THE STANDARD – SEPTEMBER 2014
Chromium exists in multiple forms or “species” and can be analyzed as the total of all chromium species or as the hexavalent species. Chromium speciation is important because the hexavalent chromium species is considered toxic and a public health concern, while the other predominant species of chromium and trivalent chromium are considered relatively benign.
Prior to the early 2000’s, public health goals generally did not exist for hexavalent chromium. More recently, high profile movies, press coverage, and national studies have resulted in pressure on various Federal and State regulatory bodies to establish low public health concentration goals and maximum contaminant levels for hexavalent chromium in drinking water based on assessments of hexavalent chromium toxicity. In 2012, the US EPA issued in the Federal Register the final Unregulated Contaminant Monitoring Rule (UCMR 3). UCMR 3 requires larger public water systems to monitor for various chemical contaminants, including hexavalent chromium. Several states are considering, have proposed, or have established public health goals for hexavalent chromium at the micrograms per liter (µg/L) level. On July 1, 2014, the California Department of Public Health’s new drinking water standard for hexavalent chromium became effective. The maximum contaminant level (MCL) of 0.010 mg/L is equivalent to 10 µg/L and is 5x lower than the former total chromium MCL in California of 50 µg/L, which is itself half of the Federal MCL of 100 µg/L for total chromium.
As health standards for hexavalent chromium in water samples are being driven lower, the methods used to analyze for hexavalent chromium must also keep pace. Many hexavalent chromium methods are based on hexavalent chromium forming a colored complex with 1,5-diphenylcarbazide (DPC). This approach is used in various methods such as US EPA Methods 7196A and 7199, US EPA Method 218.6, and US EPA Method 218.7. The lower limits have fueled a technological push to “tweak” the existing methods to new levels of sensitivity. Method 218.6 was introduced in 1994 for wastewater analysis, but modified in 2003 in response to anticipated demand for lower limits. The modifications involved increasing sample size, lowering instrument flow rates, and modifying a buffer used in the procedure. The minimum reporting levels, as published in 1994, were approximately 1 µg/L or higher. By 2003, the minimum reporting levels were lowered to approximately 0.2 µg/L and additional modifications in 2011 pushed the minimum reporting levels to 0.02 µg/L. Method 218.7 incorporating the refinements of Method 218.6, was introduced in 2011 for drinking water samples. Method 218.7 uses a less concentrated buffer to improve method performance. The minimum reporting level in Method 218.7 is still approximately 0.02 µg/L, but samples properly preserved in the field have an extended holding time, compared to earlier methods.
It is not known if the current methods will need to “see” lower in the future. There are several specialized techniques available that may offer similar sensitivity or offer definitive specificity for hexavalent chromium and trivalent chromium. These techniques include, speciated isotope dilution mass spectrometry (SIDMS) which offers similar sensitivity as Method 218.7, but chromium species conversions during sample analysis can be tracked and corrected. Additionally, x-ray absorption near edge structure (XANES) spectroscopy has been successfully applied to solid samples, eliminating the need for an extraction step.
Environmental Standards has helped numerous clients navigate the complex challenge of chromium speciation. We answer unique, specialized questions and to solve perplexing problems that our clients may encounter.
Contact Environmental Standards to learn how we can help you select the appropriate method for your speciation requirements and implement programs to ensure quality data are produced.
The US EPA released a proposed rule which will update the standards for petroleum refineries that release hazardous air pollutants, requiring them to monitor benzene concentrations around the fenceline of their facilities, reduce flaring, and improve emissions controls. The proposed rule was published in the Federal Register on June 30, 2014.
Environmental Standards’ clients, and all refineries, will benefit from focusing on, and being concerned with, quality assurance while meeting the proposed fenceline benzene monitoring requirements. US EPA is proposing to establish an ambient concentration of benzene at the fenceline that would trigger required corrective action in the event of an exceedance. According to the Proposed Rule, costs for the fenceline monitoring methods are dependent on the sampling frequency (for passive and active monitoring locations) and the number of monitoring locations needed based on the size and geometry of the facility. The proposal identifies an annual average benzene concentration standard to be measured via 2-week integrated samples at the refinery fenceline perimeter. Twelve to 24 monitors are required at each facility, dependent on facility size.
