Real World Analysis of Trace Metals in Drinking Water Using the Agilent 7500ce ICP-MS with Enhanced ORS Technology. Application. Authors.

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1 Real World Analysis of Trace Metals in Drinking Water Using the Agilent 7500ce ICP-MS with Enhanced ORS Technology Part 2 of a 3 part series on Environmental Analysis Application Environmental Authors Steve Wilbur, Emmet Soffey Agilent Technologies, Inc th PI SE Suite 300 Bellevue, WA USA Ed McCurdy Agilent Technologies Lakeside, Cheadle Royal Business Park Stockport, Cheshire, SK83GR, UK Abstract ICP-MS can be used as a powerful screening tool for the presence of toxic elements and chemicals in the environment. The biggest challenge in environmental ICP-MS is obtaining precise, accurate measurement in the large range of concentrations encountered in waters. Adding to this problem are interferences on important metals including As, Se, Cr, V, and Fe. Most developed countries have implemented programs and regulations to ensure the quality of public water systems, but without accurate, precise measurement of water samples, these requirements are difficult to meet. The Agilent 7500ce ICP-MS is specifically designed to meet these demanding regulatory requirements of environmental laboratories worldwide by analyzing a wide range of difficult and unknown sample types in the shortest amount of time. Using advanced ORS technology based on the use of simple gases, the Agilent 7500ce makes it possible to analyze multiple sample types over a wide range of analyte and matrix concentrations at well-below regulated concentrations, all in a single sequence. Introduction This application note represents part two of the three part series of environmental application notes based on the Agilent 7500ce ICP-MS. Part one details the theory of operation of the 7500ce octopole reaction system (ORS) inductively coupled plasma mass spectrometry (ICP-MS) system and the hardware and software advances incorporated into this new instrument Part three is an application note covering the analysis of various high matrix environmental samples using the Agilent 7500ce ICP-MS. Recent developments in both hardware and software have resulted in the new benchmark for environmental ICP-MS, the Agilent 7500ce. The 7500ce has taken the proven 7500c ORS technology to new levels of performance in sensitivity, stability, and ease of use. Since the inception of ICP-MS there have been a number of difficult challenges that have slowed its complete adoption over the more traditional techniques of graphite furnace atomic absorption (GFAA) and ICP optical emission spectroscopy (ICP-OES) in the environmental monitoring industry. The primary difficulties have been the very large range of concentrations encountered in waters and the potential for difficult-to-resolve interferences on critical elements such as As, Se, Cr, V, and Fe from common matrix components. Virtually all developed countries have adopted programs and regulations to monitor and maintain the quality of public water systems. In the US,

2 water quality is regulated by the United States Environmental Protection Agency (USEPA), as mandated by the Safe Drinking Water Act of In the European Union, drinking water is regulated by the Council Directive 98/83/EC of 3rd Nov., 1998 on the Quality of Water Intended for Human Consumption. In Japan, the quality of drinking water is regulated by the Japan Water Supply Act, dating from Most other developed countries have adopted drinking water quality standards based on World Health Organization (WHO) Standards, Guidelines for Drinking Water Quality, 1996, 1998, or on the USEPA standards. See Table 1. While these guidelines as they pertain to trace metals vary somewhat in their lists of regulated metals and concentrations, they are fundamentally similar. They all require accurate, precise measurement of multiple toxic metals in drinking waters at the lowest practical limits of quantification. The purpose of this application note is to demonstrate that the sensitivity, accuracy, and precision requirements for the analysis of trace metals in drinking water worldwide can be met or exceeded by a single, robust technique using the Agilent 7500ce environmental ICP-MS. Additionally, as regulated limits continue to decrease and the requirements for monitoring ultratrace levels of metals in ambient waters become more important, the Agilent 7500ce ICP-MS has the capability to meet future needs as well. For details of worldwide regulatory requirements, see Agilent Application Note EN, Meeting Worldwide Requirements for Trace Metals in Drinking Water using the Agilent 7500c ICP-MS [1]. Table 1. Elements Regulated Worldwide in Drinking Water, their Maximum Allowable Concentrations and the Agilent 7500ce Method Detection Limits (MDLs) for Those Elements EC Directive Japan USEPA Agilent WHO 98/83/EC drinking water Primary MCL 7500ce MDLs Analyte Isotope standard (µg/l) (µg/l) standard (µg/l) (µg/l) (µg/l)*** Aluminum (Al) * Antimony (Sb) ** Arsenic (As) Barium (Ba) Beryllium (Be) Boron (B) Cadmium (Cd) Chromium (Cr) as Cr Copper (Cu) Iron (Fe) * Lead (Pb) Manganese (Mn) * Mercury (Hg) Molybdenum(Mo) Nickel (Ni) (10)** Selenium (Se) Silver (Ag) * Sodium (Na) ppm 200 ppm Thallium (Tl) Uranium (U) (2)** Zinc (Zn) * *Secondary standard Provisional guideline value **Guideline MDLs determined according to USEPA criteria as described elsewhere in this document ***Regulatory concentrations converted to micrograms per liter (ppb) for ease of comparison 2

