Buoyancy corrections

The buoyancy correction needed in adsorption gravimetry has the same origin as the dead space correction in adsorption manometry it is due to the volume of the sample 

The direct determination of the buoyancy is carried out with a gas which does not adsorb at the temperature of the determination it must be chosen in the same way as the gas for Step 3 in the previous section. Helium should be avoided - this light gas does not lend itself to the precise determination required since the buoyancy correction is directly proportional to the molar mass of the gas used. 

The indirect determination of the buoyancy is obtained by the assessment of the sample volume from its density or by pycnometry - as in the previous section and with the same implications for the location of the Gibbs dividing surface. 

Due to the change in density of a gas as the temperature changes, buoyancy corrections must be made in TGA measurements. Without corrections every sample will appear to show a mass increase during a heating experiment. TGA measurements are usually corrected for the effect of buoyancy by performing a blank measurement. A blank experiment uses the same temperature program and crucible as the experiment but without a sample. The resulting blank curve (also called a b aseline) is then subtracted from the sample measurement curve. In some instruments, a standard baseline is automatically subtracted from aU measurements. 

Buoyancy correction is essential for tests such as ash content where the residue at the end of the test needs to be determined accurately, and where very small weight losses are expected. 

The temperature dependence of density at constant pressure is given by the equation 

From Table 3.1 it follows that a body with a volume of 1 mL experiences a buoyancy force in dry air of 1.184 mg at 25°C or 0.269 mg at 1000°C. This means that the body appears to become 0.915 mg heavier, i.e. to weigh more, when it is heated from 25 to 1000°C. 

Modern thermobalances are often equipped so that they can record the DTA (differential thermal analysis see Section 1.3) signal at the same time as the actual thermogravimetric measurement. 

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This method is smiple but experimentally more cumbersome than the volumetric method and involves the use of a vacuum microbalance or beam balance [22], The solid is suspended from one ann of a balance and its increase in weight when adsorption occurs is measured directly. The dead space calculation is thereby avoided entirely but a buoyancy correction is required to obtain accurate data. Nowadays this method is rarely used. 

With gravimetric methods, the magnitude of the buoyancy correction should be assessed. Particular attention must be paid to the adsorbent temperature because of the unavoidable gap between the sample and the balance case (cf. Section 6.2). 

If the buoyancy correction is ignored, the pipet s volume is reported as... 

What is the minimum density of a substance necessary to keep the buoyancy correction to less than 0.01% when using brass calibration weights with a density of 8.40 g/cm ... 

Schoonover, R. M., and Jones, F. E., Air Buoyancy Correction in High-Accuracy Weighing on Analytical Balances, Anal. Chem. 53, 1981, 900-902. 

Thus, by using very thin plates with thickness 0.1 to 0.002 mm, one can measure surface tension with very high sensitivity. In practice, by using very thin platinum plates of well-known dimension (length = 1.00 or 2.00 cm), one can calibrate the apparatus with pure liquids, such as water and ethanol. The buoyancy correction is made very small (and negligible) by using a very thin plate and dipping the plate as little as possible. 

Allowing and to be the volume and absolute temperature of the counterweight, and to be the same for the sample and its container, the buoyancy correction becomes... 

When using microbalances for adsorption measurements, those adsorbates which do not require thermal transpiration corrections are the most susceptible to buoyancy errors while those adsorbates not requiring buoyancy corrections, such as krypton, because of its low vapor pressure, are most susceptible to thermal transpiration errors. 

Buoyancy corrections are only required by the gravimetric method. 

Buoyancy correction Conventional masses are based on weighing at sea level with air density 1.2 kg m 3 and sample density 8000 kg m 3 Rarely needed. Usually ignore with error in true mass of less than 0.01 %... 

Figure 2-5 shows buoyancy corrections for several substances. When you weigh water with a density of 1.00 g/mL, the true mass is 1.001 I g when the balance reads 1.000 0 g. The... 

Safety requires you to think in advance about what you will do never do anything that seems dangerous. Know how to use safety equipment such as goggles, fume hood, lab coat, gloves, emergency shower, eyewash, and fire extinguisher. Chemicals should be stored and used in a manner that minimizes contact of solids, liquids, and vapors with people. Environmentally acceptable disposal procedures should be established in advance for every chemical that you use. Your lab notebook tells what you did and what you observed it should be understandable to other people. It also should allow you to repeat an experiment in the same manner in the future. You should understand the principles of operation of electronic and mechanical balances and treat them as delicate equipment. Buoyancy corrections are required in accurate work. Burets should be read in a reproducible manner and drained slowly for best results. Always interpolate between markings to obtain accuracy one deci-... 

Why is the buoyancy correction equal to 1 in Figure 2-5 when the density of the object being weighed is 8.0 g/mL ... 

The densities (g/mL) of several substances are acetic acid, 1.05 CC14, 1.59 sulfur, 2.07 lithium, 0.53 mercury, 13.5 Pb02, 9.4 lead, 11.4 iridium, 22.5. From Figure 2-5, predict which substance will have the smallest percentage of buoyancy correction and which will have the greatest. 

The balance says that you have weighed out 1.023 g of tris to standardize a solution of HCI. Use the buoyancy correction in Section 2-3 and the density in Table 11-5 to determine how many grams you have really weighed out. The volume of HCI required to react with the tris was 28.37 mL. Does the buoyancy correction introduce a random or a systematic error into the calculated molarity of HCI What is the magnitude of the error expressed as a percentage Is the calculated molarity of HCI higher or lower than the true molarity ... 

The buoyancy correction is 1 when the substance being weighed has the same density as the weight used to calibrate the balance. 

Finally, if the object has a greater density than the weights (d0 > c/w), buoyancy correction factor will be less than 1.000000, because the smaller volume of the object displaces a smaller mass of air than the weights. Platinum, gold, and lead are metals with appreciably greater density than brass. 

If we had not made a buoyancy correction, we would have thought the volume... 

Thermogravimetric analyses were carried out in 10°-30° temperature increments with 200-mg samples using a conventional (Mauer) TGA system. Automatic recording of weight change was used to follow reaction to equilibrium, but actual weighings were recorded only by manual operation. The sample was bathed continuously in air of controlled humidity (Pmo = 7.9 torr) flowing at 180 cc/min. Precautions were taken to minimize drafts and convective currents, and buoyancy correction curve was made to 950°C. Further details on experimental methods are available (12). 

V = apparent vol in ml corresponding to sum of scale on the two arms C = air buoyance correction, obtd from a table... 

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