Adsorbed weight, determination

In support of the association theory, colloid chemists cited non-reproduceable cryoscopic molecular weight determinations (which were eventually shown to be caused by errors in technique) and claimed that the ordinary laws of chemistry were not applicable to matter in the colloid state. The latter claim was based, not completely without merit, on the ascerta-tion that the colloid particles are large aggregates of molecules, and thus not accessible to chemical reactants. After all many natural colloids were shown to form double electrical layers and adsorb ions, thus they were "autoregulative" by action of their "surface field" (29). Furthermore, colloidal solutions were known to have abnormally high solution viscosities and abnormally low osmotic pressures. 

The amount of water adsorbed after the samples were outgassed was controlled by adjustment of the pressure in one of three ways use of a sensitive Cartesian diver manostat, use of a water source at a controlled temperature, or use of the mixed magnesium perchlorate hydrates mentioned above. The amount of water adsorbed by the sample was measured either by the gain in weight of a companion sample or by interpolation from the isotherm at 23.5° C. The heat of immersion of samples with no water adsorbed was determined with samples sealed off from the vacuum line while they were still in the furnace at 500° C. 

Interparticle volume could be measured using GPC as the total exclusion volume of high-molecular-weight polymers, and the void volume could be accurately measured as the elution volume of deuterated acetonitrile eluted with neat acetonitrile. The example of these measurements and comparison with the adsorbent mass determined by unpacking the column and weighing the dried adsorbent are shown in Table 3-5. 

Determining the molecular weights of asphaltenes is a problem because they have a low solubility in the liquids often used for determination. Also, adsorbed resins lead to discrepancies in molecular-weight determination, and precipitated asphaltenes should be reprecipitated several times prior to the determination (12). Thus, careful precipitation and careful choice of the determination method are both very important for obtaining meaningful results. 

By comparing the weight of the aerogel at 0 and 30 % relative humidity the amount of water that each RF aerogel adsorbs is determined. After storing the samples at 90 °C for 48 h and cooling down to room temperature in dry N2-atmosphere the weight at 0 % relative humidity is measured. To obtain the values at 30 % relative humidity the samples are placed in a closed cell with a specific salt-water solution. By vapor pressure depression above saturated solutions this specific solution keeps the atmosphere constant at 30 % relative humidity. 

The electric conductivity of the insoluble black polymer is 5.3 X 10 S cm. When the polymer is exposed to an iodine vapor, 0.32 atom of iodine per thiophene unit is adsorbed, as determined from the increase in weight of the polymer, and the electrical conductivity increases to 3.4 X 10 S cm at 291 K. 

The monolayer amount adsorbed on an aluminum oxide sample was determined using a small molecule adsorbate and then molecular-weight polystyrenes (much as shown in Ref. 169). The results are shown in the table. Calculate the fractal dimension of the oxide. 

When a solid such as charcoal is exposed in a closed space to a gas or vapour at some definite pressure, the solid begins to adsorb the gas and (if the solid is suspended, for example, on a spring balance) by an increase in the weight of the solid and a decrease in the pressure of the gas. After a time the pressure becomes constant at the value p, say, and correspondingly the weight ceases to increase any further. The amount of gas thus adsorbed can be calculated from the fall in pressure by application of the gas laws if the volumes of the vessel and of the solid are known or it can be determined directly as the increase in weight of the solid in the case where the spring balance is used. 

Polyacrylamide, whether charged or not, can be detected by reactions of the amide group (67,68) however, a number of substances can interfere with the determination. If the molecular weight is high enough, flocculation of a standard slurry of clay or other substrate is a sensitive method for detecting low levels of polyacrylamide (69). Once polymers are adsorbed on a surface, many of these methods caimot be used. One exception is the use of a labeled polymer. 

Various types of detector tubes have been devised. The NIOSH standard number S-311 employs a tube filled with 420—840 p.m (20/40 mesh) activated charcoal. A known volume of air is passed through the tube by either a handheld or vacuum pump. Carbon disulfide is used as the desorbing solvent and the solution is then analyzed by gc using a flame-ionization detector (88). Other adsorbents such as siUca gel and desorbents such as acetone have been employed. Passive (diffuse samplers) have also been developed. Passive samplers are useful for determining the time-weighted average (TWA) concentration of benzene vapor (89). Passive dosimeters allow permeation or diffusion-controlled mass transport across a membrane or adsorbent bed, ie, activated charcoal. The activated charcoal is removed, extracted with solvent, and analyzed by gc. Passive dosimeters with instant readout capabiUty have also been devised (85). 

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