Inductively coupled plasma mass spectrometry (ICP
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1 Reduction of Carbon-Based Interferences in Organic Compound Analysis by Dynamic Reaction Cell ICP MS The authors show that dynamic reaction cell ICP MS can eliminate a number of argonand carbon-based polyatomic interferences, allowing the determination of many critical elements in problematic organic compounds found in the semiconductor industry. Yoko Kishi, Katsu Kawabata, Haiying Shi, and Robert Thomas Inductively coupled plasma mass spectrometry (ICP MS) traditionally has been an indispensable analytical tool for the semiconductor industry because of its ability to determine analytes simultaneously at the sub-part-per-trillion (ppt) level in various process chemicals. However, it is extremely important to address certain potentially problematic areas when analyzing organic solvents directly, including: Viscosity and volatility of organic solvent. The viscosity and volatility of organic solvents have a significant effect on the efficiency of sample introduction and ICP stability. A higher viscosity solvent causes inefficient nebulization, which requires dilution either with water, if it is water miscible, or with some other organic solvent if it is not miscible with water. On the other hand, volatile organic solvents have a higher vapor pressure and most probably would result in the plasma being extinguished. A cooled spray chamber might help to reduce the vapor pressure, but it cannot solve this problem completely because some organic solvents need to be chilled to an extremely low temperature. An alternative solution is to use an optimized sample uptake rate, where virtually the entire sample is nebulized into the plasma. In fact, a cooled spray chamber is not very critical with a well-controlled sample uptake rate. Deposition of carbon on the interface cones. If organic solvents are aspirated directly into the plasma, carbon will be deposited on the tip of the interface cones. This can be avoided by adding a small amount of oxygen into the injector gas flow between the spray chamber and the torch. The amount of oxygen depends upon the organic solvent being analyzed, but it is typically 3 7% of the nebulizer gas flow. For example, longer chain hydrocarbons require more oxygen in order to burn the carbon at the tip of the cones. The amount of oxygen is very critical, because an insufficient amount can cause IMAGE COURTESY OF ARTVILLE 1
2 Organic Compound Analysis (a) Signal (cps) Blk 1 ppb (a) y=9.33x R 2 =.9999 (b) Signal (cps) Cell gas flow (ml/min) deposition of carbon at the cones, while too much can cause erosion and result in shorter cone lifetime. Because of this harsh, oxygen-rich environment, platinum cones are recommended as opposed to the traditional nickel cones. Compatibility of sample introduction device. The compatibility of sample introduction devices with organic samples also is a very critical issue because many of the solvents actually will dissolve the peristaltic pump tubing. Other materials are more resistant, but they usually are not clean enough for ppt-level determinations by ICP MS. In order to avoid contamination from the peristaltic pump tubing, self-aspiration using a concentric nebulizer fitted with narrow diameter perfluoroalkane (PFA) tubing is recommended for the analysis of organic solvents. Reduction of spectral and matrix interferences. Polyatomic spectral interferences and matrix suppression effects due to carbon species also are Blk 1 ppb Cell gas flow (ml/min) Figure 1. NH 3 cell gas optimization of (a) 24 Mg and (b) 52 Cr in a 1% isopropyl alcohol using the DRC. problematic issues in the analysis of organic solvents by ICP MS. There are several approaches used to eliminate carbonbased interferences such as CC + and ArC + using a quadrupole ICP MS system (1, 2, 3). A cool plasma is one way to reduce (c) Concentration (ppt) R 2 =.9996 y=16.73x R 2 = Table I. DRC instrumental parameters and sample introduction components. Argon plasma gas 18 L/min Argon auxiliary gas 1.2 L/min RF power 16 W Torch Quartz with 2 mm i.d. injector Nebulizer Concentric nebulizer (Meinhard TQ-3-A3) Argon nebulizer gas.6 1. L/min Argon makeup gas..3 L/min Oxygen gas.3.7 L/min Spray chamber Quartz Cyclonic (Elemental Scientific Inc.) Reaction gas NH 3 : 1 ml/min Cones Ni base with Pt insert Figure 2. Calibration curves and statistical data for (a) 24 Mg, (b) 52 Cr, and (c) 27 Al in 1% isopropyl alcohol. 2
