United States Environmental Protection Agency Risk Reduction Engineering Laboratory Cincinnati, OH 45268 Research and Development EPA/600/SR-94/050 April, 1994 EPA Project Summary Cadmium and Chromium Recovery from Electroplating Rinsewaters Arun R. Gavaskar, Robert F:. Olfenbuttel, and Jody A. Jones This evaluation addresses the prod- uct quality, pollution prevention po- tential, and economic factors involved in the use of ion exchange to recover cadmium and chromium from elec- troplating rinsewaters and to remove contaminants for reuse of rinsewater. Cadmium, chromium, and cyanide (which is part of the cadmium bath) are on EPA's 33/50 list of target chemicals. Test results showed that the water returned to the rinse after ion exchange was of acceptable quality for both the cadmium and chromium pro- cesses. The ion exchange resins are regenerated with sodium hydroxide (NaOH). On the cadmium line, the regenerant was subjected to electro- lytic metal recovery (EMR) to recover cadmium for reuse in the plating bath. On the chromium line, the regenerant was passed through a cation exchange resin in an effort to recover chromic acid. Although the recovery results were good on the cadmium line, chro- mic acid could not be recovered in this test. The pollution prevention potential of ion exchange on the cadmium and chromium rinsewater is good; however, further testing is needed to establish good recovery of chromium as chro- mic acid from the regenerant. The ion- exchange processes also proved economically viable. This Project Summary was developed by the U.S. EPA's Risk Reduction En- gineering Laboratory (RREL), Cincin- nati, OH, to announce key findings of the research project that is fully docu- mented in a separate report of the same title (see Project Report ordering infor- mation at back). Introduction This study, performed under the U.S. EPA Waste Reduction and Innovative Technology Evaluation (WRITE) Program, was a cooperative effort among EPA's RREL, the Connecticut Hazardous Waste Management Service, and the Torrington Company. The objective of the WRITE Program is to evaluate, in a typical work- place environment, examples of prototype or innovative commercial technologies that have potential for reducing waste. The ion exchange system used in this study was manufactured by CTEO Tek, Inc.* and supplied by Plating Services, Inc. Other ion exchange units and technolo- gies applicable to the same wastestream (electroplating rinsewaters) are also commercially available. The objectives of this study were to evaluate (1) the effectiveness of the ion exchange unit in cleaning the rinsewater for reuse in the rinse tanks, \2.) the pollu- tion prevention potential of this technol- ogy, and (3) the cost of ion exchange versus the cost of the former practice (dis- posal). Figure 1 shows the cadmium ion ex- change system configuration. The water from Rinse 1 tank is first passed through a filter to prevent suspended solids from contacting the resin in the ion exchange column. The anionic resin captures the cadmium-cyanide complex, and the water Mention of trade names or commercial products does not constitute endorsement or recommendation for Printed on Recycled Paper ------- is returned to the Rinse 2 tank. An emer- gency bypass valve allows this water to be discharged to waste in case cadmium or cyanide levels are found to be too high. The resin is periodically regenerated with a 15 to 20% NaOH solution, and the regenerant is taken to the electrolytic metal recovery (EMR) unit, where cadmium is recovered on the cathode and returned to the plating tank. Some cyanide is de- stroyed by decomposition during the EMR process. Figure 2 shows the chromium system configuration. The primary ion exchange resin is anionic to remove hexavalent chrome. In the future, a cationic resin com- ponent will be added to the primary resin to remove any trivalent chrome that may be present in the rinsewater. The anionic resin is also regenerated with a 15 to 20% NaOH solution. The resulting solution (so- dium chromate) is run through a second- ary (cationic) exchange unit that should convert the regenerant back to chromic acid and return it to the plating tank. Product Quality Evaluation The objective of this part of the evalua- tion was to show that water processed through the ion exchange system is clean enough for use as rinsewater in the cad- mium or chromium plating lines. Contami- nant-free rinsewater ensures a good workpiece finish. The approach was to collect three samples each of the rinsewater, before and after passing through the ion exchange system. These samples were analyzed in the laboratory to evaluate the removal of contaminants. In addition, batches of rinsewater (one batch for cadmium and one for chromium) were spiked with plating bath solution to elevate contaminant levels (cadmium or chromium), and the spiked rinsewater was run through the ion exchange to test the limits of the unit. Because rinsewater was continuously circulated through the ion exchange system during the day, three samples of the rinsewater at the begin- ning, middle, and end of a shift were taken to ensure that water quality remained relatively steady over time. Table 1 presents the results of the labo- ratory analysis of the cadmium rinsewater Workpiece -. .., .y' Metering \ ,.-* ". /Pump Make-up \ / '" u-JL^JLi ^_JLr~ *J Cadmium \stiilRin*r Ri 1 R, \ I Plating Tank \(Dragout) | \ Rinse 1. j HOT Recovered ป Emergency Bypass to Cadmium | Cyanide Wastestream Rinse 2 L , EMR Unit Make-up Water Regenerant Tank Legend * Rinse Water ป Workpiece >. Regenerant Filter Cartridge Figure 1. Ion exchange recovery of cadmium from plating rinsewater. Workptecet Catering ''.% f'" Pump Make-up Chromium I Plating Tank Recovered Chromium To Chrome Reduction Wastestream KVJT -+ซ- Rinse 1 I Rinse 2 Secondary Catkin Exchange Make-up Water Regenerant Legend * Rinse Water ป Workpiece ป Regenerant Filter Cartridge Figure 2. Ion exchange recovery of chromium from plating rinsewater. ------- Table 1. Cadmium Rinsewater Analysis Sample No. CD-X1-B1 CD-X1-B2 CD-X1-B3 CD-X1-A1 CD-X1-A2 CD-X1-A3 CD-XS-B1 CD-XS-A1 CD-R1-B1 CD-R1-B2 CD-R1-B3 CD-R2-B1 CD-R2-B2 CD-R2-B3 CD-X30-B1 CD-FB-1 Sample Description Before ion-x, Run 1 Before ion-x, Run 2 Before ion-x, Run 3 After ion-x, Run 1 After ion-x, Run 2 After ion-x, Run 3 Spike, before ion-x Spike, after ion-x Rinse 1, 9:00 am Rinse 1, 12:30 pm Rinse 1, 4:00 pm Rinse 2, 9:00 am Rinse 2, 12:30 pm Rinse 2, 4:00 pm Rinse 1, 30-min Field blank pH 11.26 11.41 11.48 11.45 11.51 11.51 NA NA 10.72 11.37 11.40 11.07 11.50 11.47 11.35 7.50 Conductivity (umhos/cm) 783 864 936 867 845 885 NA NA 278 823 985 360 860 970 760 65.3 Cadmium (mg/L) 7.28 2.23 2.58 0.015 <0.01 0.01 38.7 3.69 1.80 3.55 4.71 0.067 0.105 0.269 4.31 <0.01 Cyanide (mg/L) 35.60 9.26 13.80 0.037 0.047 0.041 117 14.6 8.55 15.60 24.70 0.28 0.62 1.23 17.60 <0.01 Iron (mg/L) 0.57 0.22 0.31 0.06 0.06 0.02 NA NA 0.28 0.34 0.41 0.11 0.07 0.09 0.33 0.21 Dissolved Solids (mg/L) 226 196 205 147 161 163 NA NA 90 190 225 80 164 191 189 50 Suspended Solids (mg/L) 1 < 1 < 1 <1 2 <1 NA NA 1 < 1 10 2 3 <1 3 1 (a) NA = not analyzed. samples. Most of the cadmium and cya- nide were removed by ion exchange in some cases, to below detection levels. The pH of the rinsewater remained steady at alkaline levels throughout the testing. A statistical t-test (95% significance level) was performed based on the aver- ages and standard deviations of the 1 -min "before" and "after" (CD-X1-) data. Sus- pended solids levels were very low in both "before" and "after" samples. After ion ex- change, concentrations of cadmium, cya- nide, and iron in the rinsewater decreased significantly. Overall dissolved solids lev- els also' showed a significant decrease after ion exchange; this indicated a de- cline in dissolved mass levels. Interest- ingly, conductivity did not show any significant change after ion exchange, in- dicating that the current-carrying capacity of the rinsewater did not change. During ion exchange, heavier ions (cadmium, iron, etc.) transfer to the resin and lighter so- dium ions are transferred to the water. Thus, dissolved mass in