Emissions Power Plants 40% of carbon dioxide emissions stem from the burning of fossil fuels for the purpose of electricity generation Cars 20% of carbon dioxide emissions comes from the burning of gasoline in internal-combustion engines of cars and light trucks with poor gas mileage contribute the most to global warming Trucks Another 13% of carbon dioxide emissions come from trucks used mostly for commercial purposes Airplanes Aviation causes 3.5 percent of global warming, and the figure could rise to 15 percent by 2050 Carbon Dioxide from Buildings Buildings structure account for about 12% of carbon dioxide emissions Methane Methane is more than 20 times as effective as CO2 at trapping heat in the atmosphere 2004 Levels of atmospheric methane have risen 145% in the last 100 years Derived from sources such as rice paddies, bovine flatulence, bacteria in bogs and fossil fuel production . In flooded fields, anaerobic conditions develop and the organic matter in the soil decomposes Nitrous oxide Naturally produced by oceans and rainforests , man-made sources-nylon and nitric acid production, the use of fertilizers in agriculture, cars with catalytic converters and the burning of organic matter Deforestation Responsible for 25% of all carbon emissions entering the atmosphere by the burning and cutting of about 34 million acres of trees each year . The Carbon Cycle Effects of Global Warming Negative Effects Rising Sea Level Change of precipitation and local climate conditions; acid rain Alteration of forests and crop yields Expansions of deserts into existing rangelands More intense rainstorms Destabilization of Ocean currents Positive Effects Can stimulate plant growth in places where CO2 and temperature are the limiting factors (preventing photorespiration which can destroy existing sugars). Melting Arctic ice may open the Northwest Passage in summer, which would cut 5,000 nautical miles from shipping routes between Europe and Asia What Can be Done: Alternatives Renewable Energy Sources
Choi, O. and A. Fisher (2003) "The Impacts of Socioeconomic Development and Climate Change on Severe Weather Catastrophe Losses: Mid-Atlantic Region (MAR) and the U.S." Climate Change, vol. 58 pp. 149
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Indoor Air Pollution
A Common Myth Air pollution occurs only outdoors Or In industrial environment Truth!!!! What is more agreeable than one’s home? Feeling safe ? Away from outside pollution ? Air inside the conditioned space can be substantially more polluted than outdoor air. Historical Perspective First indication of indoor contamination – Asbestos pollution, a carcinogenic substance, discovered by epidemiologists, used in almost all building materials about 35 years back.Banned due to adverse health effects NOT considering IAQ. Concept of IAQ first introduced among scientific community in 1980 due to some occurrences of ‘episodes indoors’. At central headquarters of EPA building at Washington, D.C.- more than 100 people fell sick within 15 minutes of entering the office. In Los Angeles, CO level in most of the well insulated buildings was three times greater than the outside level. Outcome Such episodes indoors in developed nations ended up with 1. Extensive monitoring programme development indoors 2. Identification of indoor contaminants 3. Formulation of IAQ models 4. Development of control methodologies 5. Formulation of Indoor Air Contamination Standards. 6. Identification of ‘Sick Buildings’ 7. Investigation of ‘Sick Building Syndrome(SBS)’ What is IAQ?? Air Tightness in BuildingsCauses inadequate supply of fresh air, as a result, negative pressure develops, which causes Results into the production of fungi, molds and other sickness causing microbes. Problems of IAQ Enclosed spaces inhabited by humans produce following effects-
Sources of Indoor Air Pollution in a Typical Office Building
Sources of Indoor Air Pollution in a Typical Household
Hard Facts Poor IAQ Results Indoor Air Pollutants and Their Health Effects
What is Ventilation??
A process, whereby air is supplied and removed from an indoor space by natural or mechanical means.
Why ventilation is needed indoors?
To remove heat or moisture OR to reduce the concentration of one OR more indoor pollutants
Types of Ventilation
Exfiltration: movement of air from indoor spaces to outdoor. Limitation of Natural Ventilation
Mechanical ventilation
Principle of mechanical ventilation A. In naturally ventilated buildings
Air Flow- occurs mainly due to two driving forces
2. Temperature Gradient (Buoyancy Forces)- when the inside air temperature is higher than outside air, the warm air at floor surface starts rising and the cool air starts entering as a result of vaccum created at floor surface. This effect is called as “Stack Effect”.
The feeling of illness among majority of occupants of a conditioned space is called “Sick Building Syndrome”. A variety of illness symptoms reported by occupants in sick buildings are – Headache, fatigue, irritation in eyes, nose and throat, shortness of breathe etc. Causes
The CO2 level indicates the ventilation efficiency of buildings. Building shows SBS symptoms, if CO2 concentration > 1000 ppm.
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