Carbon calibration

Reliable determinations of DOC concentrations need precise calibration. The software of the TOC 5000 instrument allows computation of a calibration curve through four data points. For seawater, standards generally range between 50 and 500 /tmol/L. There are many substances that may be used as reference material to prepare standards, but the selected material must exhibit the following characteristics  

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The furnace. For heating the tube packing, a small electric furnace E is used, similar to that described in the carbon and hydrogen determination. It is 22 cm. in length and 1 5 cm. in diameter. The furnace is maintained at 680 C., as before, by a calibrated Simmerstat and its temperature is checked from time to time with a bimetal pyrometer. 

Repeat the boiling point determination with the following pure liquids (a) carbon tetrachloride, A.R. (77°) (6) ethylene dibromide (132°) or chlorobenzene (132°) (c) aniline, A.R. (184-6°) and (d) nitrobenzene, A.R. (211°). An air condenser should be used for (c) and (d). Correct the observed boiling points for any appreciable deviation from the normal pressure of 760 mm. Compare the observed boiling points with the values given in parentheses and construct a calibration curve for the thermometer. Compare the latter with the curve obtained from melting point determinations (Section 111,1). 

Determination of boiling points. Distillation method (Fig. II, 12, 1) for carbon tetrachloride (25 nil. distillation flask and small water condenser), and SiwoloboflF s method (Fig. II, 12, 2) for carbon tetrachloride, aniline and nitrobenzene. Calibration curve for thermometer. Determination of b.p. of unknown liquid. 

Tetramethylsilane (TIMS) (Section 13 4) The molecule (CH3)4Si used as a standard to calibrate proton and carbon 13 NMR spectra... 

The purity of a sample of K3Fe(CN)6 was determined using linear-potential scan hydrodynamic voltammetry at a glassy carbon electrode using the method of external standards. The following data were obtained for a set of calibration standards. 

Susceptibility to radiation damage must be considered seriously if reference samples are to be calibrated for use in place of absolute systems. For the measurement of absolute C He, H) cross sections, films of polystyrene (CH) (which is relatively radiation hard) have been used successfiiUy, the RBS determination of carbon providing implied quantitation for the hydrogen present in the film. For a durable laboratory reference sample, however, there is much to recommend a known ion-implanted dose of H deep within Si or SiC, where the loss of hydrogen under room temperature irradiation will be neghgible. 

Similar to the pH meter, gas meters employ specific ion electrodes. The electrodes generate a potential proportional to the activity of a specific ion in solution. The calibration is achieved in standard solution and results read in mV or concentration in mg/L or ppm on the meter. The water can be adapted to monitor the concentration of carbon dioxide, hydrogen sulfide, ammonia, chloride, calcium, potassium and sodium to name a few. 

The above procedure may be adapted to the determination of molybdenum in steel. Dissolve a 1.00 g sample of the steel (accurately weighed) in 5 mL of 1 1 hydrochloric acid and 15 mL of 70 per cent perchloric acid. Heat the solution until dense fumes are evolved and then for 6-7 minutes longer. Cool, add 20 mL of water, and warm to dissolve all salts. Dilute the resulting cooled solution to volume in a 1 L flask. Pipette 10.0 mL of the diluted solution into a 50 mL separatory funnel, add 3 mL of the tin(II) chloride solution, and continue as detailed above. Measure the absorbance of the extract at 465 rnn with a spectrophotometer, and compare this value with that obtained with known amounts of molybdenum. Use the calibration curve prepared with equal amounts of iron and varying quantities of molybdenum. If preferred, a mixture of 3-methylbutanol and carbon tetrachloride, which is heavier than water, can be used as extractant. 

A clear solution can be obtained more quickly, and incidentally the transfer can be made more satisfactorily, by rapidly filtering the solution through a sintered glass funnel with exclusion of carbon dioxide with the aid of the apparatus shown in Fig. 10.9. It is advisable to calibrate the test-tube in approximately 5 mL intervals and to put the graduations on a thin slip of paper gummed to the outside of the tube. 