The proposal suggests that fenceline data at each monitor location be reported electronically within 45 days of the end of each semi-annual period, and data will be made available to the public.
Based on Environmental Standards’ prior experience with benzene analyses, the amount of data and concentrations of benzene will challenge current analytical methods. We recommend that now is the time to start implementing quality assurance programs to ensure training of sampling personnel, instrument calibration and laboratory qualifications, accurate and defensible results, and properly managed and easily accessible data.
US EPA estimates that the rules will require a capital investment of $240 million, and recurring annual costs of $40 million for all of the nation’s refineries. The cost of building quality assurance into the process and periodically checking it on the back end will be relatively insignificant. If you’re curious about the QA process and how Environmental Standards can help, contact Technical Director of Chemistry/Principal Rock Vitale, CEAC at 610.935.5577.
Public comments on the proposed rule were due August 29, 2014. US EPA held public hearings on July 16, 2014, in Wilmington, California and on August 5, 2014, in Galena Park, Texas. A decision on a final version of the rule is expected by April 17, 2015.
Update: EPA has extended the public comment period for the proposed Petroleum Refinery Risk and Technology Review and New Source Performance by 60 days; the comment period will now close October 28, 2014.
Environmental Standards performs quality monitoring activities for many industrial clients’ corporate laboratory programs. The quality monitoring activities, on-site laboratory audits, performance evaluation studies, and data validation are performed to ensure laboratory compliance to project and client-specific requirements. Corrective actions are often required based on findings identified during the various audits. In some instances, the identified findings and implemented corrective actions have wider applicability than just the individual client or laboratory facility.
A recent performance evaluation (PE) study performed on behalf of an industrial client revealed a flaw in the laboratory’s quality system and, specifically, in their data review procedures. When reporting the results for the PE sample, the laboratory reported one of the chlorinated organic compounds certified to be present in the PE sample as “not-detected.” Environmental Standards requested laboratory management to investigate the misreporting for this compound. The laboratory personnel determined that the compound was in fact present and should have been reported, but was marked as “not-detected” by the analyst. When queried why this was not observed during the internal peer review performed at the laboratory, laboratory quality assurance (QA) personnel indicated that although they have an internal peer review process, the review is performed on raw data which only include the detected compounds that were reported in the sample.
Because this compound was reported as “not-detected,” it was not included in the raw data provided to the peer reviewer and thus no confirmation or second level of review was performed for compounds manually deleted by the analyst. The laboratory recognized that this was a flaw in their quality system which needed to be addressed. Laboratory personnel implemented programming company-wide to include all edits made to the data by the initial analyst in the raw data that are included for peer review.
The various quality monitoring services provided by Environmental Standards are performed to assure high quality data are generated through the preparation, analysis, and reporting phases of a project. Catching potential errors, such as the reporting error discussed above, early on in the project can save time, money, and frustration.
Environmental Standards was recently awarded a contract by the Marcellus Shale Coalition (MSC) to coordinate and oversee an inter-laboratory study for the analysis of dissolved gases (e.g., methane) in groundwater samples.
While there are several published analytical methods for the analysis of dissolved light gases in the aqueous medium, there is not currently a US EPA published method for dissolved gases. For the published procedures that do exist (e.g., RSK-175), these methods do not provide adequate specificity for a significant number of sampling, volume, temperature, and calibration variables that can substantially impact the quantitative analysis of samples.
Given the substantial increase in oil and gas exploration on the shale plays throughout the US, the analysis of dissolved gases to establish a baseline in comparison with post completion groundwater samples has become increasingly important for regulatory and legal purposes. With the growing number of commercial and regulatory laboratories performing dissolved gas analysis, significant differences have been routinely noted during split sampling investigations. Consistent with its guiding principal of “implementing state-of-the-art environmental protection across all of their operations,” the MSC has proactively taken on this initiative.
The goal of the study is to identify those critical variables that influence commercial laboratories’ quantitation of dissolved gases in groundwater. Environmental Standards’ professional geoscientists will prepare the split samples to ensure minimal variability of the sampling process. Based on the inter-laboratory data collected and subsequent data analysis, a final report will be prepared that describes the major factors influencing the variability observed with dissolved gas concentrations reported by each of the participating laboratories.
