APPLICATION NOTE ICP-Optical Emission Spectroscopy Authors: Deborah K Bradshaw Atomic Spectroscopy Training and Consulting Laura Thompson PerkinElmer, Inc. Shelton, CT The Analysis of Water and Wastes by U.S. EPA Method 200.7 Using the Optima 8300 ICP-OES and prepFAST Auto-Dilution/ Calibration System Introduction The prevention and control of water pollution is of critical importance to protecting human and environmental health. Monitoring of water and wastes is an efficacious way to prevent the introduction of pollutants and costly remediation of drinking and environmentally important waters. The United States Environmental Protection Agency (U.S. EPA), along with local regulatory bodies, is responsible for regulating water and wastes under the Clean Water Act and the Safe Drinking Water Act. Depending on the number and type of analytes, the number of samples and the productivity requirements, several different analytical techniques can be applied to measure trace elements in water and wastes. U.S. EPA Method 200.7 Version 4.4 covers the use of inductively coupled plasma optical emission spectroscopy (ICP-OES) in radial and/or axial viewing for the determination of metals and some non-metals in water and wastes for regulatory compliance.1 Method 200.7 contains a lengthy description of procedures for the collection, preservation and preparation of samples for analysis. The objective of this work was to complete the method using the PerkinElmer® Optima® 8300 ICP-OES coupled with the prepFAST™ Automated In-Line Auto-Dilution/Calibration System (Elemental Scientific Inc., Omaha, NE). The prepFAST™ system provides a number of advantages over conventional ICP-OES introduction systems, the most significant of which is higher sample throughput and reduced memory effects. The prepFAST™ system allows accurate, syringe-driven auto dilution of samples and standards, eliminating manual dilution errors and increasing calibration range. Reducing costly high-purity reagent and sample consumption, the prepFAST™ Auto-Dilution/ Calibration System is one of the best ways to improve laboratory productivity. 7)Laboratory reagent blank (LRB) – Analyze one every 20 samples. Should be below MDL. Summary of Method 200.7 Experimental Conditions The direct analysis of samples was performed according to Method 200.7. For samples that require total recoverable analysis, refer to section 11.2 of EPA Method 200.7 rev 4.4. Below is a summary of the steps required for compliance with EPA 200.7 revision 4.4. Instrumentation 1)For direct analysis (samples with < 1 NTU), dilute, if necessary, to an appropriate volume and preserve samples to a pH < 2 with ultrapure HNO3. 2)Optimize the instrument using the plasma solution (section 10.2.3) after allowing 15-30 minutes for the plasma to stabilize to the environment. 3)Calibrate the instrument using at least one blank and one calibration standard. 4)Run the instrument performance check (IPC sample) immediately following daily calibration and verify its recovery within 5%. The IPC should also be run after every 10th sample and at the end of a sample run and recovered within 10%. 5)Prepare an inter-element correction (IEC) table, if necessary, and analyze the spectral interference check (SIC) solution to verify lack of spectral interferents in the method. This should be repeated on a periodic basis. 