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DETERMINATION OF Hf ISOTOPES IN ZIRCON BY MC FS ICP-MS A. Gerdes, A. Zeh, Yu.L. Ronkin........... .. , . . ............. U-Pb Pb-Pb ( , ) .. , .. , .. , .. , .. .......................................... 17O-18O .. , J. Surma, M. Staubwasser......... -- , .. , .. , .. , .. , .. , .. , .. ........................................ , .. , .. ....................................... Nd, Sr, Pb Mo- - ( ) .. , .. , .. , .. , .. , .. ................ .. , . , .. , .. . ():

- .. , .. , .. ........................................... .. , .. , .. , .. , .. , .. , .. ........................................... - .. , .. , .. , .. ........................................... , .. , .. , .. , .. ........................... .. , .. .............. .. , .. , .. , .. , .. .. .. , .. , .. , .. , .. , .. ................ (Q-) .. , .. Sephton and V.. Pearson............................................ . . , . , . ( . ) . . , .. , .. ............................... ɻ .. , .. .......... - () .. , .. ........................................ .. , .. ............................ - .. , .. ........................... .. , .. , .. , .. ........................................... CCO3 .. ...................... (16Ζ18, 234U238U, 235U238U) λ .. , .. , .. , .. ....................................... - .. , .. , .. , .. , .. , .. , .. , .. , .. ............................. .. , .. , .. , .. , .. .............. , , (- ) .. , .. , .. , .. , .. , .. , .. , .. , .. , .. .......................... - .. , . ................. ( ) .. , .. , .. .................... U-PB SM-ND .. , .. .................. Hf-Nd .. , .. , .. , .. , .. ........................... .. , .. , .. ......................................... .. , .. , .. , .. , .. -, .. c.................... 18 OPX-GRT-SILL-QTZ - ( ) .. , .. , .. ......................................... - - 1400-1500:

.. , .. , .. ............................ .. ........................................... .. , .. ............................... () .. , .. . , ʻ .. , .. , .. , .. .......................... 34S 33S SF .. , .. .......................... 18O D - .. , .. , .. , .. ................ - .. , .. , .. ............... - .. , .. ........................................ LA-ICPMS :

.. , .. , .

. ............................. Lu-Hf U-Pb - ( ) .. , .. , . . , .. , . . , . . , . . , . . , . . , . . , .. , . . , . . , .. .......................................... .. , .. , .. , ................................. . . , , , , , , , , ..................... 3e/4e .. , .. ............................................ - .. , .. , .. , .. .......................................... ( ) .. , .. , .. , .. ........ .. .............. 143Nd/144Nd .. ........... Rb-Sr Sm-Nd LL- .. , .. ......................................... , : .. ...................................... .. .......................... .. , .. , .. , .. ................ () , .. , .. ... - ( ) .. , .. ............ Sr-Nd ( ) .. , .. , .. , .. .............. .. , .. , .. , .. , .. , .. ......................................... Nd - : .. , .. , .. ......................................... Lu-Hf - .. , .. , .. ............... ( ) .. .......................................... SR - . . , .. .. (18O, DD) . . , . . ......... .. , .. , .. ............................. .. , .. , .. , .. .......................... Sm-Nd .. , .. , . .............. .. -, .. , .. , , .. ........................................ Rb-Sr - .. , .. , .. ........................................... - TTG ( ): . ......................................... Rb-Sr (1.23-1.20 .

) ( II) : .. , .. , .. ................ - .. , .. , .. , .. ,, .. , .. , .. .............................. , ( ) .. , .. , .. , .. , .. , .. , .. .................. ( ):

.. , .. , .. , .. , .. ... .. , .. , . , . M. , A.. , . . , . . , . A. M. M. ................ Sr 560-550 . . . , .. ...................................... .. , V. Mavromatis, O.S. Pokrovsky............ - .. , .. , .. .......................... - .. , .. , .. , .. , .. .......................................... - : ˨λ ?

