Gain extensive experience in sample testing and reporting on quantities
In the period of my internship at APPL Lab, I served in the Volatile Organic department as an intern where I successfully managed to gain extensive experience in sample testing and reporting on the various quantities. I realized during the time of my stay at the Agriculture and Priority Pollutant Laboratories Inc., APPL that this testing laboratory company is one of the most amazing and interesting facilities that is located at the Central Valley of Clovis California. The company, for a very long time been known owing to its undisputable ability to analyse environmental samples extracted from various solid wastes methods, waste water methods as well as methods of drinking water.
The laboratory adopts the latest and most popular electronic formats in the reporting of the findings from the various analyses. This enhances accuracy and convenience in the presentation of the findings of the analysis. One of the critical data deliverable is data programming which has been adopted by APPL Inc. in a bid to attain the various dimensions of the needs of the clients. The company is part of the U.S. Small Business Administration and registered as a small business owned by a woman.
Since it was started 19282, the company has managed to successfully work on and deliver various projects with varying degrees of scope and as such it has been able to gain a wide and elaborate experience in the handling of various reporting and testing. Still, the projects handled the company are not just from the localized regions around the region in which the company is located but instead from diverse location giving the company an opportunity to handle various issues. The company concentrates on the analysis of samples of soil and water. Furthermore, the company has managed to run a full service laboratory and is capable of concentrating on the issues affecting the environment even as it analyzed the soil and water samples hence has the ability to attend to the over 3000 chemical concerns during the analysis of the various samples. One of the main strengths or achievements of the company is its ability to conduct testing on air or biological contamination. While at the company, I took part in various procedures in the analysis of samples as well as the generation of suffice reporting in the Volatile Organic department.
Volatile organic compounds refer to those organic chemicals with high vapour pressure recordings at their normal temperature and the room temperature. Volatile organic compounds can maintain relatively low boiling points at extremely high vapour pressure and this facilitates vaporization or sublimation of mist of the particles from solid to liquid states. Various countries among the Canada, the United States of America and the European Union have each established their own definitions of what volatile organic compounds are. European Union defines volatile organic compounds as those compounds that have an initial boiling point lower than or equal to 250?C when the measurements are taken at standard conditions of atmospheric pressure.
Latest reporting formats for environmental sample analysis
There are various sources from which volatile organic compounds are generated and hence they are found in various places include soil, air and water. Whole some of the volatile organic compounds are naturally occurring; there is other than are artificially manufactured. Whether natural or artificially made, any volatile organic compound poses a threat to the health of the human being and to the surrounding at large. This thus leads to the need to a test for the volatile organic compounds in both the soil and water. The availability and concentration of these chemicals inside the soil and water need to be monitored in order to prevent any hazards to human health and to the environment.
Gas Spectrometry or Mass Selective Detector is one of the most reliable analytical techniques that are used in the testing of various samples. This analytical technique brings together the features of both mass spectrometry and gas chromatography in the acknowledgement of the wide range of elements that are available in a sample during testing. Gas spectrometry/ Mass Selective Detector makes use of the retention times of the relative gas chromatography and the pattern of elution of the various constituents that are found in the mixture to be tested in the detection of the volatile organic compounds in soils and water.
When conducting the Gas Spectrometry/ Mass Selective Detector, I also took part in the Agilent and Teledyne tekmar atomx. Agilent and teledyne tekmar atomx refers to combined patterns of spectral fragmentation that aid in the identification of the features of the substance being tested. This method is very helpful in the separation of the various individual components, detection of the ions as well as the transfer of the various constituents to the ionizing chamber during mass analysis.
It was possible receive most of the samples that were to be used in the lab in volatile organic analysis vials.
Soil samples: The soil samples were utilized in arriving in brass sleeves or the jars as well as in the volatile organic analysis. The samples that were coming in brass sleeves and the jars were removed from the fridge and then thawed out for about half an hour. About 5.0 g of the soil sample was the weighed out in a tare volatile organic analysis trial and 5 ml of Trap Water or Purge or MeOH was added to the vials. During the process of addition, care was taken to ensure that there was no contact between the tips of the pipette and the soil and the vials immediately closed after adding the substances.
Analyzing soil and water samples for over 3000 chemical concerns
Further, we took part in the preparations of the prewighted volatile organic analysis goals that were to be used in the Terra Core Sampling. The tare balance was used in the preparation of these samples in which 5 ml of Trap Water and Purge and about 1 g of sodium bisulphate was quantitatively transferred alongside a stir bar to the cap and via instantly. 5 ml of Purge and Trap MeOH was used for the case of preparation of vials of mid-level concentration. The vial that contained the solution was thereafter without out and the weight, lot number, time and the preservative that were used taken note of using the VOA Label program. The labels were printed and suck on each of the corresponding vials.
Water sample: volatile organic analysis vials that contained HCl were taken to the client. For those samples that were preserved, the analysis had to be started within not more than 14 days from the day of sampling. Travel blanks were prepared that went along with the volatile samples that were being taken to the laboratory for the purposes of determination of the available contaminants during the process of shipment.
There were two main methods that were ideal in testing the samples that were used in this experiment during my time in the laboratory: EPA 860 method and 524 drinking water method. EPA 8260 method was critical in the determination of the volatile organic compounds that are found in the water. The method was more specifically important in finding the matrices of the various solid wastes that are found in the water. EP 8260 method is in most cases applicable in samples whose boiling are lower than 200?C and is not influenced by the water content of such samples. In this method, the initial step is a direct injection procures which is composed of an aqueous sample dose that is made up of very high levels of concentrated analyte. The step is then followed by a purge and trap of the aqueous solution. It is recommended that the method be carried out under temperature of 40?C in order to attain higher efficiencies. The last bit of the steps in this method is vacuum distillation which is aimed at introducing the various volatile organics into the aqueous system. The automated static headspace technique is also usable in this method in aiding the addition of volatile organics into the system.