the water de- creases but conductivity remains relatively constant. Small amounts of fresh makeup water were added to the rinsewater loop from time to time to compensate for the water lost to evaporation and dragout with the parts; this also helped control conduc- tivity. Table 2 describes the results of the laboratory analysis of the chromium rinsewater samples. After ion exchange, the rinsewater pH levels were slightly al- kaline (9.31 to 9.45) because chromate ions (and any other contaminant anions) had been substituted with hydroxide ions. The alkaline pH was neutralized in the rinse tanks by the chromic acid residue on the parts (workpiece). Similar statistical analyses were per- formed on the chromium data as have been described for the cadmium data. Sus- pended solids levels were significantly re- duced by the cartridge,.filter ahead of the resin. Chromium (total chromium) and iron levels decreased significantly after ion ex- change. Iron removal may be due either to removal of ferrous suspended particles on the cartridge filter or fc> (deposition of complexed iron on the resin. As in the cadmium tests, dissolved solids mass de- creased significantly, but conductivity (cur- rent-carrying strength) remained constant after ion exchange. This is because heavier chromates in the rinsewater were replaced with lighter hydroxide ions. Pollution Prevention Evaluation The pollution prevention potential of the ion exchange technology was assessed in terms of waste volume reduction and pollutant reduction. Waste volume reduc- tion addresses the gross wastestream (e.g., Ib of wastewater treatment sludge) and affects environmental resources (e.g., landfill space) expended through disposal. Pollutant reduction addresses the specific pollutants in the wastestream (e.g., chro- mium in the sludge). Table 3 summarizes the waste volume reduction. By using ion exchange, large volumes of water are saved from going to waste. This water (an important resource) can be reused as a rinse on the cadmium and chromium lines. Without ion exchange, Torrington must maintain high rinsewater flow rates (8 gpm for the cadmium line and 2 gpm for the chromium line). These continuous flows generate large amounts of wastewater that have to be treated on site. With the ion exchange system on the cadmium line, Torrington requires only 50 gal/day to make up for dragout losses. A similar makeup rate is expected on the chromium line. Therefore, with the addi- tion of the ion-exchange system, the amount of wastewater that must be treated is reduced. Virtually eliminating the waste- water stream also eliminates the hazard- ous sludge (containing cadmium or chromium) that has to be handled, trans- ported, and disposed. In terms of pollutant reduction on the cadmium line, the pollutants of interest are cadmium and cyanide. Before ion ex- change, cadmium in the rinsewater was lost to wastewater, which was sent to an on-site wastewater treatment plant. The wastewater was treated in a steel cyanide ------- Tablt>2. Chromium Rinsewater Analysis Sample No. CR-X1-B1 CR-X1-B2 CR-X1-B3 CR-X1-A1 CR-X1-A2 CR-X1-A3 CR-XS-B1 CR-XS-A2 CR-X2-B1 CR-FB-1 Sample Description Before ion-x, Run 1 Before ion-x, Run 2 Before ion-x, Run 3 After ion-x, Run 1 After ion-x, Run 2 After ion-x, Run 3 Spike, before ion-x Spike, after ion-x Rinse 1, 30-min Field blank PH 4.83 4.67 4.41 9.38 9.31 9.45 NA(a) NA 4.68 7.50 Conductivity (umhos/cm) 103 104 106 198 126 115 NA NA 105 65.3 Total Chromium (mg/L) 20.0 18.2 21.3 0.048 0.111 0.271 33.6 0.294 19.9 0.04 Iron (mg/L) 0.90 0.85 0.87 0.15 0.20 0.26 NA NA 0.73 0.21 Dissolved Solids (mg/L) 93 99 106 96 70 71 NA NA 87 50 Suspended Solids (mg/L) 9 8 6 <1 <1 < 1 NA NA 2 1 (a) NA " Not analyzed. Tablo 3. Waste Volume Reduction Without Ion Exchange With Ion Exchange Waste Description Cadmium System Wastewater Chromium System Wastewater Amount Generated per Yearฎ 1,920,000 gal 480,000 gal Waste Description Wastewater Regenerant Fitter cartridges Wastewater Regenerant Filter cartridges Amount Generated per Yearฎ Ogal 660 gal 6 Ogal 840 gal 12 (a) Based on