TestAmerica's New Methods and Capabilities

SW 8015B/ Iowa OA-2 Analyte Addition - Crude Oil
Cedar Falls Laboratory

Method Application:

This method is used to determine the total extractable hydrocarbons as Crude Oil present in a sample.

Market Application:

At the request of the Nebraska Department of Environmental Health, the laboratory validated this analyte using the IA-OA2 method. This request was made for the potential release of crude oil from a new oil pipeline being constructed in the state.

The Legislature recently introduced a bill that would require oil companies that own, operate, or manage a pipeline in Nebraska, to file an extensive application process with the state's Public Service Commission. This would require the submission of a pre-filed testimony, application framework, in addition to providing evidence of any environmental and economic studies of the proposed pipelines.

Advantages:

This method/analyte would use area of the entire chromatogram and compare it against a crude oil standard versus the traditional OA-2 comparing the chromatogram to individual regions of refined gasoline, diesel, and waste oil standards.

Click here for more New Methods and Capabilities from TestAmerica

Methane Analysis in Waters

Ask the Expert Question:

Water samples were collected from wells that were believed to be impacted by methane due to hydraulic fracturing and analyzed by two different laboratories. Two different analytical methods were run, RSK-175 and EPA Method 18. The results from the same sample source were about an order of magnitude different. Both methods used the analysis of headspace. Do you know why such a large difference would occur?

Experts Response:

In response to your question about large differences in results from two methods - RSK-175 and EPA method 18, I suspect that the differences relate to differing approaches in purging methane from each sample. RSK-175 is intended to measure dissolved gases, such as methane, in water samples, whereas EPA method 18 is designed for analyzing volatiles in air samples. The results for EPA 18 will depend on the how the laboratory created the headspace vapor sample, as that step is not defined in the method.

I suggest you evaluate how the methane in the water sample was converted to a gaseous sample, and also evaluate how standardization was performed for EPA 18. Another contributing factor is how the integrity of the water sample was maintained from collection to time of analysis. Unless the samples remained tightly sealed until analysis was performed, some methane could have been lost prior to analysis.

In summary, both methods should provide accurate methane analysis, so the main issues to investigate are the sample preservation and handling prior to analysis, and particularly how the EPA 18 headspace was created.

View Dr. Jack Tuschall's expert profile

Question on Incremental Sampling Methodologies

Ask the Expert Question:
One of the main tenants of the Incremental Sampling Methodologies approach is the analysis of a larger analytical subsample. For organic analysis, this doesn't seem to be a problem, but it is for metals. The digestion blocks that are the norm in environmental labs basically fix the analytical sample at 1 or maybe 2 grams. In fact, the official digestion methods are only validated for these small sample sizes. Is pulverization the only way to really get around the limitation on the analytical subsample size?

Experts Response:
You are correct that using large subsamples is a common part of Incremental Sampling Methodology (ISM). For organics using 10-30 g is already the norm so this isn't really a change for organic extractions. As you point out most metals digestion methods are optimized for 1-2 g aliquots. There are two common ways to address this limitation.

What do you know about the next wave of contaminants of emerging concern from the EPA?

TestAmerica is hosting its second webinar, Measurement of Pharmaceutical and Personal Care Products in Complex Matrices on April 14 at 1:30PM EST. Dave Herbert, Business Development Manager at TestAmerica will be presenting on the impact of Pharmaceuticals and Personal Care Products (PPCP’s) in our nations waterways.

Join us for the presentation and learn how TestAmerica's efforts in this emerging market go beyond the routine analysis of water by developing method capabilities to detect PPCPs in more complex matrices including waste water and sediments. Unlike typical water analyses, wastewater and sediments matrices contain high levels of organic materials and suspended solids, and require a more rigorous extraction process to identify and measure trace level PPCPs.

Click here to learn more about the presentation and register, space is limited.

Sampling Protocols for Collecting a Tap Water Sample for Lead Analysis

Ask the Expert Question:
What are the sampling protocols for collecting a tap water sample to analyze for lead?
Expert Response:
There are 2 guidelines for collecting a sample for the testing for lead.