2 6) Perform the initial demonstration of performance (IDP) a.Instrument detection limit (IDL) – Calculated as 3x the standard deviation of 10 replicate measurements of the calibration blank. b.Method detection limit (MDL) – Calculated as 3.14x the standard deviation of seven replicate aliquots of fortified (2-3x estimated IDL) reagent water. c.Quality control sample (QCS) – Prepared from a second source. Verify that the mean concentration of three analyses is recovered within 5%. Also run QCS quarterly or after new calibration standards are made. d.Linear dynamic range (LDR) – Analyze successively higher standard concentrations until they return 90% of the stated concentration based on a typical standard curve. Verify annually. 8)Laboratory fortified blank (LFB) – Analyze one with each batch of samples. Verify within 85-115% recovery. 9)Laboratory fortified matrix (LFM) – Spike 10% of the samples prior to sample prep. Verify within 70-130% recovery. Concentration should be ≥ 30% of background concentration. 10) Reference materials – Should be run when available. All samples were analyzed with a PerkinElmer Optima 8300® ICP-OES (Figure 1) equipped with an ESI prepFAST™ Auto-Dilution System with an ESI SC-2 DX Autosampler (Figure 2). Instrumental parameters are listed in Table 1. Elements determined and wavelengths used in this study, the peak area, points per peak, and number of background points used for each wavelength are listed in Table 2. All elements were viewed axially. For some elements, alternate wavelengths were investigated in this study. The use of an alternate wavelength may be desirable for a variety of reasons – better sensitivity and greater freedom from spectral interferences are the two primary reasons. The wavelengths cited in Method 200.7 are ‘recommended’ with the following footnote: “The wavelengths listed are recommended because of their sensitivity and overall acceptability. Other wavelengths may be substituted if they can provide the needed sensitivity and are treated with the same corrective techniques for spectral interference (see Section 4.1).” It is worth investigating these alternate wavelengths for their applicability to the method. The wavelengths recommended by Method 200.7 are denoted in the table, as well as the reason for choosing an alternate wavelength in this study. Figure 1. The PerkinElmer Optima 8300 ICP-OES with Flat Plate™ plasma technology. Table 2. Analytical parameters used for EPA Method 200.7 with the Optima 8300 ICP-OES Background Wavelength Points/ Correction Analyte (nm) Peak Points Comments Al 396.153* 1 1 Al 308.215 3 2 Sb 206.836 1 2 As 188.979* 1 1 Figure 2. The prepFAST™ Auto-Dilution System with an ESI SC-2 DX Autosampler illustrating a two-step process of loading the sample into a loop and in-line dilution. Sample and Standard Preparation As 193.696 1 2 Ba 493.408 1 2 Be 313.042 1 1 B 249.677 1 2 Cd 226.502 1 2 Ca 315.887 1 1 Ce 413.764 1 1 Cr 267.716* 1 2 Greater intensity Greater freedom from spectral interferences Greater intensity and greater freedom from spectral interferences The solutions that were prepared and used for this study are listed in Table 3. All solutions were diluted in 2% HNO3. For Sn analysis, solutions were acidified to 1%HCl/2%HNO3. For calibration, a 1 mg/L (standard 5) and a 5 mg/L (standard 10) standard, depending on the element, were prepared and the prepFAST™ system was used to automatically dilute these solutions to prepare standards 1-4 (from standard 5) and standards 6-9 (from standard 10). The concentration of each calibration standard, the prepFAST™ dilution factor, and the elements applied to each standard are shown in Table 4. The prepFAST™ system was also set up to automatically dilute samples which were over the range of the calibration curve. For this reason, several standard solutions, analyzed as samples, were deliberately prepared so that the results would be high and the