Per- and Polyfluorinated Alkyl Substances (PFAS)

Per- and  Polyfluorinated Alkyl Substances (PFAS) chemical compounds are a class of emerging contaminants that are generating high levels of interest and concern in the environmental community and the public at large. These compounds have a wide range of industrial uses and commercial product applications and are present in many consumer products as well. A short list of general product categories  includes industrial polymers, stain repellents, waterproofing products, surfactants, and packaging, as well as aqueous film-forming foams (AFFF) used for firefighting. The primary sources of PFAS released into the environment can be industrial facilities where they were used or contained in raw material feedstocks; as well as sites where AFFF was used for training purposes or actual firefighting. Other potentially significant sources of PFAS are landfills and wastewater treatment plants. PFAS compounds are highly soluble in water, chemically stable and persistent. Practitioners are cautioned to carefully consider potential sources of PFAS cross-contamination in the design of their sampling programs and sampling standard operating procedures (SOPs). There is considerable information available online from regulators and academia that  provide recommendations to minimize  potential sources of cross-contamination in a wide range of items,  from clothing and personal care products to sampling equipment. For more information regarding recommended sampling techniques, please download Alpha Analytical’s PFAS Sampling Instructions for potable and non-potable water.

Alpha Analytical currently offers PFAS analytical support utilizing a number of different procedures depending on your project application.

Drinking Water-Related Applications

Alpha Analytical has considerable experience with drinking water and we offer PFAS analysis in accordance with EPA Method 537.1 and the newly released EPA Method 533. Method 533 differs from 537.1 in that it incorporates an isotopic dilution approach using extracted internal standards as part of its calibration requirements as well as other method performance upgrades. While Method 537.1 specifies a list of 18 PFAS compounds, Method 533 specifies a 25 target compound list, either of which can be reported in their entirety, or as a subset. While there is substantial  overlap between the two  lists, not all of the 18 Method 537.1 compounds are listed under Method 533. For more information on EPA Method 533, visit our website.

Other Applications

Since Methods 537.1 and  533 are limited to clean water applications, Alpha Analytical uses a different procedure for the testing of non-potable water, soils and tissue samples. This method is particularly effective in cases  where there are additional, specific PFAS compounds that need to be included that are not on either method’s target compound list. Given the lack of standardized, published analytical methods for non-drinking water sample media, and the fact that EPA 500 series methods are not allowed to be modified in this way, Alpha Analytical has developed its own procedure.

This method is also a liquid chromatography tandem mass spectrometry method (LC/MS/MS) with solid phase extraction (SPE) and it is similar to the LC/MS/MS SPE Method 533 in that it also utilizes the isotope dilution technique.  Alpha Analytical incorporates the maximum number of commercially-available extracted internal standards, consisting currently 25 13C-enriched and 2 2H-enriched compounds. (As more of these reference standards become available, they will be incorporated into our method as well. We are currently analyzing for up to 41 PFAS compounds, or any subset, using this approach.) We analyze a wide range of sample matrices in addition to aqueous samples including soils/sediments, biosolids, tissues, and food/ agricultural products such as milk and cranberries. Given our laboratory’s extensive background supporting ecological risk assessments, we also have considerable experience with the processing of fish, shellfish, soils and sediments.

We also perform the total oxidizable precursors (TOP) assay on aqueous samples. The TOP assay is an analysis by difference approach, where two aliquots of a sample are analyzed. One aliquot is   pre-treatment and the other is post-treatment, with the latter subjected to strong oxidizing conditions prior to PFAS analysis. The PFAS concentration difference between the pre- and post-treatment samples is defined as the amount of oxidizable precursors present in the sample.

Alpha is currently operating four LC/MS/MS instruments. We also have  14 PFAS-dedicated solid phase extraction manifolds and our standard turnaround time is 10 business days. Alpha currently holds National Environmental Laboratory Accreditation Conference (NELAC) certifications for both Method 537.1 and Method 533, as well as our proprietary isotope dilution method in addition to many state certifications for PFAS analysis. Alpha is also certified by the Department of Defense Environmental Laboratory Accreditation Program (DoD ELAP)  for Method 537.1, Method 533 and the isotope dilution method.

