Improved Detection of Trace Elements ina Silicon Matrix Using by tzv97744

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                                                                                                                     ICP-MS
                  Improved Detection of Trace Elements in a Silicon Matrix Using a Desolvating Nebulizer System with ICP MS                                                                                                                                                     Omaha,
                                                                                                                                                                                                                                                                                Omaha NE 68144
                           Fred G. Smith, CETAC Technologies, 14306 Industrial Road, Omaha, NE 68144 3334, fsmith@cetac com and Osamu Shikino and Kyoko Kobayashi,
                                G Smith,        Technologies,
                                                        g                      Road, Omaha,    68144-3334, fsmith@cetac.com
                                                                                                                 @                                 y        y
                                                                                                                                                        Kobayashi,                                                                                                              USA
                                                                                                                                                                                                                                                                                       402 733 2829
                                                                                                                                                                                                                                                                                PHONE 402.733.2829
                     P ki El     Japan T h i l Center 4F Yokohama Business Park, 134 G d
                                 Japan, Technical C t 4F, Y k h
                     PerkinElmer J                                    B i       P k
                                                                                Park     Godo-cho, Hodogaya-ku Y k h
                                                                                         Godo-cho H d
                                                                                               h Hodogaya-ku, Yokohama 240-0005 Japan osamu shikino@perkinelmer com
                                                                                                             k Yokohama, 240 0005 J              hiki @    ki l
                                                                                                                                   Japan, osamu.shikino@perkinelmer.com                                                                                                         FAX    402.733.5292
                                                                                                                                                                                                                                                                                       402 733 5292
                                                                                  kyoko kobayashi@perkinelmer com
                                                                                   y        y    @p
                                                                              and kyoko.kobayashi@perkinelmer.com                                                                                                                                                                      CETAC com
                                                                                                                                                                                                                                                                                WWW CETAC.com




Abstract:
                                                                                   Aspire PFA Nebulizer                                              S   iti it C      i
                                                                                                                                                     Sensitivity Comparison - I                                                 Recovery Experiment
                                                  (ICP-MS)
Inductively coupled plasma mass spectrometry (ICP MS) can routinely provide
single di it and sub-ppt d t ti li it for many elements. Since trace
 i l digit d b          t detection limits f         l     t Si     t                                     Heated PFA Spray Chamber
            p                                    p                  y
element impurities in the silicon used for solar panels can adversely affect the                                                                                      Cyclonic w. Aridus II w.
                                                                                                                                                                      Cyclonic w.        II w. 
                    operation, ICP MS
efficiency of panel operation ICP-MS is commonly used for this application
                                                                 application.
                                                                                                                                                                                                                 1 Dilute the prepared Si matrix solution to
                                                                                                                                                                                                                 1.
                                                                                                                                             El
                                                                                                                                             Element         /
                                                                                                                                                            m/z         PFA‐20 
                                                                                                                                                                        PFA 20      PFA‐20 
                                                                                                                                                                                    PFA 20         F
                                                                                                                                                                                                   Factor                                     mg/L
                                                                                                                                                                                                                    concentrations up to 5000 mg/L.
This
Thi paper will d       ib the                           d
              ill describe th use of a reaction-cell quadrupole ICP MS with a
                                                             l ICP-MS ith
                                   f       ti     ll                                                                                                                     (cps)       (cps)
           g             y
desolvating nebulizer system for detection of trace elements in a Si matrix upp
to 5000 mg/L. The nebulizer system uses a PFA nebulizer / spray chamber with
                                                                                                                                               Mg             24         5460       18700           3.4
                                                                                                                                                                                                    34           2 Prepare both non spiked and spiked (2 μg/L) Si
                                                                                                                                                                                                                 2.               non-spiked
a fluoropolymer membrane desolvator for best resistance to a sample acid                                                                       In            115        20530       51750           2.5
                                                                                                                                                                                                    25              matrix solutions.
matrix of 3 to 5% HF/HNO3 or 3 to 5% H2O2. Analyte elements of interest
include Ti, V, Fe, d Mo.
i l d Ti V F and M                                                                                                                             Ba            138        17990       43530           2.4
                                                                                                                                                                                                    24
                                                                                                                                                                                                                 3.
                                                                                                                                                                                                                 3 Calibrate ICP-MS with multielement standard
Operating conditions of the reaction cell ICP-MS and the desolvating nebulizer
                                          ICP MS
                                                                                                                                               Ce            140        19490       39800           2.0
                                                                                                                                                                                                    20                 l i (0 g/       )    d
                                                                                                                                                                                                                    solution ( mg/L Si) and measure recoveries
                                                                                                                                                                                                                                                            i
system will be described Figures of merit will include enhanced analyte
               described.                                                                                                                      U             238        17470       35950           20
                                                                                                                                                                                                    2.0             for spiked Si matrix solutions
                                                                                                                                                                                                                                         solutions.
 i   l d      d ili
signal, reduced silicon matrix effects, and analyte recoveries with a high
                          t i ff t        d    l t         i    ith hi h
concentration of silicon.
                                                                                                                                                                                    1μg/L Tuning S l ti
                                                                                                                                                                                    1 /L T i     Solution
                                                                                                                       p
                                                                                         CETAC Aridus II – Front Door Open



