ORP FOR CHEMICAL DOSAGE CONTROL IN METAL PRECIPITATION Kristine S. Siefert and Kerstin E. Lampert Nalco Chemical Company Naperville, Illinois
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1 ORP FOR CHEMICAL DOSAGE CONTROL IN METAL PRECIPITATION Kristine S. Siefert and Kerstin E. Lampert Nalco Chemical Company Naperville, Illinois Oxidation Reduction Potential (ORP) probes are commonly used in the plating industry to automate control of cyanide destruction and chromium (VI) reduction processes.1 Response of ORP probes in these oxidation-reduction processes might be expected, but ORP response in metal ion precipitation processes is not obvious. Thus, the applicability of ORP probes for chemical dosage control was unknown for processes utilizing organic precipitant products for metal removal. The following describes a research study that was done to evaluate ORP probes as process sensors in Nalco Chemical Company's NalmetTM program. Backmound Oxidation-reduction reactions involve the transfer of electrons, since oxidation (the loss of electrons) and reduction (the gain of electrons) occur simultaneously. ORP probes measure the flow of electrons by providing an active electrode for electron exchange. The active electrode is typically platinum or gold, and a voltage difference or "potential" between it and a reference electrode is measured. ORP probes for industrial use are available from a number of suppliers, including Leeds and Northrup (North Wales, PA) and Great Lakes Instruments (Milwaukee, WI). Numerous components in metal-bearing wastewaters may be "active at the electrode", meaning that the ORP probe will measure a potential when one of these components is present. Among the active components are hydrated metal ions, chelated metal ions, organics (such as formaldehyde), strong oxidants (such as hypochlorite), and strong reducing agents (such as bisulfite). When several active components are present simultaneously, ORP measures a "mixed" potential, a composite of the potentials, though one particular component may dominate the measured potential. ORP probes cannot be construed as specific sensors for any single component when multiple active components are present. In general, ORP measurements are sensitive to fluctuations in process ph due to the involvement of hydrogen ions (H+) in either the reduction or oxidation reaction. An example of such a reduction reaction is shown below in Equation (1). The corresponding Nemst equation expressing the effect of concentration of reactants and products on the reduction potential (E) is shown in Equation (2)
2 0.5 Cr2m2 + 7H+ + 3 e- = Cr H20 (1) E= log[[cr+31/[cr~~210.5[h+17] (volts) (2) 3 Thus, a 1 unit fluctuation in ph would result in a change in potential of (2.33 x 59 mv) or 138 mv. The effect of ph on ORP measurements in other processes will depend on the involvement of hydrogen ion in the reaction and the number of electrons transferred. The lack of knowledge of the reactions occurring at the electrode during metal ion precipitation makes it impossible to predict ph effects on measured potentials. When contemplating product feed control strategies for metal precipitation, several key issues were considered. First, a sensor monitoring the process must respond to either the disappearance of metal ions or the appearance of excess precipitant. Second, the sensor has to be relatively insensitive to other components in the wastewater, such as chelants, surfactants, and solids, as these components may be present in metal-bearing wastewaters. The best control, i.e., minimal underfeed or overfeed, will be achieved if the sensor shows a marked response at the reaction equivalence point, the dosage where free metal ions are absent. Finally, process control will necessarily be different for batch and continuous processes. These issues were examined in the laboratory studies. Experimental Laboratory studies were conducted with industrial equipment: Great Lakes Instruments 5-wire ORP probe with a gold process electrode and Model 672R Analyzer. The analyzer unit has an LCD display and several outputs, including 4-20 ma and 0-5 V. The 0-5 V output was connected to a strip chart recorder, and the 4-20 ma output was available for proportional control of a feed pump. One-liter grab samples of wastewater were obtained and tested in a large crystallization dish in which the ORP probe was suspended. A large magnetic stir bar in the bottom of the dish provided mixing. A Horizon ph controller with a glass ph electrode and peristaltic pumps for both acid and base were used to control process ph, typically to 0.1 units. The precipitant product was delivered to the wastewater by a syringe pump calibrated for flow rate. The tests were batch treatments in which precipitant was gradually added over time, usually 30 to 45 minutes. ORP potential and ph were recorded by a strip chart recorder. Periodically, a small aliquot (-5 ml) of wastewater was withdrawn by syringe for subsequent metalsanakysis. The aliquots were filtered through 0.45 micron membrane filters, appropriately diluted, acidified, and analyzed for metals content. A Perkin-Elmer Model 306 Atomic Absorption Spectrophotometer was utilized for all metals analyses