To find out how we can help with your upcoming emerging contaminants sampling program, contact Alpha Analytical today. We offer PFAS, 1,4-Dioxane, Perchlorate, and 1,2,3-Trichloropropane analytical support.

To speak to one of our technical experts, please fill out the form to your left. 

Perchlorate

The occurrence of perchlorate in the environment is due largely to man-made sources; however, it can be present naturally in Chilean caliche soils which are used as fertilizers due to their high nitrate content. In aqueous systems, perchlorate exists as an anion, most commonly associated with ammonium, potassium and sodium salts. Perchlorate is very soluble in water and relatively inert, making it a mobile and persistent contaminant. The production of explosives, blasting agents and rocket propellant are the largest uses for ammonium perchlorate. Perchlorate salts are also used for a wide variety of other applications. The primary health concern related to perchlorate is its potential to interfere with the thyroid gland's ability to utilize iodine to produce thyroid hormones.

Although Alpha Analytical held EPA UCMR certification for perchlorate analysis by Method 314 for UCMR 1 in 2004, we now recommend the use of IC/MS/MS methods for the analysis of perchlorate. Alpha utilizes either EPA Method 332.0 or EPA SW846 6860, depending on your application. Both of these IC/MS/MS methods greatly increases the sensitivity, removes interferences from other anions and eliminates the possibility of false positive results.

Contact Alpha Analytical today for your upcoming PFAS, Perchlorate or 1,4-dioxane analysis project. To speak to one of our technical experts please fill out the form to your left. 

1,4-Dioxane

The primary association of 1,4-dioxane with environmental releases was its use as a stabilizer and a chemical inhibitor with chlorinated solvents, particularly 1,1,1-trichloroethane. While this was the most common source, 1,4-dioxane was used for a wide variety of other industrial processes as well. In addition, it should be noted that 1,4-dioxane is present in numerous consumer and commercial products that can enter the environment via septic systems and/or landfills.

Practitioners are reminded of the additional considerations that must be taken into account if 1,4-dioxane is considered a potential contaminant of concern. 1,4-dioxane’s physical properties make it especially challenging to analyze for (and remediate) in groundwater sample media. This is especially true for groundwater associated with regulatory criteria of less than 1 ug/L.

From an analytical perspective, 1,4-dioxane can be prepared for analysis as a volatile organic compound (VOC) or as a semivolatile organic compound (SVOC). As discussed, due to its physical properties, it cannot be easily purged as a VOC. In addition, due to its use as a chemical stabilizer for some chlorinated solvents, the presence of 1,4-dioxane is often suspected at these sites. For sites with high chlorinated VOC groundwater concentrations, these high CVOC analyte concentrations require samples to be diluted, often substantially, prior to analysis. These dilutions result in very high detection limits for 1,4-dioxane given that the sensitivity by Method 8260 is marginal even without any dilution. It should be noted that dilutions would still be required for high CVOC concentrations present in a sample, regardless if the analysis is being conducted specifically for 1,4-dioxane only. For these reasons, Alpha Analytical does not recommend utilizing a VOC approach, such as Method 8260, when the required detection limit is less than 1 ug/L.

Alpha Analytical offers two analytical method options for the analysis of 1,4-dioxane when the required reporting limit is less than 1 ug/L. The choice of which method to use depends on your project application and any associated regulatory requirements. Alpha Analytical holds both DOD ELAP and NELAC certification for 1,4-dioxane analysis by either Method 8270M or Method 522. An overview of both methods follows. We would be happy to discuss the relative merits of each approach with you if you need additional information.