                     Instrumentation                                                                                                                           y    p
                                                                                                                                                     Sensitivity Comparison - II                                        Recoveries in Silicon Matrix
   ICP MS:
   ICP-MS:           PerkinElmer DRCII
   ICP-AES:          PerkinElmer Optima 7300DV                                                                                                                       Cy l i
                                                                                                                                                                     Cyclonic w.  A id II
                                                                                                                                                                                  Aridus II w.                Analyte
                                                                                                                                                                                                              A l t      /
                                                                                                                                                                                                                        m/z      DRC
                                                                                                                                                                                                                                 DRC     200 
                                                                                                                                                                                                                                         200       500 
                                                                                                                                                                                                                                                   500       1000 
                                                                                                                                                                                                                                                             1000      2000 
                                                                                                                                                                                                                                                                       2000      5000
                                                                                                                                                                                                                                                                                 5000 
                                                                                                                                             Element        m/z       PFA 100 Aspire 100
                                                                                                                                                                      PFA‐100  Aspire‐100          Factor                         ode
                                                                                                                                                                                                                                 Mode   mg/L Si
                                                                                                                                                                                                                                         g/ S     mg/L Si
                                                                                                                                                                                                                                                   g/ S     mg/L Si
                                                                                                                                                                                                                                                              g/ S      g/ S
                                                                                                                                                                                                                                                                      mg/L Si   mg/L Si
                                                                                                                                                                                                                                                                                  g/ S
   D   l ti g Nebulizer Sy t
   Desolvating N b li                 Aridus
                        System: CETAC A id II                                                                                                                           (cps)        (cps)                      Na       23       Std
                                                                                                                                                                                                                                    d    123       >130      >130      >130       89