3 Results and Discussion Printed Circuit Board: Plant #1 A wastewater sample from a printed circuit board plant with a continuous treatment process was tested. The wastewater initially contained 83 ppm of copper and had a ph of 1.4. Adjustment of sample ph to 8.0 with caustic resulted in soluble copper of 21 ppm, so the balance of copper in the untreated waste was non-chelated. The ORP study was conducted at ph 10, and approximately onehalf of the stoichiometric dosage of precipiant was-quickly added during ph adjustment to reduce hydroxide precipitation. The remaining preapitant was gradually pumped into the wastewater during the test. The test results with ORP potential in millivolts (mv) and soluble copper concentration in parts-permillion (ppm) plotted against precipitant dosage are shown in Figure 1. ORP potential decreased gradually with increasing precipitant dosage until a sharp drop of about 30 mv occurred, Seen as an inflection in the curve. Soluble copper decreased almost linearly with dosage, dropping to less than 0.1 ppm at a dosage corresponding to the bottom of the potential curve inflection. This marked response at the equivalence point suggests that good control is possible. In choosing possible setpoints for proportional control, -80 and -100 mv might be selected, since good removal of copper (4 ppm) and minimal product overfeed (<2%) were observed in the batch treatment. In a continuous treatment process, however, the presence of large amounts of precipitated metal might influence the ORP response, compared to batch treatment. Thus, control parameters should be verified on-site. Printed Circuit Board: Plant #2 A sample of wastewater was tested from a second printed circuit board plant that also has a continuous treatment process. The untreated sample contained 17 ppm of copper at ph 2.5. The results of the ORP test at ph 8.8 are shown in Figure 2. The ORP potential curve shows an inflection which is at much higher dosage than is appropriate for good copper removal. The use of the ORP potentials at the inflection for controller setpoints could result in about 40% overfeed of product. It is likely that this wastewater sample contains an interfering component that is also active at the electrode, such as an oxidant. Equalization of wastewater streams or removal of suspect streams from the continuous system might eliminate this interference. Zinc Plating: Plant #3 A sample of wastewater was obtained from zinc plating operations. Initial zinc concentration was 12.5 ppm at ph 2.6. Adjustment of sample ph to 10 caused all of the Zn to precipitate, i.e., the Zn was not chelated. To allow testing of a wastewater having chelated zinc, sodium citrate was added. Citrate ion is a relatively strong chelant that can be displaced from Zn by the precipitant product
4 Twelve ppm of Zn was ultimately chelated. An ORP test at ph 8 was conducted, and the results are shown in Figure 3. Zinc concentration with precipitant dosage eventually decreased to about 0.3 ppm, though three times the stoichiometric dosage was required. This precipitant usage reflects the relative strength of the Zn-citrate complex. While the ORP potential also declined with dosage, no particular response was observed at the equivalence point, i.e., the ORP was insensitive to the disappearance of Zn. Selection of another chelant for this wastewater test may have produced different results, since chelant type influences the reduction potential of metal ions in solution.2 Effect of DH on Cormer Removal: Svnthetic Wastewater #1 A synthetic copper-edta solution containing 24 ppm of chelated copper was tested at five phs: 8.0, 8.25,8.5,8.75,9.0. The results of the tests neur the equivalence point are summarized in Figure 4. Copper concentration decreased to ~0.1 ppm in all the tests at similar precipitant dosage. The ORP potential curves shifted somewhat with ph, though all have an inflection. Table 1 shows the effect of ph on dosage at ORP potential setpoints -60 and -80 mv. Except for the ph 8.25 test, the resulting copper concentrations were ~0.8 ppm with an overall dosage range of 