Pharmaceutical Manufacturing Industry (PMI) Wastewater Monitoring

The Environmental Protection Agency's standards for wastewater discharges are listed under Pharmaceutical Effluent Guidlines in 40CFR439. The analytical procedure for volatile organics by isotope dilution GCMS is published in method EPA 1666A.  Certain volatile, water-soluble organic compounds do not purge well from water and are analyzed by direct aqueous injection while the remainder are analyzed by the purge & trap introduction technique. Weck Laboratories now offers both purge & trap and direct injection EPA 1666A.  Compound list

Now Accredited in the State of New Jersey for Organic Analysis

New Jersey Department of Environmental Projection has issued a NELAP certificate to Weck Laboratories for the Organic Analysis categorgy.  

Download the NJDEP certificate here. 

 

Determination of Taste & Odor Causing Compounds, Geosmin and MIB in Water

Geosmin and 2-Methylisoborneol (2-MIB) are two of the most commonly occurring chemicals attributed to the unpleasant taste and odor characteristics of drinking water. In addition to water, they also contribute to a distinct earthy taste in wine and certain fish species.  These compounds are primarily formed intracellularly in bluegreen algae (cyanobacteria) and actinobacteria, and are released upon cell destruction. Although taste and odor problems are not considered a direct threat to public health, they are of great concern for many water utilities because consumers generally rely on the taste of their water as the primary indicator of its safety. Since the human nose is able to detect these compounds at low concentrations as low as 10 ng/L (ppt), the need to identify these compounds at lower levels is an important priority. With this in mind, Weck Laboratories has developed a sensitive and robust analytical method for the quantitation of Geosmin and 2-MIB using the latest GC/MS technology, incorporating state-of-the-art automated solid phase micro-extraction (SPME) in conjunction with target-specific chemical ionization tandem mass spectrometry (CI-MS/MS). With the implementation of this method, Weck Labs is able to detect these compounds below human sensory thresholds and has established a reporting limit of 1 ng/L for both Geosmin and 2-MIB.  Geosmin & MIB Data Sheet.

Analysis of PPCPs/EDCs for Groundwater Recharge-Reuse Program

While recycling is a term generally applied to aluminum cans, glass bottles, and newspapers, water can be recycled as well. Water recycling is reusing treated wastewater for beneficial purposes such as agricultural and landscape irrigation, industrial processes, toilet flushing, and replenishing a ground water basin (referred to as ground water recharge).  More from EPA Region 9 on Water Recycling and Reuse: The Environmental Benefits.

Weck Laboratories has again expanded it's target compound list for the Pharmaceutical, Personal Care Products and Endocrine Disruptors suite.  With the addition of three new analytes, the suite now covers virtually all of the suggested representative contaminants from the California Department of Public Health (CDPH) Drinking Water Program's draft regulations forGroundwater Recharge Reuse dated August 5, 2008.

Newly Added Pharmaceuticals
Amoxicillin  [antibiotic]
Dilantin (Phenytoin)  [anticonvulsant]
Iopromide  [x-ray contrast agent]
 
See all compounds here...

These suggested indicator chemicals are listed in endnote 5 - Additional Constituent Monitoring for Pharmaceuticals, endocrine disruptors, and other wastewater indicator chemicals.  The categories are hormones, industrial endocrine disruptors, pharmaceuticals, personal care products and other chemicals.

EPA 1640 Ultra-Trace Metals by ICPMS

Determination of Trace Elements in Water by On-Line Chelation Preconcentration and Inductively Coupled Plasma-Mass Spectrometrysma-Mass Spectrometry.  Weck Laboratories has developed all three sample pre-treatment options within the method which employ co-precipitation, reduction or ion exchange pre-concentration.  These steps remove the saline matrix which significantly reduces interferences and enhances the detection limits. 

PFOS / PFOA Analysis by LCMSMS

Perfluorinated compounds (PFCs) are ubiquitous carcinogenic chemicals which have many uses, including the synthesis of fluoropolymers such as Teflon®, industrial surfactants, lubricants, waxes and adhesives, among other products—with an estimated worldwide production of 5-6.5 million kg/year. The discovery of several PFCs in coastal waters both near industrial centers, and in remote environments, as well the detection of PFCs in human blood serum and in the tissues of aquatic animals has sparked concern as to the global fate of this common contaminant.  Recently, several of these PFCs have been discovered in drinking water supplies near a West Virginia manufacturing plant and near a Decatur, AL treatment plant, prompting the USEPA to issue a provisional health advisory for perfluorooctanoic acid (PFOA) at 0.4 μg/L and perfluorooctane sulfonic acid (PFOS) at 0.2 μg/L, which is ten times higher than the guidance level in New Jersey.  Weck Labs has developed a sensitive method for the analysis of two of the most common PFCs: PFOA and PFOS, which serve as representative indicators. Through the use of SPE concentration and tandem LC-MS, Weck Labs has been able to achieve reporting limits of 5 ng/L (0.005 μg/L).   PFOS/PFOA data sheet.