According to EPA's lead and copper rule for drinking water, it is recommended that you collect a first-draw sample from a tap where the sample has stood in the pipes for at least 6 hours (e.g., no flushing, showering, etc.). First draw samples collected at single-family residences should be drawn from the cold-water kitchen tap or bathroom tap. Collect the sample into a 1-liter poly container. The laboratory can acidify the sample upon receipt for preservation.

For water quality monitoring, the sampling guideline indicates that the water source should be fully flushed for 10 minutes. Then collect the sample into a 500ml (or 250ml) poly bottle preserved with nitric acid.

View Cam Pham's expert profile

Is Limit of Detection (LOD) the same as Minimum Detection Limit (MDL)?

Ask the Expert Question:Under the Department of Defense (DOD) Quality Systems Manual 4, the language has changed from Minimum Detection Limit (MDL) to Limit of Detection (LOD) (and Limit of Quantitation (LOQ)). Is the LOD the same thing as MDL? What is TestAmerica's plan on becoming consistent with this new language?

Expert Response:The DOD is using all of these designations at this time.

The MDL definition has not changed and is essentially the lowest level at which a result can be reliably distinguished from a blank.

The LOD is higher than the MDL, and is supposed to be the level at which a true concentration in the sample will reliably give a result that is greater than the MDL.

LOQ definition has not changed and is the lowest quantitative level for the sample.

When reporting data, the LOD is used as the Non-Detect (ND) value, for example, NDs will be reported as < LOD.

Detects, however, are reported down to the MDL, with J flags if below the LOQ.

TestAmerica is reporting data for DOD projects using these conventions. We are not reporting this way to non DOD projects to be consistent with non DOD quality programs.

View Dr. Richard Burrows expert profile

Sulfur in Oil Concentration

Ask the Expert Question:
We have had a need to analyze diesel fuel samples for sulfur and heat content analysis utilizing SW-846 Method 5050 and 9056 as the analytical procedure used to determine sulfate percent. Some of the samples may be analyzed for air permit compliance. The permits require us to have the sulfur content analyzed by ASTM D4294 or equivalent method.

I have read through the documentation on ASTM D4294, SW-846 Method 5050, and SW-846 Method 9056. It appears to me that the methods get to the same end point - sulfur content. However, I would like a second opinion from one of your content experts that confirms what I have concluded.

Experts Response:
The ASTM D4294 (energy dispersive X ray fluorescence technique) is widely used for measurement of sulfur in oils.

The EPA Methods 5050 and 9056 (determination of sulfate ion concentration) is a complete oxidation using a bomb calorimeter followed by analysis of the resulting sulfate. This technique is used for sulfur in oil and waste products and has been used for decades. This is a highly reliable method for determination of sulfur in oils.

Both techniques should give similar results.

View Dr. Charlie Carter's Experts profile

Source Types for Benzene Concentration Without Similar Elevated TEX Concentrations

Ask the Expert Question:
At a remediation site we are working on, there is a monitoring well that had soil samples taken during the drilling process and analyzed for BTEX. All concentrations were below 1 part per million. However, the groundwater analysis is presenting an extremely elevated level of benzene with comparable levels of the TEX components. Other wells in the area are either non-detect or have low concentrations for benzene. The data has been verified and is accurate.

We do not understand the elevated Benzene constituent. What type of source would yield such a high Benzene concentration without similar elevated TEX concentrations?

Experts Response:
When benzene is present in environmental samples it is typically an indication of contamination by gasoline or some type of hydrocarbon based fuel. In those cases, however, other aromatics such as toluene, ethyl benzene, and xylenes are present along with numerous alkanes and alkenes. In this sample, the volatiles analysis did not indicate the presence of the other gasoline constituents that we would normally expect.

Benzene was used in various commercial products up until the late 1970’s. These included Liquid Wrench, model cement, paint strippers, rubber cements, and degreasers. It was available commercially in hardware stores for various applications, much like mineral spirits and turpentine are today. Given the presence of benzene in this sample and the absence of other gasoline related constituents, it seems likely that the contamination resulted from a relatively pure source of benzene used for one of these applications.

View Dr. Charlie Carter's Experts profile

Volatile versus a Semi-Volatile Compounds

Ask the Expert Question:
What makes a compound a volatile versus a semi-volatile?

Expert Response:
There is no hard and fast rule to determine what is called a volatile compound and what is called semi-volatile. There are a variety of chemical characteristics that influence volatility, but for the most part the definitions that are used in environmental analysis are operational definitions.