3 Analytical Challenges Regulatory levels for trace metals in drinking water are periodically revised downward as our understanding of their toxicity and our ability to measure them at lower concentrations improves. Additionally, the need to monitor even lower ambient levels of trace metals in difficult matrices like seawater is becoming more important. The challenge has been to extend the dynamic range of analysis to cover the ranges of the traditionally used techniques from GFAA through ICP-OES and to remove polyatomic interferences while avoiding unwanted matrix effects. Polyatomic ions formed in the plasma and interface of the ICP-MS are the main sources of interferences. See Table 2 for a list of polyatomic interferences on various environmentally important analytes. Table 2. Possible Polyatomic Interferences in Typical Environmental Samples and the ORS Mode Used to Eliminate Them Analyte Principal Corrective isotope interferences ORS mode 24 Mg 12 C 12 C He 27 Al 12 C 14 N 1 H He Ca Ar H2 51 V 35 Cl 16 O He 52 Cr Ar 12 C, 35 Cl 16 O 1 H, 36 Ar 16 O He 55 Mn Ar 14 N 1 H, 38 Ar 17 O He 56 Fe Ar 16 O, Ca 16 O H 2 or He 60 Ni 44 Ca 16 O, 23 Na 37 Cl, 43 Ca 16 O 1 H He 63 Cu Ar 23 Na He 75 As Ar 35 Cl He 78 Se Ar 38 Ar H 2 Clean drinking water samples typically require interference control for only a few elements. As, Se, Ca, V, and Fe can be problems depending on the matrix and required detection limit (DL). While it is possible to address interferences on these elements with the use of mathematical corrections, in some matrices the results can be unpredictable, resulting in elevated DLs. As a result, these elements are frequently analyzed by another technique such as ICP-OES or GFAA. The use of the ORS not only eliminates the need for complex and sometimes unreliable mathematical corrections, it extends the dynamic range in both directions allowing lower DLs for many elements and higher maximum concentrations for others. Furthermore, many drinking water samples can be quite high in dissolved minerals that can cause additional interferences. Since most commercial environmental laboratories do not have the luxury of limiting their samples to a single, well-defined type, it is important for the ICP-MS system to be able to measure multiple, unknown matrix samples under a single set of conditions. The purpose of this work is to show that drinking waters can be analyzed with high accuracy, precision, and sensitivity, even when analyzed together, in large numbers, with much more complex unknown samples. ORS - Matrix Independent Analytical Quality The Agilent 7500ce ICP-MS uses collision/reaction cell (CRC) technology in the form of the ORS to remove polyatomic interferences. The use of CRC technology to reduce interferences in ICP-MS is well documented [2,3]. Figure 1 illustrates the efficiency of interference removal in a synthetic matrix blank containing carbon (1% methanol), chloride (1% HCl), and nitrogen (1% HNO 3 ). Under normal (no gas in cell) conditions, this matrix would cause severe interferences on several analyte elements (Table 2). An excellent test of the efficiency of interference removal can be seen in these low-level calibration plots. When interferences are present, the response curve is offset in the y direction by the magnitude of the interference, increasing the background equivalent concentration (BEC) and the DL. When the interference is removed, the calibration curve intersects the y-axis at a point much nearer to zero with a correspondingly lower BEC and DL. Figure 1 depicts sub-ppb calibration curves for chromium and vanadium in 1% each methanol, HCl and HNO 3, with and without the use of helium collision mode. 3