This study will have national importance and the results will likely lead to a highly specific consensus standard for the analysis for light gases in groundwater. In addition to the MSC, a number of stakeholders, including state and federal regulatory agencies and bodies that set industry standards, will be either participating or following the study.
News from our subsidiary, Vitale Scientific Associates, LLC
The Food Safety Modernization Act (FSMA), signed into law on January 4, 2011, enables the Food and Drug Administration (FDA) to better protect public health by helping to ensure the safety and security of our Nation’s food supply.
The vision of FSMA is prevention – preventing food safety problems before they occur, rather than reacting to problems after consumers are exposed. FSMA also gives the FDA important new tools and powers to hold importers accountable for verifying, in a manner transparent to the FDA, that the food they import is safe. Below is a series of new proposed rules and the deadline for their publication under review that will likely have a major impact on both domestic and foreign food companies. This article highlights the timetable for the major milestones in FSMA and provides a brief synopsis of each category.
Preventive Controls. All registered facilities will be required to conduct a hazard analysis, implement preventive controls, and develop a food safety plan to document monitoring, correction, and verification of preventive controls. The food safety plan and all related documents must be made available to the FDA during inspections. As part of its food safety plan, a facility for human food may be required to document sanitation procedures, a recall plan, a food allergen control program, supplier verification activities, and environmental sampling and testing. Facilities producing animal food would be required to have written plans that identify hazards, specify the steps that will be put in place to minimize or prevent those hazards, identify monitoring procedures and record monitoring results, and specify what actions would be taken to correct problems that arise. The proposed rule would also establish certain Current Good Manufacturing Practices (CGMPs) that specifically address animal food. Anyone who manufactures, processes, packs, distributes, receives, holds, or imports food must be in compliance with this provision.
Foreign Supplier Verification Program. In the first year following enactment, the FDA must inspect at least 600 foreign facilities and must double the number of inspections every year compared with the previous year for the next 5 years. Thus, the FDA has to inspect 600 foreign facilities in 2011 and increase the number of foreign inspections to 19,000 in 2016. With current resources, it will be nearly impossible for the FDA to meet inspection frequencies. The Agency likely will look to other federal, state, or local inspectors to assist the FDA in meeting the inspection frequency requirements for domestic firms.
Produce Safety. Produce safety applies to all farms that grow, harvest, pack, or hold produce that will be consumed in the United States. This includes both farms in the US and those that export to the US. FDA has taken the approach that there are certain core elements that apply to all farms: agricultural water, biological soil amendments, control of animals, sanitation of equipment and tools, and buildings and personnel issues (including training and hygiene). Under the proposed rule, farms would be required to identify reasonably foreseeable biological hazards (as opposed to chemical or physical) and take appropriate science-based measures to minimize these risks. The proposed rule is expected to affect more than 40,000 farms.
Food Defense. The FDA’s proposed rule on food defense would require domestic and foreign facilities to address vulnerable processes in their operations to prevent acts on the food supply intended to cause large-scale public harm. The proposed rule, which is required by the FDA’s Food Safety Modernization Act, would require the largest food businesses to have a written food defense plan that addresses significant vulnerabilities in food operation.
Sanitary Transport. The FDA is required to issue regulations to require that shippers, carriers by motor vehicle or rail vehicle, receivers, and other persons engaged in transportation of food to use sanitary practices. The FDA proposed rule addresses separation of food and non-food cargoes, temperature controls, preventing contamination with allergen residues, and maintenance of shipping records. The FDA is also required to conduct a study of transportation of food in the United States, including transportation by air and an examination of the unique needs of rural areas with regard to the delivery of safe food.
According to an article published in The Gold Sheet1, the number of drug recalls increased by over 300% between 2008 and 2009 as the Food and Drug Administration (FDA) tightened their scrutiny of quality control practices within the drug manufacturing process. This, combined with the normal background of product quality issues, produced over 1,700 recalls in two years. The flux in recalls appeared to stem primarily from the rush by generic drug makers to reach the market first, resulting in a lack of investment into adequate manufacturing and analytical methods that were essential to maintaining quality control of the product. In order to limit the susceptibility of manufactured drugs and excipients to economically-motivated adulteration (EMA), the FDA assembled a Task Group in 2010 that focused on identifying current US Pharmacopeial Convention (USP) monographs that have been problematic due to the reliance on outdated analytical techniques that are unfit for purpose when applied to the testing of prescription (Rx) or over-the-counter (OTC) drugs.