.. , J. Horita.................................. :

, .., .., .. , .. , .. , .. ......................... HPHT Fe3C .. , .. , .. , .. ......................... .. , .. , .. , .. , .. .................... - - ( ) .. , .. , .. , .. , .. ........................................ - ( Sm-Nd .. .......................................... Hf .. , A. Gerdes, .. , S. Sindern................................. 2, .. , .. , .. , . , .. , .. .......................................... ¨ - (IRMS) .. , .. , .. ........................... .. ........................................... Sm-Nd ʻ

.., .. ............................ 18 - ( ) .. , .. , .. , M. Coble................................. ID TIMS ID MC ICP MS .. , .. , .. ......................................... . . ....................... ( - -7) .. , .. ........................ , ( ) .. , .. , .. ................. . .......................................... ( , , ) .. , .. , .. , .. , .. ............ : - .. , .. , .. , .................. ( ) . . , . . , . . ......................................... ( ) . . , . . ......................................... Nd, Pb, Sr . . , . . ................. .. , .. ............................. - . , .. , .. , .. , .. ............... ( - 1 ) .. ............................................. Pb-Pb- Au ( , - , ) .. , .. , .. , .. .. ( , ) .. , .. ........................................ .. , .. , .. , .. ....................................... .. , .. , .. ........................ .. , .. , .. , .. , .. , .. ............................. .. , .. ............................................ .. , .. , .. , .. , .. , .. ............................ DETERMINATION OF Hf ISOTOPES IN ZIRCON BY MC FS ICP-MS A. Gerdes1, A. Zeh2, Yu.L. Ronkin Institut fr Geowissenschaften, Mineralogie, Frankfurt am Main, Germany, (axel.gerdes@em.uni-frankfurt.de) Mineralogisches Institut, Am Hubland, Wrzburg, Germany Institute Geology and Geochemistry of the Urals brunch of the Russian Academy Sciences, Russia As is known the Hf isotopic composition of zircon can be utilized as a geochemical tracer of a host rocks origin in exactly the same way whole-rock Nd isotopes are used (Zircon, 2003). But the Hf is in fact a more sensitive tracer than Nd, as Lu/Hf in the depleted mantle has increased at approximately double the rate of Sm/Nd with respect to unfractionated material. Furthermore, the well-known resilience of zircon to surficial weathering, transportation, and sedimentation processes means that the same isotopic tracing techniques can be applied to elucidate the origins of detrital zircon grains in sedimentary and meta-sedimentary rocks (Zircon, 2003). The earliest Hf isotopic studies of zircon were undertaken by conventional thermal ionization mass spectrometry of microgram quantities of purified Lu and Hf extracted from acid-digested samples via a series of cation-exchange columns. However, the poor ionization efficiency of Hf by thermal ionization requires a significant amount of zircon. Using multi collector (MC) sector field (SF) ICP-MS is much more efficient, and the emergence of laser ablation provides the ability to measure the isotopic composition of Hf in zircon.

In this work Hf isotope measurements were performed by Thermo Scientific Neptune MC SF ICP-MS at JWG coupled to the New Wave Research UP-213 laser system with a teardrop-shaped, low volume laser cell. The MC FS ICP-MS was equipped with 9 Faraday detectors and amplifiers with 1011 resistors. Data were collected in static mode (172Yb, 173Yb, 175Lu, 176Hf-Yb-Lu, 177Hf, 178Hf, 179Hf, 180Hf) during 58 s of laser ablation. The Lu-Hf laser spot was 40 m diameter. Nitrogen (~0.005 l/min) was introduced via a Cetac Aridus into the Ar sample carrier gas to enhance sensitivity (~10-20%) and to reduce oxide formation. The use of the Aridus system allowed bracketing of laser ablation analyses with solution mode analyses. Analytical protocols were the same for laser ablation and solution mode analyses. Solution mode data were acquired with 60 integration cycles over a period of min, followed by 8 min of washout with a mixture of 2% HNO3-0.5 N HF. Data were corrected and normalized following the procedure of the laser ablation analyses. The isotopes 172Yb, 173Yb and 175Lu were simultaneously monitored during each analysis step to allow for correction of isobaric interferences of Lu and Yb isotopes on mass 176.