Modified Method 8270 SIM w/Isotope Dilution

Superior chromatographic performance and greater sensitivity is achieved when Method 8270 is modified for 1,4-dioxane specifically with the mass spectrometer operated in the selected ion mode incorporating the isotope-dilution technique for greater analytical certainty. Isotope dilution techniques incorporate a deuterated form of the target analyte (1,4-dioxane-d8), which is spiked into every sample to act as a target-specific internal standard that is incorporated into the sample quantitation to normalize extraction recoveries. This approach also has the advantage of having no interference from chlorinated solvents as samples can be analyzed from sites with high concentrations of VOCs present with no dilutions required.

EPA Method 522

Method 522 has been promulgated by EPA for the analysis of 1,4-dioxane in drinking water. This procedure also utilizes GC/MS SIM (no isotope dilution) but it utilizes a different preparative procedure. Aqueous samples are extracted by a solid phase extraction (SPE) technique. It should be noted that this methodology was developed specifically for the drinking water matrix with very specific and prescriptive sample preservation requirements. These requirements can be modified for groundwater samples; however, this method so modified cannot be used to analyze public water system samples. Groundwater with varying dissolved / suspended solids content may also impact the performance of the Method 522 SPE procedure. For public water supply samples, Method 522 must be used as written for 1,4-dioxane samples. For drinking water samples from a private water supply, either the 8270 SIM isotope dilution method or Method 522 can be used, as long as all associated regulatory considerations are met.

There are a lot of additional considerations required if low level 1,4-dioxane analysis is required. Make sure to address any questions you may have with the laboratory upfront, as sampling containers and preservation will vary between the methods. Practitioners are also advised to incorporate field blanks (make sure they are 1,4-dioxane free) into their sampling programs at a conservative frequency whenever low-level analysis is required. Lastly, make sure you recognize that any detergents used for decontamination of sampling equipment could potentially be a source of 1,4-dioxane.

Contact Alpha Analytical today for your upcoming PFAS, Perchlorate or 1,4-dioxane analysis project. To speak to one of our technical experts please fill out the form to your left. 

Soil Analysis

Other than aqueous samples, soils make up the bulk of the environmental media we receive at the Alpha Analytical laboratory. (Rounding out the list are air, sediment and tissue samples.) Given that soils are so prevalent, Alpha Analytical has gained tremendous experience analyzing them in support of a multitude of environmental applications and analytical parameters. Following is a summary of our capabilities and what we analyze:   

EXPERTISE

• Initial Site Characterization
• Evaluation of Remedial Alternatives
• Post-Excavation/Confirmation Sampling
• Evaluation of Disposal Options
• Ecological/Human Health Risk Assessment

Targeted compounds

• Volatile and Semivolatile Organics
• Petroleum Analysis 
• Trace Metals
• Pesticides
• Polychlorinated Biphenyls (PCBs)
• Herbicides
• Inorganics including Cyanide, Sulfide, Hexavalent Chromium and Ignitability
• PFAS
• Dioxin/Furans
• PCB Congeners

Soil samples are often collected in support of a soil management application. The on-site soils are evaluated and categorized to determine whether or not they can be reused on the site, or if they need to be removed. If removal of the soil is not necessary, but the soil comprises some level of contamination, Alpha Analytical can recommend  available options, as there are often several, depending on the specific contaminants that are present, as well as their level of contamination. Since different soil receiving facilities have different testing requirements, in addition to having to comply with federal and state regulations, the process can be confusing and costly.  Alpha Analytical’s expertise in the latest requirements and a myriad of complicated testing protocols simplifies this process for our clients.  We understand the regulations and technical guidance compliance issues at every level. Not only that, our suites of analyses and soil management packages provide a streamlined, cost-effective  process for ordering soil testing. These packages are offered at a discounted price point in aggregate over what each individual analysis would cost. 

Alpha provides a number of information management tools that help our clients navigate the testing process. The front-end availability of our soil management packages, combined with our data management tools on the back end, can streamline and simplify your soil management applications.