                                                                                                                                               Mg            24        14060        101730          7.2         Mg       24       Std    113       108       128       >130      108
   Low-Flow
   Low Flow PFA Nebulizers:                                                                                                                    In           115        53990        404110          7.4
                                                                                                                                                                                                                Al       27       DRC    103       109       112        95        95
                                                                                                                                                                                                                K        39       DRC    124       >130
                                                                                                                                                                                                                                                    130       130
                                                                                                                                                                                                                                                             >130       130
                                                                                                                                                                                                                                                                       >130      109
                     CETAC Aspire-100 (100 μL/min)
                            A pi 100 (      μL/ i )                                                                                            Ba           138        47160        290400          6.1         Ca       40       DRC    121       >130      >130      107       107
                     ESI PFA-100 (100 μL/min)                                                                                                  Ce           140        52730        332300          6.3         Ti       48       DRC    111        96       112       106       115
                     ESI PFA-20 (20 μL/min)
                         PFA 20                                                                                                                U            238        44840        335900          74
                                                                                                                                                                                                    7.4         V        51       DRC     82        97        89        86        95
                                                                                                                                                                                                                Cr       52       DRC    123       121       122       121       120
   Note: Aridus II PFA spray chamber can accept standard 6mm                       PerkinElmer ELAN DRCII ICP MS w. CETAC Aridus II
                                                                                                          ICP-MS w                                                                  1μg/L Tuning Solution
   diameter concentric nebulizers with flow rates up to 200 μL/min
                                                            μL/min.                                                                                                                                             Fe       56       DRC    108       129       >130      121       111
                                                                                                 ASX 112FR
                                                                                             and ASX-112FR Autosampler                                                                                          Ni       60       DRC    120       123       124       122       114
                                                                                                                                                                                                                Cu       63       DRC    114       110       111       112       114
                                                                                                                                                                                                                Zn       66       DRC    119       128       118       111        96

                                                                                           Operating Conditions - I                                                                                             Ga       69       DRC    121       120       120       116       109
                                                                                                                                                  p      p
                                                                                                                                               Sample Preparation Procedure                                     As
                                                                                                                                                                                                                A        75       DRC    123       103       129        90       111

                                                                                   ICP-MS:
                                                                                   ICP MS                 P ki El
                                                                                                          PerkinElmer ELAN DRCII                                                                                Sr       88       Std    114       115       121       120       116
                                                                                   Nebulizers:            Aspire-100, PFA-20 PFA-100
                                                                                                          Aspire 100 PFA 20 & PFA 100         Silicon matrix solution prepared from a Si wafer:                 Zr       90       Std    116       115       123       120       115
                                                                                   Spray Chamber:         Glass cyclonic                                                                                       Mo        95       Std    104       110       108       110       102
                                                                                       Power:
                                                                                   ICP P                  1600 W                              1
                                                                                                                                              1.   Wash wafer with 18 Mohm deionized waterwater.                Cd       114      Std
                                                                                                                                                                                                                                  Sd     114       115       117         2
                                                                                                                                                                                                                                                                       112        02
                                                                                                                                                                                                                                                                                 102
                                                                                                                                              2.   Remove a ~2 g  gram section of the wafer.
                                                                                   Plasma Gas:            18 L/min                                                                                              Sn       118      Std    116       117       121       117       110
                                                                                                                                              3.
                                                                                                                                              3    Wash wafer section with 1% high-purity HNO3.
                                                                                   Auxiliary Gas:         1.2 L/min                           4.
                                                                                                                                              4    Add 68% HNO3 and 38% HF to wafer section and dissol e
                                                                                                                                                                                     afer        dissolve.      Sb       123      Std    115       112       114       104        89
                                                                                   Nebulizer Gas
                                                                                   Neb li er Gas:         1 15 L/min (PFA-20)
                                                                                                          1.15       (PFA 20)                 5.                  g
                                                                                                                                                   Dilute resulting solution to 5% HF.                          Ba       138      Std    115       116       122       118       116
                                                                                                          1.12
                                                                                                          1 12 L/min (PFA-100)                6.
                                                                                                                                              6    Measure Si concentration by ICP-MS (ELAN DRCII)              W        184      Std    115       117       122       120       116
                                                                                                                                                      d ICP-AES (PerkinElmer Optima 7300DV)
                                                                                                                                                   and ICP AES (P ki El         O ti
                                                                                                                                                                                                                Pb       208 
                                                                                                                                                                                                                         208      Std    113       115       120       120       113
                                                                                   Dwell time:            50 milliseconds
                                                                                   Sweeps/reading:        20                                  Note: HNO3 and HF were Tamapure AA100 grade (Tama Chemicals,           Notes: Recoveries are given in %; values > 130% are all
                                                                                                                                                       City,         Japan).
                                                                                                                                              Kawasaki City Kanagawa Japan)
                                                                                   R di g / pli t
                                                                                   Readings/replicate:    1                                                                                                                                y              p
                                                                                                                                                                                                                            < 200% and may indicate sample contamination.
                                                                                   Replicates:            3                                                                                                                                mode,
                                                                                                                                                                                                                            Std = standard mode no NH3 gas
       CETAC Aridus II Desolvating Nebulizer System                                                                                                                                                                                d     i     ti      ll   d   ith
                                                                                                                                                                                                                            DRC = dynamic reaction cell mode with NH3 gas