3 Molecular Spectroscopy Workbench 3, 25, 2, 15, 1, 5, 1 C C 2 CN Ar ArH ArC Ar 2 2 these interferences as well as to minimize the background from contaminants of the cone material. However, because of its lower temperature, a cool plasma cannot ionize many elements sufficiently, such as boron, that have high ionization potential. In addition, the cool plasma approach suffers from matrix suppression effects because most elements cannot m/z Figure 3. Overlaid spectra of NMP blank in standard (green) and DRC (black) modes. be ionized completely in a low-temperature plasma (4). This problem is more significant for organic samples with high molecular weight, such as N-methyl pyrrolidone (NMP) and photoresist, because the cool plasma doesn t have enough energy to decompose them. A cooler plasma temperature is more desirable to reduce both polyatomic ion interferences and contaminants from the cone material, but a hotter plasma temperature most definitely is required to minimize matrix suppression and to efficiently decompose organic compounds. Collision cells using multipoles and low reactive gases also have proved useful in reducing polyatomic interferences in ICP MS (5). However, this approach necessitates the use of kinetic energy discrimination to remove the unwanted collisional by-product ions that are formed inside the cell. This typically is achieved by setting the collision cell potential slightly more negative than the mass filter potential, which means the lower kinetic energy collision-product ions (as a result of the collision process) are rejected, while the analyte ions are transmitted. Unfortunately, this produces a loss of sensitivity, which is more significant for lighter elements because those ions tend to lose more kinetic energy per collision, compared with the heavier ions (6). The problem is exaggerated with organic samples because of the large number of carbon-, oxygen-, and argon-based byproduct ions that are formed. For these reasons, instruments that use collision cells with kinetic energy discrimination often have to revert Table II. Quantitative results for 1% isopropyl alcohol. A value of zero in the NH 3 gas flow column indicates that the element was determined in standard mode with no gas flow used (N.D. = less than DL). Element m/z BEC DL (ppt) NH 3 flow Element m/z BEC (ppt) DL (ppt) NH 3 flow (ppt) (ml/min) (ml/min) Li 7 N.D. 4. Cu B Zn Na Ga 69 N.D Mg 24 N.D As Al Mo 98 N.D. 1.8 K Sr Ca Cd 114 N.D..8 Ti 48 N.D..6.3 In V Sn 12 N.D..6 Cr Sb Mn Ba Fe Tl 25 N.D. 1.5 Co Pb 28 N.D..6 Ni Bi 29 N.D..2 3
4 Organic Compound Analysis Table III. Analysis of various organic compounds in different organic solvents. Elements in red were determined under DRC conditions using NH 3 as the reaction gas, while elements in black were determined under standard mode conditions. (The precision values for all quantitative data in this table were 1 4% RSD for the three replicates.) Element m/z 3% Photoresist 1% ARC in NMP in MMP in ethyl lactate in PGMEA in PGME in NMP Unspk Spk Rec Unspk Spk Rec Unspk Spk Rec Unspk Spk Rec Unspk Spk Rec Unspk Spk Rec (ppb) (ppb) (%) (ppb) (ppb) (%) (ppb) (ppb) (%) (ppb) (ppb) (%) (ppb) (ppb) (%) (ppb) (ppb) (%) Li 7 < < < Na Mg < < Al < K Ca < Cr < < Mn < Fe Ni < Cu < Zn Pb 28 < < < to using cool plasma conditions to achieve the desired detection when analyzing organic matrices (7). Dynamic reaction cell. The dynamic reaction cell (DRC ) is another approach to reducing polyatomic spectral interferences that doesn t discriminate by kinetic energy (3). This approach has been described previously in the literature for the analysis of semiconductor materials (8, 9). The dynamic reaction cell is a pressurized quadrupole positioned before the analyzer quadrupole. A highly reactive gas, such as pure ammonia, is supplied to the cell, where ion molecule chemistry occurs. Through various mechanisms, the