Take 10 mL of commercial propan-2-ol and dilute to 100 mL with carbon tetrachloride in a graduated flask. Record the infrared spectrum and calculate the absorbance for the peak at 1718 cm-1. Obtain a value for the acetone concentration from the calibration graph. The true value for the acetone in the propan-2-ol will be 10 times the figure obtained from the graph (this allows for the dilution) and the percentage v/v value can be converted to a molar concentration (mol L-1) by dividing the percentage v/v by 7.326 e.g. 1.25 per cent v/v = 1.25/7.326 = 0.171 molL-1. 

Last but not least, one should check the inertness of the auxiliary electrodes in single-pellet arrangements, both under open and closed circuit conditions and, also, via the closure of the carbon balance, the appearance of coke deposition. This is especially important in systems with a variety of products (e.g. selective oxidations), where the exact value of selectivity towards specific products is of key interest. This in turn points out the importance of the use of a good analytical system and of its careful calibration. 

The most important type of mixed solution is a buffer, a solution in which the pH resists change when small amounts of strong acids or bases are added. Buffers are used to calibrate pH meters, to culture bacteria, and to control the pH of solutions in which chemical reactions are taking place. They are also administered intravenously to hospital patients. Human blood plasma is buffered to pH = 7.4 the ocean is buffered to about pH = 8.4 by a complex buffering process that depends on the presence of hydrogen carbonates and silicates. A buffer consists of an aqueous solution of a weak acid and its conjugate base supplied as a salt, or a weak base and its conjugate acid supplied as a salt. Examples are a solution of acetic acid and sodium acetate and a solution of ammonia and ammonium chloride. 

A cylinder of carbon monoxide equipped with a suitable regulator calibrated in pounds per square inch (p.s.i.g.) is connected to the three-way stopcock. All joints and the septum must be secured with clamps or wire. A vertical tube containing mercury was connected to an exit tube from the reaction flask by the checkers. A pressure of carbon monoxide was maintained against a 500-mm. column of mercury. 

The state of research on the two classes of acetylenic compounds described in this article, the cyclo[ ]carbons and tetraethynylethene derivatives, differs drastically. The synthesis of bulk quantities of a cyclocarbon remains a fascinating challenge in view of the expected instability of these compounds. These compounds would represent a fourth allotropic form of carbon, in addition to diamond, graphite, and the fullerenes. The full spectral characterization of macroscopic quantities of cyclo-C should provide a unique experimental calibration for the power of theoretical predictions dealing with the electronic and structural properties of conjugated n-chromophores of substantial size and number of heavy atoms. We believe that access to bulk cyclocarbon quantities will eventually be accomplished by controlled thermal or photochemical cycloreversion reactions of structurally defined, stable precursor molecules similar to those described in this review. 

Gel Filtration. The lyophilized protein was redissolved in 50 mM phosphate buffer, pH 7.4 0.15 m NaCl 0.013 % sodium azide and loaded on a Superdex 75HR1030 column equilibrated with the same buffer. Elution was downward flow (0.15 ml/min) and 0.25 ml fi actions were collected. Fractions with pectin lyase activity were combined, dialyzed against distilled water and used in the next step. To estimate the molecular mass of PNL, the column was calibrated with standard proteins (Sigma MW-GF-70 Albumin, 66,000 Da Carbonic Anhidrase, 29,00 Cytochrome, 12,400 and Aprotinin, 6,500). The proteins were eluted in the conditions described above and their volumes (F ) were calculated fi om the peak maximum of the absorbance at 280 nm. The partition coefficient was obtained fi om the relationship where F, represents the bed volmne of column and F the void volume (which was calculated using blue dextran. Sigma). The molecular mass was determined using a standard curve of vs the logarithm of the molecular masses of the standards [28, 29]... 

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