4 BEC = 7.7 ppb BEC = 0.09 ppb BEC = 1.8 ppb BEC = 0.05 ppb Figure 1: Calibration plots of 52 chromium and 51 vanadium in 1% nitric, 1% hydrochloric, 1% methanol showing effects of interferences from ArC + and ClO + in normal mode on the left and after removal of interferences by the ORS using He on the right. Experimental All work was performed using a standard Agilent 7500ce ICP-MS system with standard MicroMist glass concentric nebulizer. Laboratory conditions were typical of a commercial environmental laboratory. The instrument was tuned for robust plasma conditions (Table 3) yielding sensitivity of approximately 50 million cps/ppm at mid-mass with background less than 5 cps, CeO + /Ce + less than 1% and Ce ++ /Ce less than 1.5%. The instrument automatically groups elements into the selected ORS mode and switches between modes while scanning each sample. No additional optimization is required for specific analytes or matrices. Since the instrument conditions are mostly the same for all three modes, switching is rapid and precise. Table 4 depicts the mode each element was acquired in. A Cetac ASX-510HS high speed autosampler was used. All water was ASTM type 1, 18MΩ/cm (MilliQ), and acids were Seastar semiconductor grade. Tracemetal grade acids are more commonly used but can contain contaminants at the very low DLs presented in this work. If low ppt MDLs are not required for all analytes, tracemetal grade acids are sufficient. In this work, an extended sequence of samples simulating the workload in a typical environmental laboratory was analyzed repeatedly for more than 15 ½ hours. The samples included high dissolved solids water samples, 1/10 diluted seawater samples and spikes, soil digests, interference check solutions (ICS-A and ICS-AB), standard reference materials and periodic calibration check samples. The system was calibrated once at the beginning of the sequence and not recalibrated or resloped during the entire sequence. The bulk of the sequence consisted of eight repeats of the sample block shown in Figure 2. The accuracy and precision of the repeat analyses of each sample type over the entire sequence were monitored. 4

5 Table 3. Instrumental Conditions Used in this Work and Typically Used for Environmental Samples of All Types Instrument parameter Normal mode Hydrogen mode Helium mode RF Power 1500 W <Same <Same as H 2 Sample depth 8 mm <Same <Same as H 2 Carrier gas 0.85 L/min <Same <Same as H 2 Spray chamber temp 2 C. <Same <Same as H 2 Extract 1 0 V <Same <Same as H 2 Extract V <Same <Same as H 2 Omega bias 24 V <Same <Same as H 2 Omega lens 0.6 V <Same <Same as H 2 Cell entrance 30 V <Same <Same as H 2 QP focus 3 V 11 V <Same as H 2 Cell exit 30 V 44 V <Same as H 2 Octopole bias 7 V 18 V <Same as H 2 QP bias 3.5 V 14.5 V <Same as H 2 Cell gas flow ml/min H ml/min He 15 1/2 hours continuous analysis <30 min Instrument optimization and tuning Initial calibration MDL Replicates Sample block repeated 8 times CCV Replicates Acid blank 5 Calibration Standards from 100 ppt to 200 ppb except: -Mercury from 10 ppt to 2 ppb -Mineral elements up to 200 ppm 7 replicates of low standard CCV CCB NIST 16 undiluted NIST 16 diluted 1/10 ICS-A ICS-AB 1/10 Seawater blank 1/10 Seawater spike (2 ppb) Brackish water sample High calcium water sample Soil digest 1/10 Soil digest 1/50 Figure 2. Analytical sequence. 5