highly reactive gaseous molecules react with the interfering ions to convert them either into species of different mass than the analyte or into neutral species. The analyte mass then emerges from the dynamic reaction cell free of its interference and enters the analyzer quadrupole for conventional mass separation. The advantage of using a quadrupole in the reaction cell is that the ion stability regions are well defined, as opposed to those of a hexapole or an octapole. As a result, the quadrupole inside the Normalized signal Time (min) reaction cell can be operated with a relatively narrower mass transmission window, not just as an ion guide. Therefore, optimizing the quadrupole prevents unwanted reactions between the gas and the sample matrix or solvent, which potentially can lead to new interferences, while not affecting transmission of analyte ions. Every time an analyte and interfering ion enter the dynamic reaction cell, the bandpass of the quadrupole automatically is optimized for that specific analysis and then changed onthe-fly for the next analyte. The Li (3.3%) Be (3.3%) B (1.7%) Na (1.1%) As (1.6%) Mo (2.8%) Pd (1.8%) Cd (2.3%) Sn (1.5%) Sb (3.8%) W (1.3%) Au (1.3%) Pb(1.4%) Bi (2%) Figure 4. A 15-h long-term precision run of.5 ppb analytes in PGMEA using standard mode. (Both DRC and standard condition elements were determined in the same multielement run, but are shown separately for clarity.) 4
5 Molecular Spectroscopy Workbench Normalized signal other major advantage of the dynamic reaction cell is that it can be operated using hot plasma conditions, which offer several benefits for the analysis of organic solvents, as described earlier. Experimental To exemplify the benefits of dynamic reaction cell ICP MS for the analysis of complex organic samples, the following semiconductor process chemicals were analyzed: Isopropyl alcohol N-Methyl pyrrolidone (NMP) Propylene glycol monomethyl ether acetate (PGMEA) Propylene glycol methyl ether (PGME) Methyl methoxypropionate (MMP) Time (min) Mg (3.2%) AI (1.8%) K (1.9%) Ca (2.2%) Ti (2.6%) V (1.6%) Cr(1.4%) Mn (1.5%) Fe (1.1%) Co (1.6%) Ni (2.5%) Cu (1.6%) Zn (2.4%) Figure 5. A 15-h long-term precision run of.5 ppb analytes in PGMEA using DRCmode conditions. (Both DRC and Standard condition elements were determined in the same analytical run, but are shown separately for clarity.) Ethyl lactate Photoresist Antireflective coating (ARC) The instrumentation used for this experiment was an ELAN DRC II (PerkinElmer-SCIEX, Concord, Ontario, CA). Instrumental parameters and sample introduction components are shown in Table I. Results and Discussion Removal of interferences. It is well recognized that the dynamic reaction cell can remove the argon plasmarelated interferences such as Ar +, ArH +, and ArO + completely, using pure NH 3 as a reaction gas (3). For this reason, it was decided to investigate the use of NH 3 gas for the reduction of carbon-related interferences such as CC +, CN +, and ArC + on the determination of Mg, Al, and Cr. The optimization plots for 24 Mg and 52 Cr in isopropyl alcohol are shown in Figure 1. The x axis represents the NH 3 cell gas flow rate, while the y axis is the signal intensity. The steep slope of the isopropyl alcohol blank shows that both the CC + and ArC + interferences are reduced by four to five orders of magnitude. At a flow rate of approximately.6 ml/min of NH 3 gas, the slopes of the isopropyl alcohol blank and 1 ppb spiked isopropyl alcohol become parallel, which indicates that approximately a ppt level of impurity of Mg and Cr exists in the isopropyl alcohol blank. The dynamic bandpass tuning of the DRC rejects NH 3 ions generated in the cell immediately, which prevents undesirable side reactions from taking place (3). As a result, the analyzer quadrupole always is at a more negative potential compared to the reaction cell, so that it doesn t use the difference in kinetic energy to discriminate the harmful species. All ions leaving the cell are introduced into the analyzer quadrupole mass filter, which is a critical difference between the DRC approach and the collision cell. Table II represents the results of the isopropyl alcohol