Improvements in and relating to the determination and control of compositions in chemical processes by titration

摘要

PICT:0855708/III/1 PICT:0855708/III/2 An automatic titration apparatus comprises (1) a vessel V (Fig. 1) with electrical level detector 8, electrical draining valve 2, stirrer (not shown) and end-point detector E1 E2; (2) at least one burette B with level detector 12 and filling and emptying valves 6, 7, also fitted with level-finder b; (3) one or more pipettes A, C, for reagents and diluents, these also having level detectors 9, 10, 11, filling valves 1, 3, and emptying valves 4, 5; (4) an electrical circuit associated with the end-point detector E1 E2 (Fig. 5) to give a signal which changes as the end-point is approached, this signal being passed through an anticipation circuit and a trigger circuit to control the outlet valve of the burette so that the reagent is added in discrete amounts with increasingly longer intervals; and (5) a sequencing switch (Fig. 6, not shown) controlled by the level detectors of the burette(s), pipette(s) and titration vessel and by the end-point detector, to control the various electromagnetic valves so that the operations of filling, titrating, measuring and emptying are performed in the correct order. The end-point detector is preferably a pH meter but may instead be based on change of colour, conductivity or redox potential. The pipettes A, C, are shown as one being of the overflow type and the other having an electrical level detector but these two types are interchangeable. The device b is preferably a photo-cell and lamp for detecting the liquid meniscus, but other kinds of electrical and mechanical level-gauges are mentioned as suitable. Stirring of the titration vessel may be effected by a mechanical stirrer or by blowing an inert gas through the liquid. The sample can be introduced manually or automatically and the apparatus can be arranged to cut off after the end-point is reached or to re-set itself to receive another sample. The sequence of operations is as follows (referring to Fig. 1):-(1) all valves are shut except 1, vessel V is full from the previous titration, and the sample is flowing through A; (2) valve 1 closes, b moves towards its rest position (continuing through subsequent operations (3) to (6) if necessary), valve 2 opens and vessel empties; (3) valve 2 shuts and 3 opens, filling C with diluent; (4) valve 3 shuts and 4 opens, passing diluent into V; (5) valve 4 shuts and 5 opens, delivering sample into V; (6) valve 5 shuts and 6 opens to fill burette; (7) valve 6 shuts and 7 opens, and titration commences; when about 90% of the correct amount has been delivered the circuit mentioned above comes into play and interrupts the flow from the burette for increasingly long intervals (up to 30 sec. in the end); (8) valve 7 has now closed and the device b records the level in the burette. The device b which detects the level of liquid in the burette is driven by a motor which also operates an indicator or recorder to show the amount of titrant added.