6 Table 4. Summary of Analyte Masses, Analytical Conditions, and Measured DLs in Both Screening Mode and Full Quantitative Mode for Regulated Elements MDL MDL MDL MDL ORS Mode Integration Calibration He screening Tri-Mode Analyte Isotope (typical)* time (s) range (ppb) (ppt) (ppt)** Calcium (Ca) H , Iron (Fe) 56 H , Selenium (Se) 78 H Sodium (Na) 23 He , Magnesium (Mg) 24 He , Potassium (K) 39 He , Vanadium (V) 51 He Chromium (Cr) 52 He Nickel (Ni) 60 He Copper (Cu) 63 He Arsenic (As) 75 He Beryllium (Be) 9 Norm Boron (B) 10 Norm Aluminum (Al) 27 Norm Manganese (Mn) 55 Norm Cobalt (Co) 59 Norm Zinc (Zn) 66 Norm Molybdenum(Mo) 95 Norm Silver (Ag) 107 Norm Cadmium (Cd) 111 Norm Tin (Sn) 118 Norm Antimony (Sb) 121 Norm Barium (Ba) 137 Norm Mercury (Hg) 202 Norm Thallium (Tl) 205 Norm Lead (Pb) 208 Norm Thorium (Th) 232 Norm Uranium (U) 238 Norm Useful ISTDs 6 Lithium (Li) 6 Norm ppb Scandium (Sc) 45 All ppb Germanium (Ge) 70,74 All ppb Indium (In) 115 Norm ppb Terbium (Tb) 159 Norm ppb Platinum (Pt) 195 Norm ppb Bismuth (Bi) 209 Norm ppb * Typical ORS mode selected for best overall performance for most common matrices. Screening protocol uses He collision mode only for rapid screening where optimum sensitivity is not required for all elements, MDL calculated according to EPA requirements. ** MDLs calculated according to EPA requirements. 3-sigma of seven replicate analyses of a fortified blank at 3 5 times the estimated MDL. MDLs are reported in ng/l (ppt) for ease of presentation. Lead is measured as the sum of isotopes 206, 207, and 208 to eliminate error due to variable isotope ratios. 6

7 Results and Discussion Typical calibration plots are shown in Figure 3. By using the ORS to eliminate polyatomic interferences for some analytes and to attenuate excessive signal for others, the practical dynamic range of the analysis extends from low part per trillion levels (ppt) for elements such as Se (hydrogen reaction mode), As, V, and Cu (helium collision mode) and Hg (normal mode) to 1000s of parts per million (ppm) for high concentration elements like sodium (helium collision mode). This is accomplished in a single analysis using automatic switching of ORS conditions through three modes without the need for complex on the fly resolution changes or detector gain changes. No interference correction equations were required and all analytes were measured at their elemental mass. Table 4 summarizes the ORS conditions, calibration ranges and method detection limits for this work. Note that two sets of MDLs are reported; Screening and Tri-Mode. Depending on the data quality objectives of the analytical project, the appropriate ORS mode(s) can be selected. In Screening Mode, all elements are analyzed under a single set of helium collision conditions. Since He mode depends on kinetic energy discrimination to reduce polyatomic interferences, it is independent of analyte or matrix and can be used to effectively analyze most elements under a variety of matrix conditions. In many cases, the best possible MDLs are achieved under He conditions. These cases include analytes for which there are multiple interferences at the analyte mass and cases where the interference is unpredictable or unknown. For some elements, however, it is possible to achieve better sensitivity or interference reduction through the use of one of the other ORS modes, hydrogen or normal (no gas). Typically, for the best overall performance in unknown environmental samples, Tri-Mode is used. This mode combines the best possible sensitivity with the best possible interference removal for all analytes. All data in this work was acquired under Tri-Mode conditions, in other words, optimized for maximum performance with variable, unknown matrices. Figure 3: Calibration curves (A) mercury 10 ppt - 2-ppb normal mode, (B) arsenic 100 ppt ppb helium mode, (C) selenium 100 ppt ppb hydrogen mode, (D) sodium 50 ppb ppm helium mode. 7

