Filtered samples

Total airborne particulates are determined using a high-volume air sampler equipped with either cellulose fiber or glass fiber filters. Samples taken from urban environments require approximately 1 h of sampling time, but samples from rural environments require substantially longer times. 

Because a filter sample includes particles both larger and smaller than those retained in the human respiratory system (see Chapter 7, Section III), other types of samplers are used which allow measurement of the size ranges of particles retained in the respiratory system. Some of these are called dichotomous samplers because they allow separate measurement of the respirable and nonrespirable fractions of the total. Size-selective samplers rely on impactors, miniature cyclones, and other means. The United States has selected the size fraction below an aerodynamic diameter of 10 /xm (PMiq) for compliance with the air quality standard for airborne particulate matter. 

Figure 15-1 shows the Los Angeles, California, basin stationary air monitoring network, one of the most extensive in the United States (6). At most of these locations, automated instruments collect air quality data continuously. Five pollutant gases are monitored, and particulate matter filter samples are collected periodically. 

Filter samples can be prepared to airborne workplace concentrations by spiking each filter with aqueous solution containing elements with concentrations gravimetrically traceable to ultrapure metals or stoidiiometricaUy well defined oxides. The amormts correspond for some of the materials to current threshold limit values of contaminants in workroom atmospheres provided that the simulated filter has been exposed to one cubic meter of air. The certified values are based on a gravimetric procedure, i.e. weight per volume composition of the primary reference material dissolved in high purity sub-dis-tiUed acids. The National Institute of Occupational Health in Oslo, Norway, has produced several batches of such materials certified for 20 elements. Additionally, information values are reported for four other elements see Table 6.2. 

The NIST material SRM 1866a consists of a set of three common bulk mine-grade asbestos materials chrysotile, amosite and crocidolite, and one glass filter sample. SRM 1867 consists of a set of three imcommon mine-grade asbestos materials antophyllite, tremolite and actinohte. The optical properties of SRMs 1866a and 1867 have been characterized so that they may serve as primary calibration standards for the identification of asbestos types in building materials. 

Si(Li) spectroscopy, with the capability of simultaneous quantitative analysis of 72 elements ranging from sodium through to uranium in solid, liquid, thin film and aerosol filter samples. The penetrating power of protons allows sampling of depths of several tens of microns, and the beam itself may be focussed, rastered or varied in energy. The use of a proton beam as an excitation source offers several advantages over other X-ray techniques, for example there is a higher rate of data accumulation across the entire spectrum which allows for faster analysis. 

A known quantity of sample is added to a known volume of a universal buffer solution of sufficient capacity and of known pH. The amount of sample must be sufficient to cause precipitation to occur in the formed saturated solution. After waiting for a period of time to allow the saturated solution to reach the desired steady state, the solution is filtered to remove the solid and obtain a clear solution, whose spectrum is then taken by the UV spectrophotometer. Mathematical treatment of the spectral data yields the area-under-the-curve of the filtered sample solution, AUQ. 

In the solvent-refined coal pilot plant at Wilsonville, Alabama, the coal slurry is heated to reaction temperature in 3-4 minutes residence time in the preheater. The slurry is then held in the dissolver for an additional 40 minutes before it is filtered to obtain specification solvent-refined coal. By bypassing the dissolver and going directly to the filters, samples of short-contact time (SCT) SRC were produced from Illinois 6 (Monterey) and West Kentucky coals. 

Shimo, M., A Continuous Measuring Apparatus using Filter-Sampling Technique for Environmental Radon Daughters, Research Letters on Atmospheric Electricity, 4 63-70 (9184). 

Radon concentrations were measured by use of calibrated Lucas scintillation flasks, while radon and thoron daughters and the resulting potential alpha energy concentration (PAECj were determined using filter samples (Thomas, 1972) and a continuous electrostatic precipitator (Andrews et al., 1984). The radon daughter positive... 

Potentiometric stripping analysis has been applied by Sheffrin and Williams [320] to the measurement of copper in seawater at environmental pH. The advantage of this technique is that it can be used to specifically measure the biologically active labile copper species in seawater samples at desired pH values. The method was applied to seawater samples that had passed a 0.45 pm Millipore filter. Samples were studied both at high and at low pH values. 

The possibility of widely-varying radon levels from air filter samples can be a subtle trap. We were made aware of this when we were once under pressure to provide an immediate ("preliminary") result shortly after sample preparation. 

PCCD/PCDFs have been found to be present in Arctic air samples, e.g. during the winter of 2000/2001 in weekly filter samples (particulate phase) collected at Alert in Canada. PCDD/PCDFs have been monitored since 1969 in fish and fish-eating birds from the Baltic. The levels of PCDD/PCDFs in guillemot eggs, expressed as TEQ, decreased from 3.3 ng/g lipids to around 1 ng/g between 1969 and 1990. Since 1990, this reduction seems to have levelled off and today it is uncertain whether there is a decrease or not. Fish (herring) show a similar picture. 

Both GC and HPLC columns are expensive, so it is important not to clog them during analysis. GC columns will be clogged by nonvolatile compounds. For these materials, it is important to use HPLC. Samples must also be free of suspended particles that will clog the finely packed HPLC columns. Filtering samples, especially soil extracts, before injection is essential. 

It must also be emphasized that the major mass of a heterodispersed aerosol may be contained in a few relatively large particles, since the mass of a particle is proportional to the cube of its diameter. Therefore, the particle-size distribution and the concentration of the drug particles in the exposure atmosphere should be sampled using a cascade impactor or membrane filter sampling technique, monitored using an optical or laser particle-size analyzer, and analyzed using optical or electron microscopy techniques. 

Benzoylazide.3—14 g. (0-1 mole) of the dry hydrazide are made into a clear solution with 200 c.c. of approximately N-hydrochloric acid in a filter jar (capacity 0-5 1.). The solution is cooled in ice and stirred, while 8 g. of sodium nitrite in 50 c.c. of water are added. An immediate reaction takes place and the azide separates in crystalline form. When a filtered sample of the solution is no longer made turbid by the addition of a drop of nitrite solution, the precipitate is filtered dry at the pump, washed well with water, and dried, first on porous plate and then in a vacuum desiccator over concentrated sulphuric acid and potassium hydroxide. Yield 14 g. 

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