In response to the FDA’s concerns, the USP launched a global initiative to modernize and improve many existing monographs for drug substances and drug products in the United States Pharmacopeia and the National Formulary (USP-NF). In 2011, the USP formed the Impurities in Drug Products Expert Panel to align current scientific and regulatory practices so that product quality and control of impurities can be monitored through a scientifically-based approach. The panel sought the opinions of over 20,000 stakeholders and this resulted in the generation of a new general chapter used to ensure the proper control of organic impurities (Organic Impurities in Drug Substances and Drug Products), and also triggered the USP to launch other modernization initiatives targeting additional areas of concern such as detection of toxic trace elements and residual solvents. Altogether, as of July 2014, there are more than 500 monographs on the USP’s Monographs in Need of Modernization list that are undergoing the process of modernization in order to improve current performance and efficiency.
The FDA and the USP recognized that in order to maintain quality control in the pharmaceutical industry, the current compendia had to be modernized and regulations had to be tightened. This was echoed by the record high of 2,300 recalls that were issued in 2011, and continued into 2013 when more than 1,200 recalls were distributed. However, the number of recalls due to inadequate manufacturing and the associated analytical methods has continually declined from 1,384 in 2009 to only 103 in 20131. This shows that the industry is benefiting from the steps being taken by the FDA and USP to modernize current monographs with the intent to ensure adequate testing of drug substances and drug products. Still, it is an expensive progression to maintain quality control through an appropriate analytical testing program, especially for drug compounds that do not have associated USP monographs. Yet, the expense is minimal in comparison to having products recalled, applications rejected, and reputations tarnished for lack of quality compliance.
The use of outdated or obsolete analytical methods to characterize drug substances and drug products has proven to be a costly approach resulting in tragic consequences for the drug developers and especially the customers. Even so, the wait that drug developers have endured for the monograph modernization effort has already been painfully long. The need for individual New Drug Application (NDA) and Investigational New Drug (IND) development needn’t necessarily wait.
The experienced pharmaceutical chemists at Vitale Scientific Associates, LLC (VSA) can provide alternative testing protocols that take advantage of improvements in analytical instrumentation and techniques. We help our clients improve the overall cost and efficiency of their quality control systems through the development and validation of successful alternative testing protocols and the strategic and customized integration of our Modular Quality Management System (MQMS). We have developed high-quality, scientifically-sound, and cost-efficient quality control programs that have resulted in 20 to 30 percent annual savings in analytical costs for our clients. Look forward to future articles in this series on quality control that will focus on the consequences of using inadequate analytical methods for drug characterization, and the benefits of implementing modern technologies into your analytical testing program. For more information regarding this article or our MQMS, please contact Quality Assurance Chemist/Associate Principal David Thal, CEAC or Senior Scientist Dr. James Markwiese at 865.376.7590.
1Bowman Cox, “Drug Recalls Soared Again in 2013, Driven by Contamination,” The Gold Sheet, May 2014.
Shale rock, the dense formations found to hold immense reserves of oil and gas, holds hope for our nation’s energy independence. However, shale often contains elevated concentrations of radium, a radioactive element. Hydraulic fracturing displaces potentially radium containing subterranean water, forcing it up through the wells, where it can taint drill cuttings, flow back water, and surface equipment. Radiation levels can also accumulate in sludges at the bottom of tanks, pipeline scale, and other material that comes in extended contact with the wastewater. The term for these constituents is Technologically Enhanced Naturally Occurring Radioactive Materials (TENORM).
Based on state disposal records and industry production, millions of tons of TENORM are being generated each year. Disposal practices vary from state to state and company to company. According to Thomas Aluise, a spokesperson for the West Virginia Department of Environmental Protection (WV DEP), “a lot of operators were just burying them on-site, unchecked, all over the state.”
