Four new Standard Reference Materials (SRMs) have been developed to assist in the quality assurance of chemical contaminant measurements required for human biomonitoring studies, SRM 1953 Organic Contaminants in Non-Fortified Human Milk, SRM 1954 Organic Contaminants in Fortified Human Milk, SRM 1957 Organic Contaminants in Non-Fortified Human Serum, and SRM 1958 Organic Contaminants in Fortified Human Serum. These materials were developed as part of a collaboration between the National Institute of Standards and Technology (NIST) and the Centers for Disease Control and Prevention (CDC) with both agencies contributing data used in the certification of mass fraction values for a wide range of organic contaminants including polychlorinated biphenyl (PCB) congeners, chlorinated pesticides, polybrominated diphenyl ether (PBDE) congeners, and polychlorinated dibenzo-p-dioxin (PCDD) and dibenzofuran (PCDF) congeners. The certified mass fractions of the organic contaminants in unfortified samples, SRM 1953 and SRM 1957, ranged from 12 ng/kg to 2200 ng/kg with the exception of 4,4'-DDE in SRM 1953 at 7400 ng/kg with expanded uncertainties generally <14 %. This agreement suggests that there were no significant biases existing among the multiple methods used for analysis.
We have determined the congener compositions of nine commercial Aroclor products of polychlorinated biphenyls (PCBs) to the sub-part-per-million level using high-resolution gas chromatography combined with high-resolution mass spectrometry according to US Environmental Protection Agency (EPA) Method 1668A. These Aroclor composition data should allow improved characterization and risk assessment of PCB contamination at hazardous waste sites, particularly for dioxin-like PCB congeners. By combining the data on the concentrations of each dioxin-like congener with its World Health Organization toxicity equivalency factor, we have established dioxin toxic equivalent concentrations for each pure Aroclor product.
We present an analysis of time-series measurements from a prototype fluorescence-quenching dissolved oxygen sensor moored for a six-day period in late March 1987 at 100 m depth in Saanich Inlet, British Columbia. Temporal variations in dissolved oxygen are shown to be consistent with concomitant variations in water properties obtained from a moored Aanderra RCM4 current meter and daily vertical profiles. Results suggest that fluorescence-based instrumentation have sufficient resolution and stability for a variety of mooring and profiling applications involving the measurement of dissolved oxygen concentration.
A sensor based on fluorescence quenching has been built to detect oxygen activity in gas and water. The sensor consists of a xenon flash bulb as a light source; an excitation wavelength band pass filter; a dichroic beam splitter; collimating and focussing lenses; a plastic clad silica (PCS) rod with the fluorophore immobilized at the tip of it; an emission wavelength band pass filter; a photomultiplier tube (PMT); a monitor PIN photodiode detector; and interface electronics to couple a computer to the rest of the sensor. The device demonstrates a reversible change in fluorescence quenching for changes in oxygen activity. The fluorescence signal seen by the PMT varies over a factor of 3, being highest at 0 oxygen activity and lowest at atmospheric oxygen activity. The device exhibits a 63 % response time of less than 1 second for gases and less than 10 seconds for oxygen dissolved in water. The noise floor of the sensor is approximately 1%. The present embodiment of the device was designed to allow the sensor to operate in the marine environment. The optical components, computer, batteries, and power supply circuitry are mounted on a rack that is enclosed in a pressure housing. The immobilized fluorophore is exposed to sea water. The light travels along the PCS rod, through a pressure seal, to the rest of the system. Present investigations are centered around long term stability of the fluorophore and constituents of the real ocean that will interfere with the quenching mechanism.
A simple and rapid method has been developed to measure the bitumen, water, and solids content of Athabasca oil sand samples in order to efficiently serve both plant operations and research needs. A solvent blend of 74% toluene and 26% isopropyl alcohol extracts both the bitumen and the water from the solids producing a homogeneous liquid phase. The bitumen is determined gravimetrically on an aliquot of this solution. A Karl Fischer titration is used to measure the water concentration. Solids are measured gravimetrically or can be reported by difference. Mass balances between 99.05 and 100.25% are achieved routinely.