analysis by the method of standard additions, together with the NH 3 gas flows used (a value of zero indicates that the element was determined in standard mode). The background equivalent concentration (BEC) and detection limit (DL) were calculated based upon the isopropyl alcohol blank signals and three times the standard deviation of blank isopropyl alcohol, together with the slope obtained from the calibration curves. Three of the calibration curves (with statistical data), for, 2, 6, 1, and 2 ppt AN ICP MS SYSTEM OPERATING UNDER OPTIMIZED SAMPLING CONDITIONS CAN MINIMIZE THE AMOUNT OF UNDESIRABLE CARBON-BASED SPECIES ENTERING THE MASS SPECTROMETER WHEN ASPIRATING ORGANIC MATRICES. 5
6 Organic Compound Analysis 24 Mg, 52 Cr, and 27 Al in a 1% isopropyl alcohol, are shown in Figure 2. It should be emphasized that isopropyl alcohol was chosen for this test because it represents one of the most important organic solvents used in the semiconductor manufacturing process. As a result, the Semiconductor Equipment and Materials International (SEMI) standards organization sets extremely high purity levels for this chemical. Because of its high purity, no clean organic solvent was available for a calibration blank and as a result, the method of standard additions was used for quantitation. Cell gas optimization. Some elements showed slightly higher BEC values because of impurities in the isopropyl alcohol, as confirmed by the cell gas optimization graphs. In order to achieve the best BEC for each analyte in a multielement run, three different NH 3 gas flows (.3,.6, and 1. ml/min) were used, as shown in Table II. Once the measurement is initiated, the DRC vent valve is closed and the gas flow is adjusted to the highest flow in the method. First, the data acquisition for the elements with the highest cell gas flow (for example, Ca) are performed automatically. Then the cell gas flow is reduced to the second highest flow, and the data acquisition performed automatically after 15 s of stabilization time. Once the data acquisition for all elements in the DRC mode is completed, the vent valve is opened to evacuate NH 3 gas from the cell, and the data acquisition for all elements in the standard mode is performed after 15 s of stabilization time. For the analysis of all the elements listed in Table I, it takes about 2 1/2 min for three replicates using a 1-s integration time for each element. Controlling the cell gas flow with the vent valve is essential to the successful operation of the DRC. When the standard mode is applied, the cell gas is stopped and the vent valve is opened, which evacuates NH 3 gas from the cell. This allows the pressure inside the cell quickly to become the same as the main quadrupole mass filter. Without having the vent valve, the pressure in the cell would become higher, even though no gas is introduced. This would reduce the mean free path of the ions and cause formation of by-product ions in the cell by the collisional process. Therefore, to eliminate by-product ions with the collision cell approach, kinetic energy discrimination must be used every time, even for elements determined in the non-collision gas mode (6). Analysis of various organic compounds. The same DRC conditions for isopropyl alcohol were used for other organic matrices such as NMP, PGMEA, PGME, MMP, photoresist, and antireflective coating. Because the DRC conditions are independent of matrix, the same condition was used for all the solvents. Figure 3 is the overlaid spectra of a sample of NMP in standard and DRC modes. The DRC mode at.5 ml/min of NH 3 gas flow can eliminate the majority of argonand carbon-based spectral interferences although to achieve the best BEC values, the three different cell gas flows, shown in Table II, are preferred. Figures 4 and 5 show 15-h longterm precision runs for.5 ppb of 27 analytes in PGMEA using standard mode and DRC-mode conditions respectively. This test was performed overnight by continually aspirating the sample contained in a capped, large-volume PFA bottle. (An autosampler was not used for this test because solvent evaporation in open containers would have been a problem during the time period.) Both sets