Desorption from activated charcoal

Filippone GA, Fish SS, Lacouture PG, Scavone JM, Lovejoy FH. Reversible adsorption (desorption) of aspirin from activated charcoal. Arch Intern Med 1987 147 1390-2. 

The ROPs include sampling, sample preparation, and analysis instructions for low-volume Tenax and XAD-2 air samples. Only the preparation of an XAD-2 low-volume air sample is presented in this article, while the thermal desorption of a Tenax tube is described in the context of gas chromatographic analysis see Chapter 10). Active charcoal is such a strong adsorbent that it requires more effective extraction methods than XAD-2 resin or Tenax tubes. Thus, the recoveries of CWC-related chemicals tend to be lower from active charcoal than from other air sampling materials. Furthermore, active charcoal is not usually used for the collection of organophosphorus chemicals. The sample preparation methods for active charcoal samples have not been validated in international round-robin or proficiency tests. 

Posner, J. C. Desorption of Organic Analytes from Activated Charcoal II Dealing with the Problems, Am. Ind. Hyg. Assoc. J. 42, 647 (1981)... 

Various sample enrichment techniques are used to isolate volatile organic compounds from mammalian secretions and excretions. The dynamic headspace stripping of volatiles from collected material with purified inert gas and trapping of the volatile compounds on a porous polymer as described by Novotny [3], have been adapted by other workers to concentrate volatiles from various mammalian secretions [4-6]. It is risky to use activated charcoal as an adsorbent in the traps that are used in these methods because of the selective adsorption of compounds with different polarities and molecular sizes on different types of activated charcoal. Due to the high catalytic activity of activated charcoal, thermal conversion can occur if thermal desorption is used to recover the trapped material from such a trap. 

Air samples are usually collected to solid adsorbents such as Tenax, XAD resins, graphitized carbons (e.g. Carbopak), active charcoal, or porous polymers (e.g. Chromosorb). The chemicals are eluted from the adsorbent to a liquid or gas phase by liquid-solid elution or extraction or by thermal desorption. Extraction is the most common method. Thermal desorption can be applied when analysis is by GC (gas chromatography) method, and, recently, the use of automated thermal desorption has been proposed to provide increased sensitivity in GC/MS analysis of a wide range of CWC-related chemicals 8. ... 

Activated Charcoal. The original intent of the research was to develop a sampling technique that used coconut-shell charcoal to collect vinyl acetate vapors from air samples. Therefore, the breakthrough volume and desorption efficiency of vinyl acetate on coconut-shell charcoal were studied. 

Thermal Desorption Thermal desorption is an alternative GC inlet system particularly used for VOC analysis. However, the analytes subjected to thermal desorption must be thermally stable to achieve successful analysis. Otherwise, decomposition occurs. This technique is mainly used for determination of volatiles in the air. Such a methodology requires sample collection onto sohd sorbents, then desorption of analytes and GC analysis. Traditionally, activated charcoal was used as a sorbent followed by extraction with carbon disulfide. However, solvent desorption involves re-dilution of the VOCs, thus partially negating the enrichment effect. Therefore, the sampling method is to pump a sample of gas (air) through the sorbent tube containing certain sorbents in order to concentrate the VOC. Afterwards, the sample tube is placed in thermal desorber oven and the analytes are released from the sorbent by application of high temperature and a flow of carrier gas. Additionally, desorbed compounds are refocused in a cold trap and then released into the GC column. Such a two-step thermal desorption process provides a narrow chromatographic band at the head of the column. 

Samples collected on adsorbents can be desorbed by heat (thermal desorption) or by solvent extraction. Thermal desorption of samples from charcoal is not efficient however, because of the high temperature needed (950°C) to remove hydrocarbons from the charcoal (192). For this reason, most ACS passive headspace procedures use carbon disulfide to extract the adsorbed liquid residues. In 1967 Jennings and Nursten (193) reported concentrating analytes from a large volume of aqueous solution using activated charcoal as the adsorbent and extracting with carbon disulfide. Since then many adaptations of this method have been used to detect accelerants in fire debris, but currently dynamic headspace methods are seldom used because of the inconvenience of sampling and possible contamination issues with equipment. 

From 4.5 mJ/pulse, the PAH signal increases again and does not disappear after thousand shots the destruction of the carbon matrix releases PAHs present in the deeper graphene layers. Moreover, the desorption of fluoranthene is achieved in the same Ed interval as pure fluoranthene sample (see Fig.l-f and Fig.5). The origin of this common behaviour will be discussed in the next chapter, in the light of the results of a similar study realised on two other matrices activated charcoal and black carbon. 

Because amorphous carbon as graphite heats up strongly under MW irradiation [4], its use as a sensitizer has been widely reported [5-10] (Sect. 7.1). Recently, MW-as-sisted esterification of carboxylic acids with alcohols was performed on activated carbon in good yields (71-96%) [98]. For our part, when charcoal powder was used as a support, we had difficulty in desorbing the reaction products [15]. Even with a continuous extractor, the desorption was never quantitative. The desorption of reaction products from graphite powder is much easier than from amorphous carbon powder. 

The analyte must be efficiently recovered. The usual mechanism for solvent desorption is selective displacement of the analyte. Selective displacement occurs as a more polar solvent displaces a less polar one on charcoal, just as a more active ion displaces a less active one on ion exchange resins. CS2 is frequently used to recover substances from charcoal, but simple alcohols cannot be displaced from charcoal by CS2, and it is necessary to add l%-5% of another alcohol to the CS2 to facilitate desorption. Frequently, low recoveries can be increased by increasing the quantity of solvent, if analytical sensitivity permits. Prospective solvents may be chosen based on polarity or solubility of the analyte. 

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