Currently, the most commonly used digestion method for the extraction of metals analysis is EPA 3050, a strong acid digest designed to illustrate what might be environmentally available. In an attempt to maximize efficiency within the lab and increase turn-around, all efforts must be made to increase sample preparation efficiency without sacrificing quality.

It’s expected that a higher temperature digest than what is currently being used may result in metals migrating from the soil matrix into the acid solution at a faster pace, as this is an endothermic reaction.

The technological advantage AGAT Laboratories is pursuing is to discover the optimum time and temperature for the most efficient acid digest is sought.

The analysis of Microtox on drilling muds calls for 90 minutes of centrifugation to clarify a supernatant prior to quantification. Often, the clouding of the supernatant solution is a result of the presence of cellulose-based polymers, specifically Xanthan Gum and Carboxymethylcellulose. These polymers are used in the field to hold hydrocarbons, water and soils together in drilling mud suspensions, allowing drilling engineers to manipulate mud densities and viscosities in the drilling process.

AGAT Laboratories hypothesizes that dropping the pH will fill populate carboxyl group sites with protons, effectively bringing the polymer out of suspension in water during centrifugation. AGAT Laboratories is trying to find out if the polymers are selectively precipitated out of a solution without alteration of hydrocarbon concentrations, is it possible to optimize the method for more efficient throughput in the laboratory?

Reference methodologies for the quantification of Petroleum Hydrocarbons in air samples have not been developed to cover the criteria developed by the CCME. In this development program, AGAT Laboratories attempts to establish if the extension of the CCME criteria from soils to air is viable.

Procedures for sample preparation, standard preparation and evaluation will be developed. Success will enable AGAT Laboratories to perform environmental analysis of ambient and occupational air samples.

The analysis of Fe2+ and Mn2+ in water is typically performed by HPLC with a post column reaction with PAR. Presence of other strong complexing agents in water samples is masking the detection of Fe2+ and Mn2+, and altering retention times. Therefore, when performing this analysis by HPLC, multiple sample dilutions are often required which significantly increases the method detection limits for these two analytes.

In this program, AGAT Laboratories attempts to develop a method of water sample pre-treatment, allowing us to avoid dilutions, reduce method detection limits and stabilize the observed retention times for cations of Fe2+ and Mn2+.

Drilling wastes, per analytical protocol, are digested as wet samples or “as received”. This runs contrary to a typical metals digestion procedure of soil samples. The hypothesis being pursued in this program concerns whether or not moisture present in over-saturated samples dilutes the acid used in the digestion procedure enough to affect how well metals are being brought into solution. In addition, the fact that the samples do not undergo homogenization typical in soil or sediment analysis programs could perhaps influence the consistency of the results and the recovery of metals from samples laden with clay or other dense soil types.

AGAT Laboratories investigates whether significant evidence is present to confirm or dispute the use of “as received” digests on drilling muds.

Drilling waste samples often originate at “Barite Sites” destined for analysis of both total and extractable Barium, often at requested rush turn-around times.

AGAT Laboratories intends to investigate whether an elevated drying temperature causes significant oxidation, enough to bias the results. If successful in determining that the high drying temperature does not affect the analyte concentration significantly, AGAT Laboratories will have decreased preparation and analysis time, thereby decreasing analytical turn-around time significantly.

In this project, AGAT Laboratories is examining the use of chelation agents in tandem with conventional ICP-MS technology for the analysis of trace metals. ICP-MS is the standard technique for trace metals analysis commonly seen in environmental samples. However, it is limited in its ability to analyze samples with high dissolved solids content and/or high concentrations of certain elements with reasonable accuracy and precision using standard methodologies.

AGAT Laboratories attempts to utilize chelating agents to mitigate potential mass conventions, thereby allowing for the determination of trace metals in marine samples.

 The SPLP procedure is used to simulate the leaching effect on various contaminants of concern, illustrating the environmental effects over time. This information is useful during the design, construction and monitoring of landfill sites and for projects involving solidification/stabilization as a remediation tool. This project is intended to examine how best to maximize the amount of Total PCBs that are recovered from the leachate fluid for analysis. This will provide the end users of the data a more accurate and precise measurement of Total PCBs that may leach from material over time.

Resolution of Chlorate, Chlorite and Bromate ions by Ion Chromatography (IC) is not possible when analyzing common anions such as Nitrate, Nitrate, Chloride, Fluoride, Phosphate, Sulphate and Bromide using columns recommended by standard methods for aqueous samples. This is due to the co-elution of the peaks in the resulting chromatography.

This project will seek to resolve each of these compounds using an alternative column.

Analysis by GCMS using traditional columns such as DB-5 is the standard approach for PAHs. However, limitations in the chromatographic separation of several PAHs exist where similar retention times and molecular masses are encountered. Newer specialty columns offer the possibility of resolving these isomers by looking at fluorescence of molecular geometry for the identification of PAHs.

Our investigation will verify the performance of these columns relative to generally accepted standard methods for the resolution of these columns.

 This project will seek to provide an adaptation of the Atlantic RBCA method for Extractable Petroleum Hydrocarbons (EPA) analysis. This is to be applied to biological tissues, specifically fish oil and fish muscle, by breading these down to an aqueous solution. This would allow for the extracted EPA from the tissue to be recovered for analysis using the Atlantic RBCA method for EPH analysis by GC/FID.

 Currently no standard method exists for the extraction and analysis of total PCBs in paint chips. Existing standard EPA methods for extracting soil and solid samples will be applied to this matrix and investigated to determine fit-for-purpose in the matrix.

 This project will seek to apply existing analytical techniques for the testing of Total Phenolics in water samples to soil matrices such as solids and sediments using distillation followed by colorimetric analysis using segmented flow colorimetric analysis.

AGAT Laboratories’ Mississauga facility uses a Purge and Trap GC/MS approach to analyze for Volatile Organic Compounds in soils and water. It has been observed that many client samples are extremely contaminated with high levels of hydrocarbons or volatile compounds, yet require that the reporting detection limit for vinyl chloride be at or below the low and required guidelines. On occasion, the reporting detection limit is adjusted and as such, is above the guideline requirements due to the dilution(s) required. These dilutions are performed in order to minimize/prevent contamination of the purge and trap system as well as answering calibration limitations.

To meet client and regulation requirements, an alternative technique is proposed for such samples. Headspace analysis GC/MS may allow a more highly contaminated and concentrated sample to be analyzed using a lower dilution level such that the reporting detection limit is not as affected. AGAT Laboratories would like to investigate the performance of headspace analysis GC/MS in comparison to Purge and Trap GC/MS for the detection of vinyl chloride in the presence of varying high levels of Trichloroethylene and Hydrocarbons.