Currently, state regulators are caught between environmental and public health groups demanding more regulation, and the energy industry, which says it’s already taking proper precautions. In response to public pressure and evidence of negligent disposal practices by a few members of the industry, West Virginia, Pennsylvania, and North Dakota are revising limits for acceptable radiation levels of TENORM and strengthening disposal rules.
On July 10, 2014, the WV Secretary of State approved the WV DEP Solid Waste Management Emergency Rule (33 CSR 1), which took effect immediately. The emergency rule establishes procedures for the acceptance, handling, and disposal of TENORM.
All solid waste facilities that accept TENORM for disposal must install fixed radiation detection equipment. The fixed detector must be capable of measuring exposure rates from ten microroentgens per hour (10 µR/hr) to greater than fifty milliroentgens per hour (> 50 mR/hr.). If a load of drill cuttings or associated waste is confirmed to be less than 10 µR/hr, considered average local background level, the waste may be disposed of in the facility. If the load of waste is confirmed to be equal to or greater than 10 µR/hr, a combined concentration of radium-226 and radium-228 must be determined.
The combined radium-226 and radium-228 concentration must be analyzed by a State approved method. If the combined concentration in the waste is less than five picocuries per gram (5 pCi/gr), considered average local background level, the waste may be disposed in the facility. If the concentration is greater than 5 pCi/gr, the load must be rejected.
If solid wastes cannot be managed at a solid waste landfill because of elevated levels of TENORM, the waste must be sent to a permitted radioactive waste disposal facility.
Next Article: Frack to Fill to Fail. The Importance of Radium-226 and Radium 228-Sample Collection and Method Selection.
Written by Quality Assurance Specialist/Associate Principal David I. Thal, CEAC.
There has been a notable surge in acquisitions of US environmental laboratories over the last 3 ½ years, much of it due to the globalization affecting business at large. It was no great challenge to identify 27 laboratory companies purchased since 2010 (see list below).
This is a mixed blessing. Laboratory firms become more skilled and stronger through acquisition; they build their intellectual assets through the acquisition of procedural knowledge and the interaction of scientists, technicians, and business managers who benefit from observing and researching in multiple systems. Good laboratory firms are more frequently acquiring and being acquired, than weak ones. The seasoned laboratory client understands the value of this process, but knows that everyone must increase vigilance during the transition.
“That which does not kill us makes us stronger,” wrote Nietzche. Anyone who has been through an environmental laboratory merger or acquisition as a client, a laboratory acquirer, or a laboratory acquired will affirm that it is a great opportunity for learning, and for chaos. Have you ever heard the term “growing pains” used to explain why the analysis is complete, but the report will take some time as new formatting glitches are ironed out? Ever encounter invoice confusion during and after integration of accounting systems? Ever scratch your head because you sent the sample to the laboratory in Memphis and the report comes back from Omaha, but you find out somehow that most of your work was performed in Vancouver?
How about this one? “The application of the dilution factor is done in the new laboratory information management system (LIMS) and because this particular test is performed in an area of the laboratory with a legacy software configuration, the dilution factor was applied twice. The problem has been identified and we have taken steps at a system level to prevent anything like this from happening again.” These glitches aren’t simple oversights. They may occur in generally very well-managed integrations. The point is that integrating a full service laboratory incorporates so many processes that even herculean planning and review can become overwhelmed by the complexity.
During my career in the laboratory industry, I worked in one laboratory that had been acquired 11 times in 23 years, and for another firm that operated under four owners over the course of my 19 years there. I have seen elegant, well-managed transitions, and others that seemed to be designed to create chaos and disruption. My observation is that successful laboratories have generally built their processes around the needs of their market and then have built systems around their processes. So when an acquiring laboratory tries to incorporate a type of analysis it has not previously managed or tries to incorporate services to a market it has not served before, the complexity and schedule for the integration expands significantly. Integrations optimistically scheduled for completion within a few weeks can actually take months or years! This is an industry-wide phenomenon. While those with more experience in acquisition and integration have some clear advantages, no laboratory company should be considered to be immune. In some cases, the managers who oversaw the previous integrations have themselves moved on.