For example, to make evaluating the data more straightforward -- in terms of facility or regulatory acceptance criteria --  Alpha provides comprehensive electronic data management tools via the Alpha Data Exchange (ADEX)/Data Merger, our exclusive online data portal.  The format we use for ADEX, the Criteria Checker, presents the data in Excel tabular format with the analytical parameters, samples and regulatory requirements Once you select the regulatory criteria (up to 10 at a time),  the table displays which analytes, in which samples, have detected results (or a detection limit) greater than the criteria you selected. 

Important note: Since many environmental sampling programs often encompass multiple media, we recommend reviewing each media separately as outlined on each page of our website for a more complete perspective of our capabilities in this area.

Federal Programs

Soil sampling is governed by several  federal and state level regulatory programs. Following is a  brief overview of a few of these major initiatives,  as well as the privatized programs set up by  three states  for the management of their lead-designated hazardous waste sites.

Resource Conservation Recovery Act (RCRA)  & Toxic Substances Control Act (TSCA)

The RCRA  and the TSCA are  federal regulations that guide the analytical processes connected with applicable site investigations and remediation programs.  Used by many states as a foundation for their regulatory programs, a document created by the  RCRA, the SW-846,   provides general guidelines that laboratories can follow to generate data.(It is important to note that the  SW-846 is  is not prescriptive, as it was written for guidance only.) Alpha Analytical supports most SW846 methods and is one of  few laboratories with a large enough available sample capacity for Soxhlet Extraction (Method 3540) sample extraction required for PCB analysis under the TSCA in some EPA Regions. 

We support the following SW-846 analytical methods from the RCRA:

• Volatile Organics by SW-846 8260
• Semivolatile Organics by SW-846 8270
• Pesticides by SW-846 8081
• PCB by SW-846 8082
• Herbicides by SW-846 8151
• Metals by SW-846 6010 or 6020
• Water quality parameters by SW-846 methodology

 The TSCA regulations place considerable focus on PCBs, and, among other things, prescribes sample extraction methods that are acceptable to these programs. 

State Programs 

Given the lack of specific analytical method performance and quality control/quality assurance standards, some states have adopted more stringent performance criteria. The states have incorporated these standards into laboratory analysis components of their privatized clean up programs.

Massachusetts Contingency Plan/Compendium of Analytical Methods

In 1999, the Massachusetts Department of Environmental Protection (MassDEP) determined there was too much uncertainty associated with the use of SW-846 methods, as written in support of the Massachusetts Contingency Plan (MCP) decision making.  As a result, MassDEP formed a workgroup composed of DEP personnel, environmental consultants and laboratory technicians to review the SW846 procedures and define specific requirements  and performance criteria for individual analytical methods included in theMCP methods manual, “The Compendium of Analytical Methods (CAM).” Alpha Analytical staff participated in the workgroups and was regularly involved with CAM training programs, and later with the associated Representativeness Evaluation and Data Usability Assessment workgroup and training programs. As a result of this involvement, Alpha Analytical has gained considerable experience with the CAM and generating data of known quality using the methods.   

Connecticut DEP Reasonable Confidence Protocols

Similar to what Massachusetts did with the CAM in support of the MCP, the Connecticut Department of Energy and Environmental Protection also  added specificity to the SW-846 guidance document with the Reasonable Confidence Protocols (RCP) to  support  the state’s Remediation Standard Regulations. Alpha Analytical employees were also heavily involved in the RCP workgroup and subsequent training programs, expanding our level of expertise in both states.

New Jersey Data of Known Quality Protocols (DKQP)

Along the same lines and with the same intent as the Massachusetts and Connecticut programs, New Jersey developed the Data of Known Quality Protocols (DKQP). Through the same participatory framework as the other states, Alpha Analytical has gained tremendous experience and knowledge of regulations in New Jersey. 

If your soil analysis project is located in Massachusetts, Connecticut and New Jersey, Alpha’s project managers and technical staff are uniquely qualified to help.