8 Certified Reference Materials NIST 16 certified reference water was analyzed repeatedly throughout the sequence, both neat (without any additional acidification or matrix matching) and diluted 1/10 into 1% nitric/0.5% hydrochloric acid. Figure 4 shows the mean recoveries and %RSDs for all certified analytes in both the undiluted and diluted samples. Note that there is no difference in either the recoveries or % RSDs between the neat and diluted samples even though they differ significantly in matrix and concentration. Continuing Calibration Verification USEPA methods and good laboratory practices mandate that calibration validity be checked periodically and updated if necessary. This was 120 accomplished by measuring the continuing calibration verification (CCV) and continuing calibration blank (CCB) after every 10 analytical samples according to USEPA method The CCV sample is typically a midpoint calibration standard. The CCB is equivalent to the calibration blank. Method requires that the calibration check results be within ±10% of the actual value in order for the calibration to be in control. If any element falls outside the ±10% limit, the system must be recalibrated before proceeding with additional analyses. Figure 5 depicts the results of the 13 replicate CCV analyses during the 15.5 h sequence (one for each ten sample analyses and five more at the end of the sequence. At no time during the sequence did any element exceed the ±10% limit. No recalibrations or adjustments to the initial calibration were performed Percent (%) % RSD Be Be B B Na Mg Al Al K Ca V Cr Mn Fe Co Ni Cu Zn As Se Mo Ag Cd Sb Ba Ba Pb Pb -5.0 mean recovery (undil) mean recovery (1/10 dil) %RSD undiluted %RSD 1/10 diluted mean recovery (undil) mean recovery (1/10 dil) %RSD undiluted %RSD 1/10 diluted Figure 4: Mean recovery and percent relative standard deviation (%RSD) for eight replicates each NIST 16 (neat) and NIST 16 (diluted 1/10) acquired over 15.5 h using a single calibration CCV Recovery h total run time Percent recovery Be Na Mg Al Al K Ca V Cr Mn Fe Co Ni Cu Zn As Se Mo Ag Cd Sb Ba Hg Tl Pb Th U CCV Replicate number Figure 5. Results of 13 separate analyses of the CCV sample over the 15.5 h sample sequence. All analyte elements are reported. Acceptable control limits according to USEPA method are ±10%. At no time did any element fall outside the 10% control limits. 8

9 Summary Improvements in ion optic and octopole design, created specifically for the environmental laboratory, have resulted in an ICP-MS instrument with unprecedented sensitivity, matrix tolerance, and stability. This work was designed to replicate the workload in a typical environmental laboratory where sample matrices are not always under the control of the analyst and are frequently unknown. Under these conditions, it is not practical to matrix-match calibrations to multiple, unknown sample matrices. It is also not practical to depend on complex matrix or analyte specific reaction cell conditions. The data shown in this note were all generated using a single set of calibration standards in 1% nitric acid / 0.5% HCl. Calibration was performed once only at the beginning of the sequence and not repeated or updated during the sequence. No attempt at matrix matching either the calibration standards or CRC conditions was made. No mathematical interference corrections were employed and all analytes were measured at their elemental masses. Sample matrices varied from a clean drinking water CRM, both acidified and unacidified, through high total dissolved solids (TDS) ground waters. Also included were simulated waste samples designed to detect potential interference problems (EPA ICS-A and ICS-AB) as well as typical soil digests and 1/10 spiked simulated seawater. The results of these samples will be discussed in detail in part three of this series. In all cases, recovery of expected values was within expected limits. In summary, it is now possible, using a single ICP-MS instrument to analyze multiple sample types, over a wide range of analyte and matrix concentrations at well-below regulated concentrations in a single sequence. Conclusions The Agilent 7500ce ICP-MS was designed specifically to meet the demanding requirements of environmental laboratories worldwide that must adhere to rigorous regulatory requirements while analyzing a wide range of difficult and unknown sample types in the shortest amount of time. Using advanced ORS technology based on the use of simple gases, the 7500ce is easy to set up and operate, and delivers unprecedented DLs in a wide range of unknown sample types. References 1. S. Wilbur and Emmett Soffey, Meeting worldwide regulatory requirements for trace metals in drinking water using the Agilent 7500c ICP-MS, Agilent Technologies, publication EN 2. Comparing collision/reaction cell technology for real-world application, Agilent Technologies unpublished Technical Brief, available from your local Agilent Representative. 3. E. McCurdy and G. Woods (2004), The Application of collision/reaction cell inductively coupled plasma mass spectrometry to multi-element analysis in variable sample matrices, using He as a non-reactive cell gas JAAS 2004, 19 (3). For More Information For more information on our products and services, visit our Web site at 9

10 Agilent shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material. Information, descriptions, and specifications in this publication are subject to change without notice. Agilent Technologies, Inc Printed in the USA March 31, EN

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