If you are using a laboratory that has been acquired, is acquiring, or is being acquired, consider moving your audit cycle around to bring it up in the rotation. If this conflicts with other program needs, consider a special purpose audit or investigation to understand how the acquiring firm is addressing management of change, novation of contracts, integration planning, integration of quality systems, integration of operations and systems (LIMS, Accounting, Reporting), consolidation and transfer of operations, evaluation of conflicts-of-interest, and conflict-of-interest resolution.
Notable Environmental Laboratory Consolidations (2010-2014)
- SPL (Traverse City, MI; Lafayette, LA; and Houston, TX – January 2011)
- Entech, Evergreen, Southwest Water (2008-2009)
ALS Global acquired:
- Analytical Laboratory Services (Middletown, PA early 2011)
- Columbia Analytical Services (Kelso, WA; Houston, TX; Rochester, NY; Jacksonville, FL; Simi Valley, CA – November 2011)
- DataChem (Cincinnati, OH; Salt Lake City, UT; 2013)
Element Materials Technology acquired:
- Sherry Laboratories (Daleville, IN; South Bend, IN; Columbus, IN; Scott, LA; Lafayette, LA; Houma, LA – March 2013).
- Quantus Analytical (Cincinnati, OH – June 2012)
- Advanced Scientific Laboratories (Pompano Beach, Orlando & Miami, FL – September 2010)
- BioHygiene Laboratories (Torrance, CA – April 2009)
Eurofins Scientific (EUFI.PA) acquired:
- Frontier Global Sciences (Bothell, WA – September 2012)
- Eaton Analytical (former MWH) (Monrovia, CA – September 2012)
- UL (Drinking Water Laboratory) (South Bend, IN – March 2014)
- Air Toxics (Folsom, CA – February 2012)
- Lancaster Laboratories (Lancaster, PA – February 2011)
- Calscience (Garden Grove, CA – May 2014)
Pace Analytical Services acquired:
- Microseeps (August 2013)
- Zymax (Escondido, CA – August 2013)
- Pocono Environmental Laboratories
- Tritest (Raleigh, NC – June 2012)
- Heritage (Indianapolis, IN – September 2013)
- Braun Intertec (Minneapolis, MN – July 2014)
- Xenco (Boca Raton – July 2011)
- Enviroscan Analytical – Rothschild, WI (Assets Purchased)
- ERMI Environmental Laboratories (Allen, TX – November 2011)
- NTC Laboratory Services (Virginia, MN – April 2011) (Assets Purchased)
- Prior to 2011 – Laucks, Northeast Analytical Laboratories, Alpha Omega, ELAB, Northern Analytical Laboratories
SGS North America acquired:
- Analytical Perspectives (Wilmington, NC – April 2012)
- Galson Laboratories (Syracuse, NY – July 2014)
- Herguth Laboratoires (Vallejo, CA; Naperville, IL – January 2013)
- Environmental Testing Corporation (September 2011).
In May 2014, Eurofins Environment Testing US of Lancaster, Pennsylvania, acquired Calscience Environmental Laboratories, Inc., located in Garden Grove, California. Calscience is now known as Eurofins Calscience, Inc.
Galson Laboratories was acquired by SGS SA, the company announced on August 7, 2014. Galson Laboratories, an SGS Company, will become the SGS Center of Excellence for Industrial Hygiene Lab Services within its global network. Galson Laboratories operates and is headquartered in Syracuse, NY, with five strategically located service centers.
Wisconsin DNR’s Lab Certification Program completed a review of existing state reciprocity agreements in 2013. At that time, the Program concluded that except for South Carolina, all reciprocal agreements would be terminated for not meeting the “substantial equivalence” test. After additional review, Wisconsin has decided to terminate the reciprocal agreement they had with South Carolina.
Four Massachusetts laboratory companies that perform commercial-scale environmental testing have agreed to pay a total of $1.75 million for allegedly failing to obtain required state permits and control their hazardous air pollutant emissions. Alpha Analytical, Inc., Accutest Laboratories of New England, Inc., Spectrum Analytical, Inc., and Con-Test Analytical Laboratory must also comply with state air permitting requirements and install emission control equipment for sample analyses that will reduce hazardous air pollutant (HAP) emissions by 95 percent.