values of 16 hr/day, 5 days/wk, 50 wk/yr. (b) Based on pilot tests conducted by the Torrington Company and resin capacity. treatment tank using chlorine gas, sodium hypoohlor'rte, calcium hypochlorite, and NaOH to oxidize the cyanide. The cad- mium and other metals formed hydrox- ides that settled in the clarifier as sludge, which was then hauled off site for dis- posal. The treated water was discharged to the municipal sewer under a permit. At Torrington, prior to ion exchange, approximately 69 Ib of cadmium,and 281 Ib of cyanide were discharged annually. Now, because most of the cadmium can be recovered and reused, this pollutant is virtually eliminated from the wastestream. Some cyanide is also destroyed in the cadmium recovery process. On the chromium line, without ion ex- change, approximately 80 Ib of chromium Is discharged annually. With ion exchange, most of the chromium will be captured on the resin, which will be regenerated with NaOH. The regenerant then will pass through a cation exchange resin for con- version of sodium chromate to chromic acid. However; when this recovery was performed during the pilot unit testing, the final regenerant liquid still showed a pH of 13.08. This indicates that sodium chro- mate had not been converted to chromic acid; if it had been, the pH would have been much lower. This may be because (a) an excess of NaOH was used to re- generate the resin and/or (b) insufficient resin was available to exchange all the .sodium in the regenerant. Further testing is needed to determine the feasibility of the chromic acid recovery process. Economic Evaluation The economic evaluation involves com- paring the costs of the ion exchange op- eration with those of the former practice (counterflow rinse). These comparisons are summarized in Tables 4 and 5. Operating costs for ion exchange recovery are much lower than those for counterflow rinse alone. The main cost saving is the reduc- tion in Wastewater treatment costs. In addition to operating cost savings, the recovered cadmium has value because it is reused in the plaiting bath as a cad- mium anode. The cost of cadmium an- odes is approximately $15/lb. The resulting value of the 69 Ib/yr of recovered cad- mium is approximately $1,036/yr. The chromium deposited on the ion ex- change resin also has value if it can be successfully recovered as chromic acid. The cost of chromic acid is approximately $2.50/lb. Approximately 80 Ib/yr of chro- mium metal is deposited on the ion ex- change resin. This corresponds to about 154lb of chromic acid (CrO3). However, further testing is needed to establish the feasibility of chromic acid recovery from the chromium in the regenerant. The purchase price of the cadmium ion exchange system was $8,100 (including ion exchange resin column, pumps, and collection tanks). The EMR equipment price was $4,125 (including rectifier, pump, anodes, cathodes, and solution tank). In- stallation cost at Torrington, including ma- terials (piping, etc.) and labor, was approximately $3,500, to which $5,000 was added to approximate the cost of in-house pilot testing to determine specifications for the individual plant. The purchase price of the chromium ion exchange system is estimated to be $8,200 (including ion exchange resin column, pumps, and tanks). Installation cost at Torrington is expected to be $3,500, in- cluding materials '(piping, etc.) and labor. ------- Table 4. Operating Costs Comparison for Cadmium System Item Amount Used per Year Unit Cost Total Annual Cost Without Ion Exchange Freshwater Wastewater treatment With Ion Exchange Freshwater Chemicals (50% NaOH) Energy Labor i Routine maintenance - filter cartridges - EMR anode plates - EMR cathode plates - labor Waste Disposal - regenerant - filters 1,920,000 gal 1,920,000 gal 12,500 gal 96 gal 1564 kWhr 173hr 6 1 12 24 hr 660 gal 6 $0.70/1000 gal $22/1000 gal Total $0.70/1000 gal $ 1.50/gal $ 0.075/kWhr $7/hr $5 $30 $30 $7/hr $22/1000 gal $ 400/36 units Total $ 1,344 $42,240 $ 43,584 $9 $144 $117 $ 1,211 $30 $30 $360 $168 $15 $67 $ 2,151 Table 5. Operating Costs Comparison