A completely a utomatic apparatus h as been develop ed for t he prepa rative-scale p urification of compo unds by gas-liquid chromatograph y. A clock timer periodically activates a pump t hat injects a sample into the column . The recording potentiometer o n which t he chromatogra m is t raced has a swit ch m oun ted at t he upper margin. Collection of t he p urified main component occurs when t he recorder p en goes to t he end of the scale and t rips t he swi tch . The sensitivity of the detector bridge circuit is adj usted so that only t he t race caused by t he major component will activate the collection process.T oluene, ethylbenzene, and mesitylene were purified wit h the apparatus. Best results were obtained with tolucne. In one pass t hrough t he apparatus, 92 percen t of the impurities were removed fro m the toluene and t he p urified product was collected at a rate of 25 ml of liquid per day.
High pressure liquid chromatography (HPLC) was used to resolve FD&C Blue No. 1 (Brilliant Blue), FD&C Blue No. 2 (Indigotine), Amaranth (formerly certified as FD&C Red No. 2 ) , FD&C Red No. 3 (Erythrosine), FD&C Red No. 4, FD&C Red No. 40, FD&C Yellow No. 5 (Tartrazine), FD&C Yellow No. 6 (Sunset Yellow FCF), and FD&C Green No. 3 (Fast Green FCF). These synthetic acid fast dyes as found in wine and flavor samples were extracted with wool yarn and analyzed by HPLC and thin layer chromatography. The 2 methods are compared for sensitivity and resolution. The HPLC procedure is a quicker way to screen a larger number of samples for artificial colors with better resolution than that obtained by thin layer chromatography. HPLC can separate FD&C Red No. 40 from FD&C Red No. 4 and this could not be achieved by using the described TLC solvent system. The FD&C dyes most commonly found in flavors and distilled spirits were FD&C Red No. 40, FD&C Yellow No. 5, and FD&C Yellow No. 6.
M eas ur em ents of t h e heat capac it y of mC't h y lph osp ho ny l di flu o ri de (CH , P OF2) , methylphospho nyl di chl o rid e (CI-I 3PO Cl,), and m ethylphospho ny l chlo ro flu o ri de (CH aPOC lF) " 'ere m a de fro m a bo ut 15 to 335 oK by m eans of an adi abat ic calorim C'ter. These hi g hl y react ive and toxic su bstances were pu rifi ed in a com pletely closed glass appa rat us b.v co mbini ng s low crysta ll izat ion a nd fractional m eltin g proced lll·C'S. TI1l' puri t ies dC't('l" min ed b~' t hr fr eezin g-e ur vc mf't hod a re s hown to be generall y in agrC'emc nt with t hosE' valu es ohtain C' c\ h. v t he calo r.imetri c m et hod. From t he r('s ults of t he Iwat, m eaSll re m (' nt~, t he t ri p le-point k mperatu rc, heat o f fu sio n, and t heir co rrespo nclin g est im ated un certai nties \\"('I'e foun d to bp, res pectively, 236.34 ± 0.05 oJ\: and 1I ,878 ± 12 J / mo le fo r CH 3POF 2, 306. Triple-point tC'mpe rat ures obtain ed b.v thp fr cez ing-cu rve me t hod a rc in ag rec m ent \\" ith t he above val lies. A tab le of smoothed values of heat capac ity, enthalpy, entha lp y fun ct io n, ent ropy, G ib bs fr ee ene rgy, and G ibbs frp e e nergy fun ct ion fl'om 0 to 335 OK was obtained from t he d ata. T he ent ropy a nd its co rrespondin g pst im ated unce rt.ainty fo r C H3P OF2, CH 3POC I2, and CH3P OC IF in t heir respcc tive condenspd phase at 298. 1.5 o J( a nd sat urat ion press ure \Vas fo und to be 208.3 ± 0.3, 164.8 ± 0.3 , a nd 216.4 ± 0.4 J /d pg mole, rcs pecti ve ly. The entropies in the gaseo us state fLt 298. 15 OK a nd 1 atm press ure "-ere found to be 312.7 ± 3, 339.7 ± 3, a nd 335.0 ± 3 J /deg mol e, respecti ve ly.
After preliminary cleanup, sodium saccharin can be quantitatively determined in wines and proprietary drugs by using high pressure liquid chromatography. The preliminary cleanup removes materials that cause column deterioration, loss of baseline stability, and interfering peaks. The average experimental error found in analyses of 6 wines for sodium saccharin content was 2.3% and the standard deviation was 0.01. In the analysis of 10 cough medicines and vitamin preparations, the difference between declared and experimental values for sodium saccharin averaged 5.7%. The recovery for the extraction process ranged from 97.8 to 101.6%.
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