prepFAST™ system would perform a dilution. Yttrium was used as the internal standard during sample analysis. Cr 205.560 1 1 Co 228.616 1 2 Cu 324.755 3 2 Fe 259.939 1 2 Pb 220.353 1 2 Li 670.794 1 2 Mg 285.213* 1 2 Mg 279.077 1 2 Mn 257.610 1 1 Mo 203.845 1 2 Ni 231.604 1 2 P 178.223* 1 2 Greater freedom from spectral interferences Table 1. Instrumental Parameters P 177.435* 1 2 Greater freedom from spectral interferences ParameterValue Nebulizer Type ESI PFA Spray Chamber Non-baffled cyclonic InjectorSapphire P 213.617* 1 2 P 214.914 1 766.490 3 2 Se 196.026 1 1 Si 251.611 1 2 Ag 328.068 1 1 Plasma Gas Flow (L/min) 8 Aux Gas Flow (L/min) 0.2 Na 589.592* 1 2 Neb Gas Flow (L/min) 0.55 Na 588.995 1 1 RF Power (watts) 1500 Sr 421.552 1 2 ResolutionNormal Tl 190.805 5 2 Read Delay (sec) 50 Sn 189.927 1 2 Peak Processing Peak area Ti 334.942 1 1 Calibration Type Linear, calculated intercept V 292.402 1 2 Torch Cassette Position -3 ESI Flow Rate (μL/min) 500 Zn 206.200* 1 2 ESI Loop Size (μL) 3000 Zn * Alternate wavelengths 1 Software-suggested wavelength 1 K 213.857 Greater intensity Argon interference (shoulder) Greater freedom from spectral interferences 2 3 Table 3. Solutions used for the calibration and QC procedures in the analysis of water by EPA Method 200.7 Designation Analytes Part Number Preparation Cal Standard 1-5, IPC Solution LFM 100 mg/L: Al, Sb, Ba, Be, Cd, Ca, Cr, Co, Cu, Fe, Pb, Mg, Mn, Mo, Ni, K, Se, Ag, Na, Sr, Tl, Sn, Ti, V, Zn 1000 mg/L: Ce 1000 mg/L: Li Instrument Cal. Std. 2: N9301721 N9300110 N9300129 Diluted to 1 mg/L for S5 Cal Standard 6-10 IPC Solution LFM 1000 mg/L: B 1000 mg/L: P 1000 mg/L: Si N9303760 N9300139 N9300150 Diluted to 5 mg/L for S10 QCS 1 100 mg/L: As, Be, Ca, Cd, Co, Cr, Cu, Fe, Li, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sr, Ti, Tl, V, Zn QC Standard 21: N9300281 Diluted to 0.4 mg/L QCS 2 1000 mg/L: K QC Standard 7A: 500 mg/L: Si N9300280 100 mg/L: Al, B, Ba, Na 50 mg/L: Ag Diluted 1000x QCS 3 1000 mg/L P N9303788 Diluted to 0.4 mg/L QCS 4 1000 mg/L Sn N9303801 Diluted to 0.4 mg/L SIC A & SIC B 5000 mg/L: Al, Ca, Mg Interferents A 2000 mg/L: Fe N9300226 1000 mg/L: Fe Stock N9300126 Prepared to 200 mg/L: Al, Ca, Mg; 300 mg/L: Fe The SIC B was spiked with the solutions used to prepare the calibration standards Sample Analytes B Solution: N9300227 Diluted 10x Sample See Tables for Elements and Concentrations Initial Calibration Verification (ICV): N9300224 Diluted 10x Sample See Tables for Elements and Concentrations HPS DWSS Secondary Drinking Water Standard Diluted 10x Sample See Tables for Elements and Concentrations HPS DWPS Primary Drinking Water Sol. A Diluted 100x Sample See Tables for Elements and Concentrations HPS CRM TMDW Trace Metals in Drinking Water No dilution 100 mg/L: Cd, Ni, Zn 60 mg/L: Sb 5 mg/L: Pb 50 mg/L: Ba, Be, Co, Cr, Cu, Mn, V 20 mg/L: Ag 10 mg/L: As Lab Sample: Sample (LM), First Morning Tap Water Sample Duplicate (LMdup), Sample Spike (LFM) Results As an initial qualification of the system, the IDLs and MDLs were determined for each of the wavelengths. The IDLs were determined over two separate days. All results are shown in Table 5. Concentrations of the analytes in the fortified solution used for the MDLs are also listed in Table 5. To validate the calibration curve, the QCS solution was analyzed after calibration was complete. The QCS solution was prepared from an alternate stock source, as is required by U.S. EPA Method 200.7. Results are shown in Table 6. The solution used for the alternate source QCS did not contain Ce. Rather than risk having contamination occur by spiking in stock, it was decided to leave the solution without this element. The QCS should be within 5% of the known value. All of the values were within this variance except for Na and K. When calibration was carried to 0.5 mg/L (rather than 1 mg/L), both of these elements were also within 5%. 