                                                                                          Operating Conditions - II
                                                                                           p      g                                                   p      g
                                                                                                                                                     Operating Conditions - III                              Summary:
                                                                                                                                                                                                             S
                                                                                   Desolvating Nebulizer System: CETAC Aridus II             ICP MS:
                                                                                                                                             ICP-MS:                   PerkinElmer ELAN DRCII
                                                                                                                                                                                                             1.
                                                                                                                                                                                                             1 A desolvating nebulizer system with nitrogen gas addition can
                                        TM
                                 Aridus II Schematic                                                                                         ICP Power:                1600 W                                    i ifi
                                                                                                                                                                                                                significantly enhance analyte signal with reaction-cell based
                                                                                                                                                                                                                           tl    h       l t i     l ith      ti      ll b  d
                                                                                   Nebulizer Gas (from ICP-MS):    0 90 L/min (PFA-20)
                                                                                                                   0.90                      Plasma G
                                                                                                                                             Pl      Gas:              18 L/ i
                                                                                                                                                                          L/min                                 quadrupole ICP-MS, depending on solution uptake rate. A
                                                                                                                                                                                                                              ICP MS,
                                                                                                                              (Aspire-100)
                                                                                                                   0 90 L/ i ( pi 100)
                                                                                                                   0.90 L/min (A         )   Auxiliary Gas:            1.2
                                                                                                                                                                       1 2 L/min                                20 μL/min PFA nebulizer provided a factor of 2 to 3 fold signal
                                                                                                                                             Nebulizer Gas:            0.9 L/min                                                         μL/ i
                                                                                                                                                                                                                enhancement while a 100 μL/min PFA nebulizer provided a
                                                                                                                                                                                                                   h           t hil                     b li        id d
                                                                                                                                                                                                                6 to 7 fold improvement.
                                                                                   Spray Chamber Temp:             110 C
                                                                                                                   110°C                     Reaction G
                                                                                                                                             R    ti Gas:              NH3
                                                                                   Membrane O
                                                                                   M b            Temp:
                                                                                            Oven T p               160°C                     Desolvation System:                           w. PFA-20
                                                                                                                                                                           CETAC Aridus II w PFA 20          2. The 20 μL/min PFA nebulizer provided the best p
                                                                                                                                                                                                                       μ                     p                performance for
                                                                                                                                                                                                                                                           mg/L
                                                                                                                                                                                                                higher Si matrix concentrations up to 5000 mg/L, with lower Si
                                                                                                                                             Spray Chamber Temp:           110°C
                                                                                                                                                                           110 C                                                      ICP MS
                                                                                                                                                                                                                matrix loading to the ICP-MS and consistent overall analyte
                                                                                   Ar Sweep Gas Flow:                  (PFA-20)
                                                                                                             7.1 L/min (PFA 20)                         Oven Temp:
                                                                                                                                             Membrane O en Temp            110°C                                recoveries.
                                                                                                             6 5 L/min (Aspire-100)
                                                                                                             6.5       (Aspire 100)          Ar Sweep Gas Flow:            8.3
                                                                                                                                                                           8 3 L/min
                    CETAC Aridus II Schematic                                                                                                   Addition G
                                                                                                                                             N2 Addi i Gas:                     / i
                                                                                                                                                                           4 mL/min
                                                                                      Addition Gas:
                                                                                   N2 Additi G                  L/ i ( th b li
                                                                                                                      (b              )
                                                                                                             4 mL/min (both nebulizers)

								
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