The operational definition is whether a compound will purge from aqueous solution in a purge and trap device. If a compound will do so at a high enough rate to be detected and quantified, then it is considered to be volatile. If an analyte is only found in a semi-volatile analysis and is not present in the volatiles analysis, then almost by definition it is not volatile.

There are also, however, some physical chemical characteristics of volatile compounds. The key characteristics are (1) vapor pressure or boiling point, and (2) aqueous solubility. As the vapor pressure increases, a compound’s volatility increases. As its aqueous solubility decreases, it also becomes more volatile from an aqueous solution.

For example, 1,2,4-trichlorobenzene is about the highest boiling compound routinely included in a volatiles analysis. Its boiling point is listed as 214.4 degrees Celsius, and it is quite water insoluble. Nitrobenzene’s boiling point is 210.9 degrees Celsius, but it is more soluble in water due to the polar nature of the nitro group. It does not purge with sufficient efficiency, so it is not considered a volatile.

View Dr. Charlie Carter Experts profile

Dust Sampling Methods and Equipment

Ask the Expert Question:
There are abandoned mine land sites in our area that are often used for recreational activities. These activities generate a great deal of dust. The sediments and mine wastes in these areas are potentially contaminated with heavy metals and could put people using these public areas at risk. Can you provide any information on methods to sample the dust? Also, where can I obtain the equipment to do the sampling?

Experts Response:
There are several considerations for deciding upon how to approach monitoring the dust.

The first consideration is: what will you compare your data to with regard to health standards or risk criteria? The answer will help to define how you will collect the samples. For example, it may make sense to compare your results to the National Air Quality Standard for the particular heavy metals contamination present, and/or the PM10 standard for Total Particulate. Some counties in the US even have their own ambient air quality criteria.

Your choice of criteria will dictate how the samples should be collected; the detection levels required and for what time period the samples must be collected. As an example, the National Air Quality Standard for Lead requires that a sample be collected for a 24 hour period.

A second consideration is: do you have a source of electrical power, or will it be necessary to use sampling equipment that is battery powered? Battery powered equipment may pose a problem if your sampling period must cover 24 hours.

TestAmerica does have air sampling pumps available for clients depending upon your sampling criteria. Click here to contact our expert, Mike McGee to inquire about the equipment and methods available.

View Mike McGee's Experts profile

What is the difference between total metals vs. dissolved metals analysis and what form the metal is being analyzed

Ask the Expert Question: 

Can you explain the difference between total metals versus dissolved metals analysis and what form of the metal is being analyzed?

Expert Repsonse: 

Total metals analysis for water samples include the metals content both dissolved in the water and present in the particulates in the water. Typically a dissolved metals analysis of a water sample is performed by removing the particulates with a filter, then analyzing the filtered water for metals. The most common filters used for this purpose have a 0.45 um pore size.

Total metals analysis results should always be greater than or equal to dissolved metals analysis results, because dissolved metals is a subset of total metals. Dissolved metals are generally considered more mobile and biologically available. Thus, the dissolved metals results are useful for risk assessment and fate & transport studies.

The specific metal species (or form) present in the dissolved fraction is highly dependent on the metal of interest. Most of the dissolved species are solvated metal cations such as Na(I) or Cr(VI). Some metals species are present as oxy anions such as arsenite.  

Water solubility of the elemental metals (i.e. neutral valence state) is generally quite low. For example this website states elemental mercury [Hg(0)] has a water solubility limit of 56 ug/L at 25C (http://www.inchem.org/documents/cicads/cicads/cicad50.htm#2.1).

Most regulations use total metals results because it is often considered more conservative and protective, however, depending on the purpose of the regulation it might be based on dissolved or total metal concentrations.

View Dr. Mark Bruce's Experts profile.

What are the differances and applications of HRGC/HRMS and GC-MS/MS instruments

Ask the Expert Question:

What is the difference between the HRGC/HRMS and GC-MS/MS instruments?
What are its major applications?

Experts Response:

By definition HRGC/HRMS stands for “High Resolution Gas Chromatography/High Resolution Mass Spectrometry” and GC-MS/MS stands for “Gas Chromatography/Tandem Mass Spectrometry”.