4 No dilution, acidification to 2% with HNO3 The ruggedness of the prepFAST™ system to dilute solutions was tested in two different ways. First, standard calibration curves created by using the prepFAST™ system were run over several days. In all cases, for all the wavelengths used, the correlation coefficient was > 0.999, and in most cases > 0.9999. Next, an instrument performance check (IPC) was Table 4. Standards and dilutions Analyte Standard Std. Number prepFAST™ Conc. (μg/L) Dilution Factor Al, Sb, As, Ba, Be, 1 20 Cd, Ce, Ca, Cr, Co, 2 50 Cu, Fe, Pb, Li, Mg, 3 100 Mn, Mo, Ni, K, Se, 4 500 Ag, Na, Sr, Tl, Sn, 5 1000 Ti, V, Zn B, P, Si 6 7 8 9 10 50x 20x 10x 2x 1x 50 100x 10050x 50010x 10005x 500001x Table 5. Detection limits using the Optima 8300 ICP-OES with the prepFAST™ Auto-Dilution/Calibration System and EPA Method 200.7 parameters Wavelength IDL MDL Analyte (nm) (μg/L) (μg/L) Spike Concentration for MDL Solution (μg/L) 0.280.70 0.4 Table 6. Quality Control Sample (QCS) Alternate Source Wavelength QCS DeterminedRecovery Analyte(nm) (μg/L) (μg/L) (%) Al 396.153 Al396.153 100 97.9 97.9 Sb 206.836 1.21.3 3 Sb206.836 400 408 102 As 188.979 0.961.8 As188.979 400 401 101 Ba 493.408 0.010.018 0.05 Ba493.408 100 101 101 Be 313.042 0.060.083 0.4 Be313.042 400 407 102 B 249.677 0.66 B249.677 100 98.6 98.6 Cd 226.502 0.050.050 0.4 Cd226.502 400 415 104 Ca 315.887 0.39 0.58 1 Ca315.887 400 413 103 Ce 413.764 0.49 0.49 1 Ce413.764 --- --- Cr 267.716 0.12 0.15 0.4 Cr267.716 400 417 104 Co 228.616 0.21 0.22 0.4 Co228.616 400 408 102 Cu 324.755 0.48 0.69 1 Cu324.752 400 416 104 Fe 259.939 0.16 0.12 0.4 Fe259.939 400 415 104 Pb 220.353 1.2 1.1 3 Pb220.353 400 414 104 Li 670.794 0.020.023 0.05 Li670.784 400 396 99.1 Mg 285.213 0.11 Mg285.213 400 419 105 Mn 257.610 0.020.027 0.05 Mn257.610 400 416 104 Mo 203.845 0.37 0.78 1 Mo203.845 400 401 100 Ni 231.604 0.21 0.35 1 Ni231.604 400 409 102 P 178.223 2.5 3.8 5 P178.221 400 400 100 K 766.490 0.37 2.4 1 K766.490 10001045 105 Se 196.026 1.5 1.9 3 Se196.026 400 406 102 Si 251.611 1.7 3.8 5 Si251.611 500 526 105 Ag 328.068 0.170.27 0.4 Ag328.068 50.0 52.1 104 Na 589.592 0.36 Na589.592 100 102 102 Sr 421.552 0.0040.011 0.05 Sr421.552 400 419 105 Tl 190.805 0.04 0.91 1 Tl190.801 400 405 101 Sn 189.927 0.44 0.48 1 Sn189.927 1000 973 97.3 Ti 334.942 0.05 0.07 0.4 Ti334.940 400 410 103 V 292.402 0.15 0.26 0.4 V292.402 400 419 105 Zn 206.200 0.100.88 0.4 Zn206.200 400 409 102 0.55 0.30 1.7 3 3 0.4 1 analyzed after calibration, throughout the analysis, and at the end of the run. These solutions were prepared from standards 5 and 10 (depending on the analyte), using the prepFAST™ system. The results for each wavelength are shown in Table 7. For all analytes except B, P, and Si, the dilution factor was 4x. For B, P, and Si, the dilution factor was 5x. The IPC solution should not vary more than 10% during an analysis. All readings fell into this range with the average recovery reported below. WinLab™ for ICP software can automatically re-analyze any quality control sample that falls out of range, if necessary. The effect of potential interferences was investigated. An interferent solution (SIC A) was prepared from a commercial solution, and fortified to an Fe concentration of 300 mg/L, as recommended in the Method (see Table 3). A portion of this solution was also spiked with a known concentration of --- most of the analytes