Determination of Melamine and Cyanuric Acid by LCMSMS

Melamine and cyanuric acid are nitrogen rich compounds which have been used as adulterants in a means to artificially inflate the protein content in imported food products. When found individually, melamine and cyanuric acid are not toxic; however, when combined in the bloodstream, they accumulate in the kidneys and form very large insoluble crystals (melamine cyanurate), which in turn can lead to renal failure and ultimately, death. This toxicity has prompted the U.S. FDA to set a standard for human consumption at 0.063 mg per kg of body mass per day(1). In an effort to determine the extent of this contamination, Weck Labs has developed a highly sensitive method for the quantification of melamine and cyanuric acid in aqueous matrices through the use of direct injection LC-MS/MS, achieving reporting limits of 1 μg/L.  Melamine & Cyanuric Acid data sheet.

Determination of Bicine in Gas Treating Amine Solutions by ICMS

 As a degradation product of alkanolamine and alkylalkanolamine solutions, N-N-bis(2-hydroxyethyl)glycine, also known as bicine, is commonly found in gas treating amine solutions. The proposed pathways for the formation of bicine in amine solutions are all from alkanolamines and alkylalkanolamines such as DEA and MDEA. For example, some possible pathways are by either reacting DEA with glyoxal or through direct oxidation of DEA, MDEA, or TEA by O2 or SO2.  Studies have shown that high levels of bicine contribute to the formation of Heat Stable Amine Salts (HSAS), and to the corrosion of amine plant equipment.  HSAS have been shown to contribute to the corrosivity of amine solutions when present in concentrations of 1000 to 250 ppm, and bicine itself has been identified as a chelator which can initiate a rapid corrosion process in the presence of H2S.  An effective removal system combined with frequent testing are important aspects of reducing costs associated with gas treating.  Weck Labs has developed an efficient, robust, and precise method for the determination of bicine in gas treating amine solutions as low as 20 mg/L (ppm) by ion chromatography coupled with tandem quadrupole mass spectrometry.As a degradation product of alkanolamine and alkylalkanolamine solutions, N-N-bis(2-hydroxyethyl)glycine, also known as bicine, is commonly found in gas treating amine solutions. The proposed pathways for the formation of bicine in amine solutions are all from alkanolamines and alkylalkanolamines such as DEA and MDEA. For example, some possible pathways are by either reacting DEA with glyoxal or through direct oxidation of DEA, MDEA, or TEA by O2 or SO2.  Studies have shown that high levels of bicine contribute to the formation of Heat Stable Amine Salts (HSAS), and to the corrosion of amine plant equipment.  HSAS have been shown to contribute to the corrosivity of amine solutions when present in concentrations of 1000 to 250 ppm, and bicine itself has been identified as a chelator which can initiate a rapid corrosion process in the presence of H2S.  An effective removal system combined with frequent testing are important aspects of reducing costs associated with gas treating.  Weck Labs has developed an efficient, robust, and precise method for the determination of bicine in gas treating amine solutions as low as 20 mg/L (ppm) by ion chromatography coupled with tandem quadrupole mass spectrometry.  Bicine data sheet.

ASTM D6646 - Determination of the Accelerated Hydrogen Sulfide Breakthrough Capacity of Activated Carbon

This method compares the performance of granular or pelletized activated carbons used in odor control applications, such as sewage treatment plants, pump stations, etc. The method determines the relative breakthrough performance of activated carbon for removing hydrogen sulfide from a humidified gas stream.  This test method is intended to evaluate the performance of virgin, newly impregnated or in-service, granular or pelletized activated carbon for the removal of hydrogen sulfide from an air stream, under laboratory test conditions.  A humidified air stream containing 1 % (by volume) hydrogen sulfide is passed through a carbon bed until 50 ppm breakthrough of H2S is observed. The H2S adsorption capacity of the carbon per unit volume at 99.5 % removal efficiency (g H2S/cm3 carbon) is then calculated. 

LCMSMS Capacity Expanded! 

Weck Laboratories has added a 2nd new LCMSMS system.  The Applied Biosystems 4000 QTrap is a high performance ion trap and a high sensitivity triple quadrupole mass spectrometer in one system.  It's primary use is for new methods development and for pharmaceuticals, personal care products & endocrine disruptors analysis.  Our PPCP/EDC target compound list is now expanded with lower detection limits.  Our first LCMSMS, a Varian 1200L system, runs routine samples for EPA 535 UCMR2 and EPA 331.0 perchlorate. 

Acrylamide Analysis by LCMSMS

Acrylamide is primarily used as a coagulant to aid in the filtration of drinking water & wastewater during treatment. Other uses of include improvement of production from oil wells; in making organic chemicals and dyes; in the sizing of paper and textiles; in ore processing; in the construction of dam foundations and tunnels.  It is measured at Weck Labs by direct-injection Liquid Chromatography-Tandem Mass Spectrometry (LCMSMS) with a reporting limit of 0.1 ug/L.

Weck Laboratories has received the ACIL Seal of Excellence & Special Recognition for being in the "Top Five" labs in Proficiency Testing scores for 2008

This program provides users with a mechanism for evaluating environmental testing laboratories. Participants are committed to ensuring the integrity of data, meeting customer's quality needs and setting the standards of performance for the testing laboratory industry.  Any environmental testing laboratory who wants to be recognized as a participating laboratory must maintain proof of an annual ethics training and an early detection system for questionable analytical practices, submit a signed code of ethics and twelve months of Proficiency Testing (PT) scores, and distribute satisfaction surveys to their customers.