The 176Lu and 176Yb were calculated using 176Lu/175Lu of 0.02658 and Yb/173Yb of 0.795015 (both JWG in-house values). The latter is identical to the mean of the values given by Chu et al. (2002) and Segal et al. (2003). The correction for instrumental mass bias used an exponential law and a 179Hf/177Hf value of 0.7325 (Patchett et al., 1981) for correction of Hf isotopic ratios. The mass bias of Yb isotopes generally differs from that of the Hf isotopes with a typical offset of Hf/Yb of around 1.04 to 1.08 when using 172Yb/173Yb of 1. (mean of Chu et al., 2002 and Segal et al., 2003). This offset is determined for each analytical session by averaging the Hf/Yb of multiple analyses of JMC 475 solution doped with variable Yb amounts and all laser ablation analyses of zircon with a 173Yb signal strength of 50 mV. The mass bias behavior of Lu was assumed to follow that of Yb. For analyses with a 173Yb signal of 130 mV the Hf/Yb offset factor was calculated using the mean Yb of the individual analysis.

For analyses with a 173Yb signal of 130 mV the Yb and Lu isotopic ratios were corrected using the respective of the individual integration steps (n = 55) divided by the average / Yb offset factor of the complete analytical session. It has been noted before that the Yb interference correction is crucial for precise and accurate 176Hf/177Hf obtained by laser ablation analysis (e.g., Woodhead et al., 2004;

Kemp et al., 2006). A range of Yb isotope ratios are reported in the literature (e.g., Chu et al., 2002;

Segal et al., 2003;

Vervoort et al., 2004;

Amelin and Davis, 2005). At moderate Yb/Hf ratios of 0.06 these different Yb isotope compositions propagate into shifts in 176Hf/177Hf similar to the analytical uncertainty (Kemp et al., 2009). However, for higher Yb/Hf the different compositions can result in considerable over- or undercorrection (Kemp et al., 2009). The most appropriate composition for interference correction might vary for different instrumentations. At JWG an Yb composition similar to the mean of Chu et al. (2002) and Segal et al. (2003) has yielded the most consistent 176Hf/177Hf ratios for a range of variably doped JMC 475 solutions. Recent studies have shown that the within-run precision of 176Hf/ 177Hf can be considerably improved (up to 2-3 times) when the Hf mass bias (e.g., Slama et al., 2008) or the mean Yb mass bias of each analysis (Gerdes and Zeh, 2006;

Wu et al., 2006) is used for estimating the 176Yb/ 173Yb of each individual ratio. However, using the Hf mass bias can yield inaccurate results. For example at a Hf/Yb of 1.05 it causes an overcorrection of 0.80, 1.3 and 1.8 epsilon units for a 176Yb/177Hf of 0.02, 0.04 and 0.06, respectively. Also the use of the mean Yb mass bias can yield inaccurate results due to the difficulty in precisely determining the Yb mass bias for analysis with low Yb signals. In general analyses with Yb signal of 50 mV display a larger scatter in Hf/Yb compared to data obtained with higher signal strengths. This can result in a difference of up to 2 epsilon units compared to the data corrected by means of a uniform daily Hf/Yb offset factor. The use of this offset factor also improves the external reproducibility by about 40-70%. The external reproducibility (2 SD;

n50) over more than 6 months of analysis of reference zircon 91500, GJ-1, and Plesovice (176Hf/ 177Hf= 0.282298 0.000026, 0.282003 0.000018 and 0.282482 0.000015, respectively) at JWG is about 0.005-0.009% ( 1 epsilon unit). The same holds true for zircon of unknown samples (e.g., sample Berdyaush, see this issue) that have larger variation of 176Yb/177Hf compared to the reference zircons. Multiple analyses of Lu- and Yb-doped JMC solutions show that results with a similar precision and accuracy can be achieved also if Yb/Hf and Lu/Hf is 5-10 times higher than in most magmatic zircons. Note that any under- or overcorrection for Yb and Lu interference on mass 176 would result in a correlation of the Hf/177Hf and 176Yb/177Hf ratios. All data were adjusted relative to a JMC 475 176Hf/177Hf ratio of 0.282160 and quoted uncertainties are quadratic additions of the within-run precision and the reproducibility of the 40-ppb JMC 475 solution (2SD = 0.003%, n =10 per day). These uncertainties are similar or slightly worse than the daily values and also the long-term reproducibility of the reference zircons GJ-1 and Plesovice (Gerdes & Zeh, 2009).

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