for Chromium System Item Amount Used per Year Unit Cost TotalAnnual Cost Without Ion Exchange Freshwater Wastewater treatment With Ion Exchange 480,000 gal 480,000 gal Freshwater 12,5.00 gal Chemicals (50% NaOH) 240 gal Energy 1492kWhr Labor 149 hr $ 0.70/1000 gal $15/1000 gal Total $0.70/1000 gal $ 1.SO/gal 0.075/kWhr $7/hr $336 $7,200 $7,536 $9 $360 $112 $ 1,043 Routine maintenance - filters - labor ' Waste Disposal - regenerant - filters 12 24 840 gal 6 $5 $7/hr $15/1 000 gal $ 400/36 units Total $60 $168 $13 $67 $ 1,832 The approximate cost of $5,000 for in- house testing was also added for this unit. A rough estimate of the payback period can be obtained by the following formula: Payback, years = capital costs operating cost savings + recovery value Therefore, the payback period for the cadmium ion exchange system is less than 1 year. For the chromium system, the pay- back period is approximately 3 years. Be- cause chromic acid recovery from the regenerant-is yet to be established, no recycled chromium value is assumed. The above payback period estimation is a simple calculation that (does not take into account such factors as> taxes, depre- ciation, inflation, etc. A more detailed eco- nomic evaluation, based on Ithe worksheets provided in the Facility Pollution Preven- tion Guide (EPA 600/R-92/088), was per- formed that took these factors into account. The results showed that, for the cadmium process, the return on investment (with cost of capital equal to 15%) was still less than 1 year. For the chromium process, the return on investment (with cost of capi- tal equal to 15%) was over 5 years. This includes capital costs of engineering and installation as well as increased overhead costs due to addition of the units. Conclusions and Discussion The evaluation showed that rinsewater on both cadmium and chromium lines at Torrington Company can be reused after subjecting it to filtration and ion exchange to remove impurities. Large volumes of water are thus saved, and large amounts of hazardous metals sludge are kept from the environment. The sidestreams from ion exchange are negligible compared with the wastewater and sludge wastestreams that are generated in the absence of ion exchange. The ion exchange resin can be regenerated with NaOH. On the cadmium line, the regenerant can be subjected to EMR and the cadmium recovered on the cathode. This electrode, with the depos- ited cadmium, is then inserted in the plat- ing tank as a cadmium anode. Thus, a hazardous pollutant, cadmium, is reused. On the chromium line, further testing is needed to establish the feasibility of re- covering chromium as chromic acid for reuse in the bath. Without ion exchange, the rinsewater must undergo an expensive wastewater treatment process. The cost of operating the ion exchange unit is more than offset by the savings in wastewater treatment costs and by the value of the recovered product. In addition to the direct economic benefits, the ion exchange system also reduces Torrington Company's potential liability by virtually eliminating the risks involved during off-site transport and dis- posal of hazardous sludge. The full report was submitted in fulfill- ment of Contract No. 68-CO-0003, Work Assignment No. 3-36, by Battelle under the sponsorship of the U.S. Environmen- tal Protection Agency. A-U.S. GOVERNMENT PRINTING OFFICE: 1994 - 55WW7/80Z22 ------- ------- ------- Awn R. Gavaskar, Robert F. Olfenbuttel, andJodyA. Jones are with Battelle Memorial Institute, Columbus, OH 43201-2693 Lisa Brown Is the EPA Project Officer (see below). The complete report, entitled "Cadmium and Chromium Recovery from Electroplating Rinsewaters," (OrderNo. PB94-156395; Cost: $19.50, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Risk Reduction Engineering Laboratory U.S. Environmental Protection Agency Cincinnati, OH 45268 United States Environmental Protection Agency Center for Environmental Research Information Cincinnati, OH 45268 Official Business Penalty for Private Use $300 BULK RATE POSTAGE & FEES PAID EPA PERMIT No. G-35 EPA/600/SR-94/050 ------- |