摘要 |
PURPOSE:To analyze trace S with a small amt. of a sample and with good accuracy by burning the sample in gaseous oxygen flow, passing the combustion gas through an absorption part contg. a small amt. of absorbent liquid to have gaseous SO2 absorbed and adding a decolored Para Rosaniline soln. and H2CO soln. to the absorbent liquid so that said liquid forms a color. CONSTITUTION:The gaseous oxygen flow formed by passing oxygen of the first class level through a chromium-satd. sulfuric acid 7 and a silica gel column 8 to clean up said oxygen is fed to a quartz tube 6 heated by a combustion furnace 3 to burn S in the sample weighed in the boat 2 in the tube 6. An absorption part 4 contg. potash bulbs 4-1 in a support table 4-2 formed by opening a hole to foamed polystyrene is connected by a silicone tube, etc. to the tube 6 so that the generated SO2 is absorbed therein. The absorbent liquid is then delivered by gaseous O2, etc. to a beaker, etc. and a specified amt. thereof is exactly separated and respectively a specified volume of a soln. decolored by adding HCl to 0.2V/V% soln. of Para Rosaniline and 0.5%V/V soln. of H2CO are added to the separated liquid. Part of the liquid is taken after resting for about 20min and the absorbancy at 550nm wavelength is measured. The measured absorbancy is compared with a preliminarily obtd. calibration curve and the S in the sample is quantitatively determined with high accuracy. |