Starting with the GC-MS/MS, this equipment is fitted with what can be described as a dual mass spectrometry and are generally triple quads (or 3 quadrupoles).  Using a triple quad versus a standard GCMS give greater sensitivity (i.e. allows for lower detection limits from sub part per billion to sub part per trillion) and give greater resolution than a standard GCMS.  For example a standard GCMS can resolve masses 1 atomic mass unit apart.  A triple quad can resolve masses ~1000 atomic mass units apart.  Using GC-MS/MS resolution increase allows for much greater selectivity than standard GCMS.  Another feature of the GC-MS/MS is the dynamic range is much greater than a normal GCMS. 

HRGC/HRMS is a completely different type of instrument for very specific applications.  This instrument is fitted with a huge magnet and has electric sectors, lens and a 6 to 8 foot flight tube.  Using this type of configuration jumps the resolution to 10,000 atomic mass resolutions.  You can separate molecules that may have the same retention time but different masses 0.0001 amu apart.  Also the HRGM/HRMS allows for sensitivity to sub parts per quadrillion level and below and you can easily see 0.5fg on column of 2,3,7,8-TCDD (which is difficult to impossible for a standard GCMS or GC-MS/MS to see).  The dynamic range for the HRGC/HRMS is greater than 2000 times the low point so there is a lot of room to see the low end and the high end without saturating the detector.

There are many methods written for both types of instruments and you can use them for specific needs.  If you are looking for gross contamination then a GCMS is the way to go for general screening and for analytes with little public health risk.  GC-MS/MS is perfect for confirmation of low level GCMS results.  If you are looking to confirm low level results of analytes with high public heath risk then the HRGC/HRMS may be a better option.

EPA Issues National Guidance to Address Proper Maintenance, Removal, and Disposal of PCB-Containing Fluorescent Lights

Release date: 12/29/2010

Contact Information: Tisha Petteway, petteway.latisha@epa.gov, 202-564-3191, 202-564-4355 Dale Kemery, kemery.dale@epa.gov, 202-564-7839, 202-564-4355

WASHINGTON – The U.S. Environmental Protection Agency (EPA) today released guidance recommending that schools take steps to reduce potential exposures to PCBs from older fluorescent lighting fixtures. The guidance, part of EPA’s ongoing efforts to address potential PCB exposures in schools, is based on evidence that the older ballasts contain PCBs that can leak when the ballasts fail, leading to elevated levels of PCBs in the air of schools that should not represent an immediate threat but could pose health concerns if they persist over time.

The guidance document is available online at http://www.epa.gov/pcb.

Polychlorinated biphenyls, or PCBs, are man-made chemicals that persist in the environment and were widely used in construction materials and electrical products prior to 1978. PCBs can affect the immune system, reproductive system, nervous system and endocrine system and are potentially cancer causing if they build up in the body over long periods of time.

“As we continue to learn more about the potential risks of PCBs in older buildings, EPA will work closely with schools and local officials to ensure the safety of students and teachers,” said EPA Assistant Administrator for Chemical Safety and Pollution Prevention Steve Owens. “This guidance on safely addressing the risks from PCB-containing light fixtures is part of EPA’s ongoing efforts to protect the health of our children and provide them with safe, healthy learning environments.”

Until the late 1970s, PCBs were commonly used as insulators in electrical equipment because they have a high tolerance for heat, do not easily burn, and are non-explosive. EPA banned the processing and distribution in commerce of PCBs in 1979 pursuant to the Toxic Substances Control Act due to their toxic effects. However, uses of older PCB-containing ballasts were allowed to continue, provided that the ballasts had not failed and the PCBs were not leaking.

EPA believes many schools built in the U.S. before 1979 have light ballasts containing PCBs. A recent pilot study of three schools in New York City found that many light ballasts in the schools contained PCBs and had also failed, causing the PCBs to leak and contributing to increased levels in the air that school children breathe. EPA regional offices have also worked with school officials to address leaking PCBs in light ballasts in schools in Oregon, North Dakota, and Massachusetts.

Given their widespread use before they were banned, if a school was built before 1979 or has not had a complete lighting retrofit since 1979, the fluorescent light ballasts probably contain PCBs. Although intact, functioning ballasts do not pose a health threat, these lighting ballasts will all fail in time. For that reason, EPA recommends older PCB-containing lighting ballasts should be removed, whether as part of a previously scheduled lighting retrofit program or a stand-alone project.