and used as SIC B. Only a few of the wavelengths showed visible spectral peak interference: As, Cd and V. Several of the other wavelengths suffered from an effect that produced slight baseline effects. When the analysis of the SIC A solution produced results of more than ±5.5 µg/L, a baseline effect was decided to have occurred. At that time, an IEC factor was applied to the data. All results are shown in Table 8. In all cases, except for Li, the determined value for the spiked solution, SIC B, was within 10% of the expected value. Contamination occurred during the SIC B solution preparation; therefore, the Li results are not reported. Several solutions of known concentration were analyzed as samples to determine system reliability. Results are shown in Tables 9-13. The Analytes B solution (Table 9) showed all but one diluted result for Sb within 10% of the expected value. 5 Table 7. Initial performance check (IPC) run periodically and at end of run; prepared from calibration standards 5 and 10 by the prepFAST™ system Wavelength Analyte (nm) Check Concentration (μg/L) After Calibration Check #1 Check #2 (μg/L) (μg/L) (μg/L) End of Run Recovery (μg/L) Average (%) Al 396.153 250 245 243 244 235 96.7 Sb 206.836250 255 253 258 247 101 As 188.979250 253 252 255 249 101 Ba 493.408250 252 250 249 242 99.3 Be 313.042250 245 244 244 247 98.0 B 249.677 1010 1040 1050 1050 104 Cd 226.502250 248 246 247 246 98.7 Ca 315.887250 251 251 251 249 100 Ce 413.764250 252 250 248 240 99.0 Cr 267.716250 249 249 249 240 98.7 Co 228.616250 261 259 262 255 104 Cu 324.752250 251 250 252 239 99.2 Fe 259.939250 249 251 249 245 99.4 Pb 220.353250 257 257 260 242 102 Li 670.784250 239 235 237 234 94.6 Mg 285.213250 248 255 251 237 99.1 Mn 257.610250 248 246 246 237 97.7 Mo 203.845250 254 254 256 237 100 Ni 231.604250 243 243 244 251 98.1 P 178.2211000 1047 1058 1074 1094 107 K 766.490250 239 238 239 229 94.4 Se 196.026250 253 251 255 247 101 Si 251.6111000 1050 1040 1050 1070 105 Ag 328.068250 253 253 255 239 100 Na 589.592250 244 240 244 240 96.8 Sr 421.552250 257 248 254 243 100 Tl 190.801250 253 252 256 249 101 Sn 189.927250 254 252 255 246 101 Ti 334.940250 257 256 256 243 101 V 292.402250 249 249 250 239 98.7 1000 Zn206.200 250 247246 246 264 100 The same is true for the IPC solution (Table 10) – this solution was diluted 10x by the user and then run using the prepFAST™ system either directly and/or with a 10x or 100x dilution. All recoveries for a drinking water secondary standard (HPS DWSS) were well within acceptable ranges compared to the known values (Table 11). A trace metals drinking water (HPS TMDW) standard was analyzed without dilution of any kind (Table 12). Determined results are within 15% of the certified values, except for Cu and Ag, where contamination was suspected. A drinking water primary standard (HPS DWPS) was also run (Table 13). 6 A first-morning tap water was collected to use as a sample (laboratory matrix, LM). This solution was run in duplicate and a portion was fortified with the analytes of interest as a laboratory fortified matrix (LFM). Results are shown in Table 14. Duplicates were all within acceptable limits and, with the exception of Ag, all spike results were within 15%. Based on the determined Zn and Cu concentrations in the sample, the spiked concentration should have been higher. The low Ag recovery was caused by a potential precipitation due to a significant chloride concentration in the sample. Table 8. Recovery of the SIC solution with and without the use of inter-element correction (IEC) factors Wavelength SIC A Analyte (nm) (μg/L) Comment SIC B Added (μg/L) Sb Found (μg/L)) SIC B No IEC SIC B with IEC Recovery Found Recovery (%)(μg/L) (%) 206.836 6.4 200 203 102 As 188.979 * 200202 101 N/A NA Ba 493.408 * 200201 101 N/A N/A Be 313.042 * 200194 97.0 N/A N/A B 249.677 -12 20002111 106 2122 106 Cd 226.502 39 200 111 184 92.0 Ce 413.764 -7.3 200 186 93.0 193 96.5 Cr 267.716 * 200189 94.5 N/A N/A Co 228.616 * 200187 93.5 N/A N/A Cu 324.752 10 200214 107 204 102 Pb 220.353 * 200186 93.0 N/A N/A Mn 257.610 * 200186 93.0 N/A N/A Mo 203.845 * 200191 95.5 N/A N/A Ni 231.604 -9.3 200 183 91.5 191 95.5 P 178.221 32 20002098 105 2067 103 Se 196.026 -82.87 200 60.1 198 99.2 Si 251.611 Fe interference Fe interference 221 120.2 197 98.5 16 20002128 106 2122 106 Ag 328.068 * 200209 104 N/A N/A Sr 421.552 * 200200 100 N/A N/A Tl 190.801 8.7 200 188 94.0 180 90.0 Sn 189.927 * 200182 91.0 N/A N/A Ti 334.940 * 200197 98.5 N/A N/A V 292.402 15 200 104 97.0 Zn 206.200 Fe interference * 208 200197 194 98.5 N/A N/A * No baseline effect Table 9. Sample analysis: recovery of the Analytes B solution+ (referenced to a 10x user prepared dilution) run in duplicate, for most elements, with a further 10x prepFAST™ dilution Known Wavelength Value Determined Recovery Analyte (nm) (μg/L) (μg/L) (%) Replicate 1 prepFAST™ Diluted 10x Recovery (μg/L) (%) Replicate 2 prepFAST™ Diluted 10x Recovery (μg/L) (%) Sb 206.836 6000 5088*84.5 5296 88 --- --- As 188.979 1000 905.390.5903.9 90.4 --- --- Ba 493.408 5000 4947*98.9 5064 101 4894 97.9 Be 313.042 5000 4855*97.1 4965 99.3 4830 96.6 Cd 226.502 100009830*98.3 10320 103 10130 101 Cr 267.716 5000 4880*97.6 5099 102 4990 99.8 Co 228.616 5000 4941*98.8 4931 98.6 4854 97.1 Cu 324.752 5000 4788*95.8 4860 97.2 --- --- 106 105 Pb 220.353 500 499.7 100 530.5 525.2 Mn 257.610 5000 4834*96.7 4743 94.8 4630 92.6 Ni 231.604 100009695*96.9 10090 101 9876 98.8 Ag 328.068 2000 1952*97.6 2042 102 1999 99.9 V 103 5019 100 102 10000 100 292.402 5000 4922*98.4 5128 Zn 206.200 100009763*97.6 10160 + Solution was run as a sample, not for any method requirement purposes. * Indicates over calibration range for sample run directly. 7 Table 10. Sample analysis: recovery of the ICV initial calibration verification solution+ (referenced to 10x user-prepared dilution) with further prepFAST™ dilutions at 10x or 100x, when necessary Replicate 1 Replicate 2 Known prepFAST™ prepFAST™ Wavelength Value Determined Recovery Dilution Determined Recovery Dilution Analyte (nm) (μg/L) (μg/L) (%) Factor (μg/L) (%) Factor Al 396.153 2000019900 99.7 100x --- --- Sb 206.83660006260 10410x --- --- --- As 188.97910001010 1010x --- 999 99.9 10x Ba 493.408 2000020200 101 100x --- --- --- Be313.042500494 98.6 0x 517 10310x Cd 226.502 500 480 96.00x 491 98.1 10x Ca 315.887 5000053000 106 100x --- --- Cr 267.716 1000 982 98.20x 994 99.4 10x Co 228.616 5000 4800 98.810x --- --- Cu 324.75225002750 11110x --- ----- --- --- Fe 259.939 100009660 96.6 10x 10400 104 100x Pb 220.353 300 291 97.00x --- --- --- Mg 285.213 5000049300 98.6 100x --- --- --- Mn 257.610 1500 1500 99.810x --- --- --- Ni 231.604 4000 3880 97.010x --- --- --- 766.490 5000049200 98.5 100x --- --- --- K Se 196.026 500 491 98.10x Ag 328.06810001018 1020x 495 99.0 10x 995 99.5 10x Na 589.592 5000047400 94.5 100x --- --- Tl 190.801 1000 952 99.2 10x 95.20x 992 --- V 292.40250005200 10410x --- --- --- Zn 206.200 2000 1960 --- 97.910x --- --- + Solution was run as a sample, not for any method requirement purposes. Table 11. Recovery of a drinking water secondary standard HPS DWSS (referenced to analyst prepared 10x) Known Wavelength Diluted Value Determined Recovery Analyte (nm) (μg/L) (μg/L) (%) 8 Replicate 1 prepFAST™ Diluted 10x Recovery (μg/L) (%) Replicate 2 prepFAST™ Diluted 10x Recovery (μg/L) (%) Cu 324.752 5,0004815 96.35040 101 --- --- Fe 103 9910 99.1 Mn 257.610 5,0004902 98.04850 259.939 10,00010070 101 10000 97.0 4790 95.8 Zn 206.200 5,0005073 101 5170 103 5190 104 Table 12. Recovery of a trace metals drinking water standard HPS TMDW (no dilutions were made) Table 13. Recovery of a drinking water primary standard HPS DWPS (referenced to analyst prepared 100x) Known WavelengthValue Determined Recovery Analyte(nm) (μg/L) (μg/L) (%) Known WavelengthValue Determined Recovery Analyte(nm) (μg/L) (μg/L) (%) Al396.153120 130 110 As188.979 1000 1018 102 Sb206.836 10 11 110 Ba493.408 500 483 96.6 As188.979 80 79 98.4 Cd226.502 500 508 101 Ba493.408 50 48 96.0 Cr205.5601000 907 90.7 Be313.042 20 23 115 Se196.026 500 496 99.4 Cd226.502 10 11 110 Ag328.068 100 1011 101 Ca315.887 35000 36000 102 Cr267.71620 20 100 Co228.616 25 23 92.0 Cu324.752 20 25 125 Fe259.939100 98 98.0 Pb220.353 40 41 102 Mg285.213 9000 9000 99.9 Mn257.610 40 41 102 Mo203.845 100 99 99.0 Ni231.60460 57 95.0 K 766.4902500 2658 94.1 Se196.026 10 10.06 100.1 Ag328.068 2 1.5 76.9 Na589.592 6000 6800 113 Sr421.552250 250 99.6 Tl190.80110 9.2 92.0 V 292.40230 30 100 Zn206.200 70 74 106 9 Table 14. Lab sample analysis with sample duplicate and spike Analyte Wavelength (nm) LM LM Duplicate Fortification LFM Found Recovery (μg/L)(μg/L)(μg/L)(μg/L)(%) Al 396.153 11.811.8200 216 102 Sb 206.836 13.814.4200 184 85.7 As 188.979 5.6 5.3 20018087.9 Ba 493.408 9.529.70200 210 100 Be 313.042 3.443.48200 201 99.0 B 249.677 17.918.3500 539 104 Cd 226.502 1.181.16200 195 97.0 Ce 413.764 0.7900.904200 191 95.0 Cr 267.716 1.571.56200 194 96.0 Co 228.616 < MDL Cu 324.752 14631466200 1654101 Fe 259.939 10.810.9200 202 95.5 Pb 220.353 4.1 3.6 20019193.8 Mn 257.610 5.965.99200 189 91.5 Mo 203.845 2.192.22200 195 96.5 Na 589.592 1898118790200 * Ni 231.604 9.159.43200 213 102 P 178.221 73.3 72.7 10001152107 K 766.490 21592134200 239095.2 Se 196.026 7.097.79200 192 92.6 Si 251.611 17901820500 226094.0 Ag 328.068 0.1120.018200 133.565.5** Sr 421.552 56.857.4200 252 97.5 Tl 190.801 8.307.63200 188 90.4 Sn 189.927 1.171.12200 193 96.0 Ti 334.940 < MDL V 292.402 2.122.14200 197 97.5 Zn 206.200 41341820060598.4 < MDL < MDL 200 200 195 195 97.5 * 97.5 * Spike to sample ratio was < 1 ** See note in text Conclusions This study has demonstrated the capabilities of the PerkinElmer Optima 8300 ICP-OES to produce results that meet the rigorous requirements outlined in U.S. EPA Method 200.7. The accuracy and precision of the instrument allows less time to be spent on meeting the performance requirements. The ESI prepFAST™ system simplifies sample preparation, allowing higher sample throughput, while reducing memory effects and minimizing errors and contamination. The evaluation has clearly demonstrated that the Optima 8300 ICP-OES coupled with the prepFAST™ system is well-equipped to handle the real-world demands of U.S. EPA Method 200.7 for the analysis of water samples. It has also shown that the analytical accuracy of reference materials is excellent, together with the spike recoveries in real-world drinking water samples. References 1.EPA Method 200.7 Revision 4.4, “Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry.” http:// water.epa.gov/scitech/methods/cwa/bioindicators/ upload/2007_07_10_methods_method_200_7.pdf PerkinElmer, Inc. 940 Winter Street Waltham, MA 02451 USA P: (800) 762-4000 or (+1) 203-925-4602 www.perkinelmer.com For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs Copyright ©2013, PerkinElmer, Inc. All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners. 011151A_01