Gas Spectrometry/Mass Selective Detector and Agilent and Teledyne tekmar atomx methods used for detection of volatile organic compounds
Another yet important method that was carried out in this laboratory is 524 drinking water methods. This method involves the extraction of the volatile organic compounds and the surrogates that have low solubility in a sample matrix through building up an inert gas through the used aqueous sample. The purged constituents are captured in a tube that contains the suitable materials as the solvent. Upon the completion of the purging process, the sorbent tube undergoes heating and back flushing suing helium. This is done in order to desorb the components of the trapped sample into the capillary gas chromatography. Programming of the column temperature is done in order to enhance the separation of the various method analyte which then undergo detection by mass spectrometry.
The measured retention times and mass spectra of the compound eluting from the gas chromatography column are used in the identification of such compounds. The measure spectra and retention times are compared against the reference retention times and mass spectra as recorded in the database. These reference spectra and retention times are often obtaining through taking measurements of the calibration standards under similar conditions that are used for samples. Procedural standard calibration was used in the quantification of the analyte. The concentration of the components that has positively been identified is measured by comparing the response of the mass spectrometry of the quantification ion that has been generated by the compound under question with that of the mass spectrometry response of the quantification ion that has been generated by a compound which was used as an internal standard. The surrogate analyte are measured using the same procedure as the internal standard calibration owing to the fact that their concentration is known in all the samples.
Internal Standards: Each of the field samples and quality control is added internal standards. A retention time criteria of +/- 30 seconds deviation from the midpoint retention time that is standard in the ICAL is adopted. An area response criteria of +/- 50% IS is also provided of the ICAL midpoint standard.
Tuning: Tuning of the instrument is done before ICAAL and at the start of every period that lasts 12 ours. A standard solution that contains 25 ug/ml of BFB in methanol is made and introduced into the instruments for use in tuning. The criteria of the BFB tuning and criteria for GC/MS calibration verification must be met before the commencement of analysis of the samples.
EPA 860 and 524 Drinking Water methods utilized in testing
Initial Demonstration of Capability: The SOP# QC006 is used in the completion of the Demonstration of Capability, DOC.
Verification of Calibration Curve: The same standard that is used in ICAL applies to the Calibration Curve Verification standard. A close CCV is needed for the case of DoD 5.0 projects. It is a requirement that all the analyte and surrogates that have been reported lie within +/- 50% of the true value and in cases where the CCV fails to meet the outlined criteria; a notification is sent to the client who then provides or declines directions on further progress.
A method blank which is extracted and analyzed within 12 hour batches for each analysis. The initial calibration of each of the samples to be tested is checked and verified once after every 12 hours during the process if analysis which also involves the introduction technique.
A number of materials are required to aid in attaining the EPA 8260 method including the
- Purge and trap that was usable for the solid and aqueous samples
- automated static headspace device that was mainly used for solid samples
- azeotrophic distillation apparatus
- vacuum distillation apparatus
- desorption devices
- an air sampling loop
- injection port liners
- methanol
- stock solutions
- gas chromatographic columns
- hexadecane
- hydrochloric acid and
- Polyethylene glycol
For the 524 drinking water method, the materials that were required included:
- Sample
- Containers
- Syringe valves
- Purge and trap systems
- GC/MSD system
Among the main reagents included
- Water
- Vinyl chloride
- Sodium thiosulfate
- Hydrochloric acid
- Reagent water
- Ascorbic acid
This process or method involved the preparing of reagent blank in which the syringe was filled using reagent aster and then adjusted to the required level as the bubbles were being driven out. The recommended volume of the fortification solution that is contained in the internal standard and surrogates in then introduced through the Lure Lok valve into the reagent water. The reagent blank is then taken to the purging device where it undergoes further testing. The samples are then gathered and properly stirred to keep their ground conditions with a LRB set handed over along each of the samples to ascertain that the control reagent blank has the ability to check the situation and the conditions of the sample under test.
Spectra and chromatogram curves are used in the presentation of the concentration of the various reagents against the time elapsed.
The retention time and a comparison of the mass spectrum of the sample upon background correction are used in the identification of the various compounds in the samples alongside the characteristic ions as in the reference mass spectrum. Three ions with the highest relative intensity are used in the definition of the characteristic ions derived from the reference mass spectrum. In case here such ions are less than three, then any ions having a relative intensity of more than 30% is used.
Figure 1: An example of chromatograph
Figure 2: An example of spectra
There are various standard components of Relative retention Time:
RRT= RTc/RTIS
Where:
RRT = Relative retention time for every target analyte
RTc=Retention time of a target analyte
RTIS= Retention time of the internal standard
Calculations including RRT and concentration of each identified analyte in the sample were done with the aid of computers by programing them into the instrument.
I found an opportunity to engage in different methods and techniques that are used in testing at APPL lnc Laboratory. The internship offered me an opportunity to learn how the different laboratory software and important and usable in data reporting and instrumentation, preparation of samples for analysis and well as extraction of samples of water and soil. The internship period at APPL lnc Lab was such an amazing moment that offered me various challenging opportunities and learning platforms. Ranging from the avalanche of instruments and the diverse team of experts and professional in the company, I was surrounded by immense resources that saw me get the best out of the company. I not only gained more knowledge on volatile organic analysis but also have the opportunity of having hands-on tasks and engagements that enabled me gain the practical aspect of the sessions.
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