Schools that have older ballasts should examine them to see if they have failed or if PCB leaks are present. If a light ballast is leaking PCBs, federal law requires the immediate removal and disposal of the PCB-containing ballasts and disposal of any PCB-contaminated materials at an EPA approved facility.

To prevent exposure if leaking ballasts are discovered, school personnel should wear protective clothing, including chemically resistant gloves, boots, and disposable overalls while surveying the ballasts. Replacement of leaking ballasts should be performed in a well-ventilated area, or supplemental ventilation or respiratory protection should be provided to reduce the potential for breathing in fumes.

While replacing lighting ballasts requires an upfront investment, there are state, federal and private funding programs available to potentially provide funding. In addition, replacing older ballasts with newer lighting fixtures will result in energy savings that will increase energy efficiency in schools and likely pay for itself in less than seven years, depending upon hours of operation and local energy costs.

EPA has also developed information on how to properly handle and dispose of PCB-containing fluorescent light ballasts and properly retrofit lighting fixtures to remove potential PCB hazards.

In September 2009, EPA issued guidance to communities about potential PCB contamination in the caulk of pre-1978 buildings. EPA also announced additional research into the potential for PCBs in caulk to get into the air. Research on that and other issues related to PCB exposures is ongoing.

School districts, building owners and others desiring technical guidance should contact EPA at 1-888-835-5372.
Parents who are concerned their children may be attending a school with PCB-containing ballasts should ask their schools whether they have a plan to address PCBs in their schools.

More information on PCBs: http://www.epa.gov/pcb

Information on handling and disposing of PCB-containing light ballasts: http://www.epa.gov/epawaste/hazard/tsd/pcbs/pubs/waste.htm

PCBs hotline: 1-888-835-5372

Source: U.s. Environmental Protection Agency (2010, December). EPA Issues National Guidance to Address Proper Maintenance, Removal, and Disposal of PCB-Containing Fluorescent Lights. Retrieved January 3, 2011 from http://yosemite.epa.gov/opa/admpress.nsf/0/6C03FDEC1E63274C8525780800693D7D

Types of Analysis to Detect Polychlorinated Biphenyls (PCB's)

Ask the Expert Question:

What types of analysis can be used to detect Polychlorinated Biphenyls (PCB’s)?

Experts Response:
PCB’s are normally reported on the basis of Aroclors, but can also be reported as congeners or homolog totals. The following will provide information on each.

Aroclors- Usually, seven to nine commercial mixes are evaluated and reported as total concentration for each Aroclor. This is always done by EPA Method 8082. There are some subtle differences among laboratories, but generally, the detection limit is determined by a statistical MDL, based on the analysis of seven low-spiked blanks. The RL must generally be above the MDL (usually by a minimum factor of 3), and must be supported by a valid calibration point. It is not uncommon for typical MDL’s to run from 0.1 to 0.5 ug/L, with RL’s running about 1 ug/L. This is the least expensive option for testing PCB’s.

Individual Congeners- Usually 12 to 64 individual compounds can be reported by method 8082 or the NOAA Status and Trends method.  As above for aroclors, detection limits are generally determined by a statistical MDL.  The RL must generally be above the MDL and must be supported by a valid calibration point. It is not uncommon for typical MDL’s to run from 0.3 to 0.8 ng/L, with RL’s running about 1 ng/L. This is the least expensive option for testing PCB’s congeners, although the price is considerably higher than PCB aroclors (above).

All 209 congeners, or any subset of them are also analyzed and reported by EPA Method 1668A or 1668B. The detection limit used here is a sample-specific signal-to-noise measurement performed for each analyte on the actual sample. Average detection limits run around 0.005 ng/L. Typical RLs run from 0.02 to 0.2 ng/L. This method is the most comprehensive and provides the lowest detection limits.  As a result, it is also the most expensive option for PCB analysis.

Homolog totals- These can be reported by a modification of EPA Method 8270. A homolog total is a result for all the congeners at a given level of chlorination. Typical detection limits from 0.0025 to 0.02 ug/L for individual homolog totals. The RL for the total of all homologs is 1 ug/L. This is the medium cost option compared with the other two methods.