of elements were determined in the same multielement run with no recalibration, but are shown separately for clarity. This kind of stability test measures the capability of an ICP MS system to run organic samples unattended without carbon deposits building up on the cones. Running an instrument for h of daily use is considered fairly typical for a highthroughput semiconductor lab. Table III is a summary of the quantitative results (average of three replicates) of a number of photoresists and anti-reflective coatings diluted with various USING PURE NH 3 ASTHEREACTIONGASANDONESET OF DRC CONDITIONS, THE FULL SUITE OF SEMICONDUCTOR ELEMENTS CAN BE DETERMINED IN MANY OF THE ORGANIC ELEMENTS USED IN THE INDUSTRY. organic solvents.concentration values of the organic compounds were measured against external aqueous stock standard solutions (PEPure, PerkinElmer Life and Analytical Sciences) made up in the organic solvent (which also was used as the blank). Whereas the reported spike recovery data were generated by making spiked additions directly in the actual samples, all sample preparation and dilutions were performed gravimetrically in PFA bottles. It should be noted that these organic chemicals are not as wellregulated by the SEMI standards organization as isopropyl alcohol and as a result there are no published elemental specifications or guidelines in the SEMI Book of Semiconductor Standards. For this reason, the list of analytes represents a typical suite of elements that are used within the industry. Summary It has been demonstrated that an ICP MS system operating under optimized sampling conditions can minimize the amount of undesirable carbon-based species entering the mass spectrometer, when aspi- 6
7 Molecular Spectroscopy Workbench rating organic matrices. It also has been shown that by using a dynamic reaction cell, the argon- and carbon-based polyatomic spectral interferences can be reduced significantly, allowing for the determination of many of the traditionally problematic elements by ICP MS with good spike recovery and precision. Using pure NH 3 as the reaction gas and one set of DRC conditions, the full suite of semiconductor elements can be determined in many of the organic compounds used in the industry. In addition, running with hot plasma conditions allows for the determination of elements with both high and low ionization potential in a multielement run, with the minimum of matrix suppression, even for complex organic matrices. References 1. F. Meyer, J. White, and M. Radle, Semiconductor International (Web site), June E. McCurdy and D. Potter, Semiconductor International (Web site), October, S. Tanner and V. Baranov, Plasma Source Mass Spectrometry (The Royal Society of Chemistry, Cambridge, 1999), p K. Kawabata and Y. Kishi, Proceedings from Semiconductor Pure Water and Chemical Conference, Los Altos, CA, pp (21). 5. I. Feldman, N. Jakubowski, C. Thomas, and D. Stuewer, Fresenius Journal of Analytical Chemistry 365, (1999). 6. N. Yamada and J. Takahashi, Winter Conference on Plasma Spectrochemistry, Scottsdale, AZ, January, J. Takahashi, K. Youno, and K. Mizobuchi, Proceedings from Semiconductor Pure Water and Chemical Conference, Los Altos, CA, pp (24). 8. K. Kawabata Y. Kishi, and R. Thomas, Analytical Chemistry 75(9), 423A, J.M. Collard, K. Kawabata, Y. Kishi, and R. Thomas, Micro, (1) 39 46, 22. Katsu Kawabata is semiconductor business development specialist for PerkinElmer Instruments. Yoko Kishi is ICP MS product specialist for the Semiconductor Business Unit of PerkinElmer. Haiying Shi is an analytical chemist for Brewer Science (Rolla, MO). Robert Thomas is principal of Scientific Solutions (Gaithersburg, MD). Reprinted from SPECTROSCOPY, September 24 Printed in U.S.A. Copyright Notice Copyright by Advanstar Communications Inc. Advanstar Communications Inc. retains all rights to this article. This article may only be viewed or printed (1) for personal use. User may not actively save any text or graphics/photos to local hard drives or duplicate this article in whole or in part, in any medium. Advanstar Communications Inc. home page is located at _1
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