 
The participants have committed to a uniform code of ethics and provide Performance Evaluation data and Customer Survey data for comparison to other participants. The Seal of Excellence participants demonstrate that they are proud of the quality they achieve and always operate with customer service as a top priority.  The results of the program's PT scores, customer satisfaction scores, list of Seal of Excellence Qualified Participants and the laboratory contact information are made public. All other customer information is held in the strictest confidence between the laboratory and the program administrator. 

The Award is presented to laboratories scoring greater than 90% on the combined average of all the PT studies for the previous twelve months and ranked better than 3 on overall customer satisfaction and timeliness as measured by the Seal of Excellence Survey.  The Twelfth annual Seal of Excellence Awards were presented at the ACIL Annual Meeting on October 13, 2008.  For additional information on the Seal of Excellence program contact the Program Administrator
at (302) 368-1211 or email mmoore@advancedsys.com.

We've been busy at the lab bench!

Our staff here at Weck Laboratories has been busy with new method development, facility expansion and process automation.  Our expansion includes approximately 500 square feet of additional radiochemistry space including a new sample preparation hood. 

Pharmaceutical & Personal Care Products (PPCP) & Endocrine Disruptor Compounds (EDC)

Our method development chemists have developed analytical procedures for surveying water sources for the presence of trace levels of Endocrine Disruptor Compounds (EDCs) and Pharmaceutical and Personal Care Products (PPCPs). These include reproductive hormones, flame retardants, alkyl phenols, opiates, analgesics, stimulants, anti-convulsants, statins & plasticizing agents. The various methods employ solid phase extraction and Gas Chromatography/Mass Spectrometry (GCMS) and Liquid Chromatography /tandem Mass Spectrometry (LCMSMS).  Detection limits range from the low parts per billion (ug/L) to the low parts per trillion (ng/L).

USEPA Unregulated Contaminant Monitoring Rule No. 2  (UCMR2)

Weck is one of the first and few laboratories in the nation to be approved for all 5 Methods.  The Unregulated Contaminant Monitoring Regulation supporting the second cycle (UCMR 2) of monitoring was signed on December 20, 2006. The UCMR 2 requires monitoring for 25 contaminants using five analytical methods during 2008-2010.  Public water systems (PWSs) are responsible for their laboratories, and must ensure they are following the methods and meeting the quality control (QC) criteria specified in UCMR 2. Laboratories must post sample analytical results and required QC data electronically via the Safe Drinking Water Accession and Review System (SDWARS).

Ultra Low-Level Pyrethroid Pesticides by GCMS-NCI-SIM 

Environmental monitoring of pyrethroid pesticide residue is becoming an increasing concern in stormwater, agricultural run-off, and sediments as some organophosphorus pesticides are replaced with pyrethroids.  Very low levels, down to 10 nanograms per liter in water and 0.5 micrograms per kilogram in soil can be detected via Selected Ion Monitoring (SIM) mode Negative Chemical Ionization (NCI) Gas Chromatography/Mass Spectrometry (GCMS).  Target compounds and limits are listed here...

Low-Level Poly-Chlorinated Biphenyl (PCB) Congeners by GCMS-SIM

Weck is currently capable of determining the concentration of 25 of the 209 possible congeners of PCB at 10 ng/L (ppt) levels.  The congeners range from 2,4'-Dichlorobiphenyl to Decachlorobiphenyl.  The target compounds are removed from water samples by automated Solid Phase Extraction (SPE) and are analyzed by electron impact ionization GCMS in the Selected Ion Monitoring (SIM) mode.  

Low-level Perchlorate by ICMSMS or LCMSMS

Weck Laboratories has been performing the above two liquid chromatography-tandem mass spectral methods since 2006 and has analyzed over 1300 samples!  Recently the California Department of Public Health added two new methods to their certification process.  Weck has been approved for EPA 331.0 LCMSMS and EPA 332.0 ICMSMS techniques for low-level perchlorate to 0.1 ug/L in water.  Note that these two methods require a sterile sampling procedure using sterile syringe, 0.2 micron filter and bottle.  Please contact a laboratory project manager for details.

para-Chlorobenzensulfonic Acid (pCBSA)

pCBSA is a by-product from the manufacturing of the banned pesticide DDT.  It is measured at Weck Labs by Ion Chromatography-Tandem Mass Spectrometry (IC/MS/MS) with a reporting limit of 1 ug/L.

Ultra Low-Level Organophosphorus Pesticides by GCMS-SIM 

Weck Laboratories can analyze organophosphorus pesticides via Selected Ion Monitoring (SIM) mode Gas Chromatography/Mass Spectrometry (GCMS) at 25 times lower detection limits than EPA method 8141A.  This later method employs GC/NPD at detection limits of 250 nanograms per liter, whereas the GCMS-SIM method reaches down to 10 ng/L.  Target compounds and limits are listed here...