2 4% of the mean dosage. These results indicate that ph is not a strong factor in ORP dosage control, at least for chelated copper. In actual wastewater, the presence of other active components might produce different ph effects. Table 1. Effect of ph on Dosage at Fixed ORP Setpoints (-60 & -80 mv) -60 mv -60 mv -80 mv -80 mv ph DosaPe Cu,uum Dosage Cu.p~m ND~ 338 ND o ND=non-detectable (<0.1 ppm) Mixed Metals. Comer and Nickel: Svnthetic Wastewater #2 A synthetic, chelated wastewater containing copper and nickel was prepared with sodium citrate. Initial copper and nickel concentrations were 16 and 23 ppm, respectively. An ORP test was conducted at ph 8.5. The results are shown in Figure 5. The ORP potential curve showed two inflections; the first corresponding to disappearance of copper and the second to nickel disappearance. The potential 4 312
5 curve inflection for copper was larger than that for nickel. These results suggest that ORP can be used for process control when these two active metals are present. Brass (Cu/Zn)Platine: Plant #4 Wastewater was provided from brass plating operations in which copper and zinc were chelated with cyanide before chlorine destruction. The resulting wastewater was strongly buffered at ph 8.5 and had 90 ppm of copper and 9 ppm of zinc. Normal treatment consisted of precipitant addition to the batch tank with water recirculation for mixing. An ORP test was conducted without ph adjustment or control, and the results are shown in Figure 6. As is typical of mixed metal wastes, copper was preferentially removed by the precipitant to c1 ppm before substantial zinc removal occurred. The ORP potential curve shows a strong inflection corresponding to the disappearance of copper and then a steady decline in potential with decreasing zinc concentration. Though ORP did respond to zinc removal, the potential curve simply leveled off at excessive precipitant dosage. This response could cause product dosage control to be more variable, compared to control at an inflection in the potential. A single set of ORP potential setpoints must be used for proportional control of this batch process, since both metals must be removed. Thus, these setpoints must correspond to Zn removal. Conclusions While metal ion precipitation is not a redox process, it appears that removal of certain metals can be accurately monitored with ORP probes. In laboratory studies, marked response of ORP was seen at the equivalence point (dosage corresponding to metal ion disappearance) for a copper-bearing wastewater, a synthetic copper-nickel wastewater, and a copper-zinc wastewater. No response was seen for a zinc wastewater that had been chelated with citrate ion. ORP responds to the disappearance of certain metal ions, such as copper and nickel, that are active at the electrode. The effect of ph on ORP response was observed for synthetic, chelated copper wastewater. The inflections in the ORP potential curves shifted somewhat with ph, but the effect on dosage at two fixed potential setpoints was minimal. Thus, there was little impact of ph on ORP response, though actual wastewater may contain other active components that ure affected by ph. The presence of an interference in one circuit board plating wastewater predicted severe product overfeed under ORP control. The need for waste stream equalization or removal of the suspect stream from the continuous process was suggested
6 Acknowledeements The authors wish to acknowledge - David Picco of Nalco Research for his capable work. References 1. Snowden. E Curtis and Bernard 1. Galetti, Oxidation-Reduction Potential: Theory and Application- to Plating-Waste Controls, ISA Trans., 7(4), 3049, Stumm, Werner and James J. Morgan, Aquatic Chemistry: An Introduction Emphasizing Chemical Equilibria in Natural Waters, John Wiley & Sons, Inc, New York, 36543,
7 ORP RESPONSE TO Cu REMOVAL ILLUSTRATING POSSIBLE CONTROL PARAMETERS (Figure 1) L -0- Pum cu -0- ORP mv OOSAGE (PPMI ORP RESPONSE TO CU REMOVAL ILLUSTRATING EFFECT OF INTERFERENCE (Figure 2) 300L M ool\ ORP mv I I m - I I I I -100 I, I 1 0 OOSAGE (PPM1 '. 4 ORP RESPONSE TO REMOVAL OF zn CHELATEO WITH CITRATE (Figure 3) 2 o z n L -0- ORP mv E -0- PPM ZN V E L DOSAGE loem1 31 5
8 ph EFFECT ON ORP RESPONSE FOR CHELATED Cu REMOVAL (Figure 4) V S k -0- ph A- ph V- DH ph PH OOSAGE lppm1 ORP RESPONSE TO w/ni REMOVAL FROM MIXED METAL WASTEWATER (Figure 5) P O P m M : L 1 2. " M -60 E t A L -140 S 0 T -0- ORP mv -0- PPm NI - A- Dum cu oo~aom (ppml M.OR --- ORP RESPONSE TO Cu/Zn REMOVAL FROM BRASS PLATING WASTEWATER (Figure 6) M E T A L S -0- orp mv -D- zn xi0 -A- ppm Cu
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