If lower RL’s are needed, TestAmerica has a variety of options that can be explored such as higher sample volumes, clean hands/dirty hands techniques, etc.  These usually involve some modification to your sampling plan. 

Questions related to Mercury

Ask the Expert Question: 

What species of mercury is most commonly found in fish tissues?  Is it typically considered solid or is it dissolved mercury that they take in through their use of the water?

Expert Response: 

Methyl mercury is the most common mercury species that bioaccumulates in the food chain, but there have also been reports of other organo mercury species found in aquatic tissues. Although methyl mercury does have some water solubility, most of the methyl mercury accumulated in fish is from the food consumed by the fish rather than being absorbed directly from the water. So the mercury is ingested either as food or on solid particles consumed along with the food source.

Ask the Expert Question:

What is the solubility and volatility of methyl mercury?

Expert Response:

Physical properties for methyl mercury are available at this link:   http://www.scorecard.org/chemical-profiles/html/mercury.html.  The boiling point is about 357°C. Methyl mercury is considered insoluble in water. Measured concentrations in water are in the parts per trillion range or lower.

Ask the Expert Question:
What forms of mercury would you expect to see in an industrial scrap yard?

Expert Response: 

An industrial scrap yard could have a variety mercury species. Elemental mercury was commonly used in switches and other electrical equipment for many years. It was also common in thermometers and gas pressure measurement devices. Mercury was used in paint in various organic and inorganic forms. Mercury has also been a minor component in some metal alloys. Mercury was common in some batteries, lighting equipment and as an industrial catalyst. Thus, the specific mercury species would be highly dependent on the type of scrap brought in and how well segregated the scrap streams were.

 

Ask the Expert Question:

How well can the lab define the type of mercury that we are dealing with in the <100 ng/l range?

Expert Response: 

TestAmerica can measure total mercury down to 0.5 ng/L and methyl mercury down to 0.05 ng/L.  We do not currently have the capability to measure other mercury species.

Potassium permanganate to oxidize phenol from landfill leachate as treatment process

Ask the Expert Question: 

We would like to use potassium permanganate (KMnO4) to oxidize phenol from landfill leachate as a treatment process (i.e. reduce phenol below POTW required limits) prior to sending leachate to a local POTW. However, we are not sure what could potentially be formed when the KMnO4 oxidizes the phenol and how these subsequent formation products should then be removed. 

Expert Response: 

The reaction product of phenol and permanganate will be 1,4-benzoquinone. It is not regulated, and I suspect that it will be degraded in a biological treatment system. Since your treated leachate is going to a POTW, this should be sufficient to eliminate both the phenol and the by-product.

Ask the Expert Question: 

We also would need to know what potassium permanganate (KMnO4) would do to ammonia, cyanide, hydrogen sulfide and dissolved metals which are also present in the leachate at lesser concentrations than the phenol. 

Expert Response: 

Regarding the reaction of permanganate with the other constituents, I would expect ammonia to be oxidized to nitrate, cyanide to carbon dioxide and nitrate, and sulfide to sulfate. 

With the metals it would depend on the specific metals and their oxidation states.  For example, the leachate probably contains some dissolved ferrous iron because the landfill will be a reducing environment. The reaction with permanganate will convert this ferrous iron to ferric iron, and that would almost certainly result in a ferric oxide precipitate. These constituents are likely to react with permanganate more quickly than phenol, so you will have to add sufficient permanganate to oxidize these before you will get thorough oxidation of the phenol.

Blue ice for shipping laboratory samples

Ask the Expert Question: 

Can blue ice be used to ship samples to the laboratory?

Expert Response: 

The requirement is to receive environmental samples at 6 degrees Celsius. Any means that can ensure the 6 degree requirement would be suitable. However, it has been demonstrated that blue ice or cooler packs are very poor at lowering sample temperatures to the 6 degree requirement when the sample temperatures upon collection already exceed that temperature. This can result with sample temperatures being above the required temperature when received at the laboratory.

Ice however, will lower sample temperatures even when collected above the desired temperature if there is sufficient contact time between collection and receipt at the laboratory, and when there is sufficient ice to last the journey to the lab. Also, if the trip to the lab is short in duration, it may be necessary to chill the samples in the field prior to packing them for shipment.  Therefore, Ice is the preferred cooling mechanism, and some local enforcement bodies make it a requirement.