电子自旋共振（ESR）测年方法在我国早更新世考古遗址年代学研究中的应用探索
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摘要
对于东亚地区早更新世考古遗址的研究可以帮助我们理解人类最早何时走出非洲以及他们是如何在亚洲大陆生存与演化等一系列问题。一些在我国境内发现的最早期的人类活动证据目前并没有被国际学术界普遍接受，在很大程度上归因于这些早期遗址年代的不确定。由于测年时段和测年对象的限制，这些早更新世遗址中的大多数无法采用诸如钾氩/氩氩测年法等经典的同位素测年方法进行年代学研究。电子自旋共振（ESR）方法是一种常用的早期遗址考古测年方法，其中ESR骨化石测年可以应用于早更新世遗址的年代学研究。由于骨化石的体系不封闭，所以在计算ESR年代时需要考虑铀在化石样品中的加入过程。传统ESR化石测年中通常采用两种人为假定的铀加入模式：早期铀加入模式（EU模式）和线性铀加入模式（LU模式）来分别计算样品年龄，并认为样品的实际年龄介于EU与LU模式年龄之间。但在实际研究中采用上面两种模式计算得到的样品年龄往往相差较大，另外一些研究表明化石样品还存在铀的近期加入现象，所以传统ESR化石测年给出的年龄结果往往存在较大的不确定性。
本论文采用ESR与铀系分析相结合的测年方法（US-ESR测年法）对我国两处早更新世古人类活动遗址–重庆巫山龙骨坡遗址和河北阳原泥河湾盆地东谷坨遗址展开了年代学研究工作。该方法通过对动物牙齿化石中不同牙组织的铀系同位素分析来重建铀在化石样品中的加入过程，并通过计算铀吸收参数p加以定量描述。与传统的ESR化石测年方法相比，由于其避免了采用不同铀加入模式所引入的人为因素，所以得到的化石年龄结果具有更高的可信度。由于该测年手段涉及ESR和铀系测年两种不同的年代学方法，测年机理和实验分析过程都较为复杂，且在年代测定过程中需要对近30个计算参数进行逐一探讨和分析，所以该方法在我国旧石器考古遗址尤其是早更新世考古遗址的年代学研究方面尚鲜有应用。
论文研究的龙骨坡和东谷坨遗址分别是我国南方和北方两处具有代表性的早期人类活动遗址，都曾采用传统的ESR化石测年方法进行过年代学研究。其中龙骨坡遗址历史上曾经是一个洞穴，上世纪80年代的早期发掘中曾出土两块疑似古人类化石、石制品和大量动物化石。在2003-2006年的中法联合考古发掘中又出土了大量的石器，并对遗址的地层进行了更为详细的描述。
本论文研究的17颗哺乳动物牙齿化石样品均采集自这次联合发掘。分析研究显示除遗址南壁两个样品中有铀的早期加入外（-0.7
本论文采用ESR与铀系分析相结合的测年方法（US-ESR测年法）对我国两处早更新世古人类活动遗址–重庆巫山龙骨坡遗址和河北阳原泥河湾盆地东谷坨遗址展开了年代学研究工作。该方法通过对动物牙齿化石中不同牙组织的铀系同位素分析来重建铀在化石样品中的加入过程，并通过计算铀吸收参数p加以定量描述。与传统的ESR化石测年方法相比，由于其避免了采用不同铀加入模式所引入的人为因素，所以得到的化石年龄结果具有更高的可信度。由于该测年手段涉及ESR和铀系测年两种不同的年代学方法，测年机理和实验分析过程都较为复杂，且在年代测定过程中需要对近30个计算参数进行逐一探讨和分析，所以该方法在我国旧石器考古遗址尤其是早更新世考古遗址的年代学研究方面尚鲜有应用。
论文研究的龙骨坡和东谷坨遗址分别是我国南方和北方两处具有代表性的早期人类活动遗址，都曾采用传统的ESR化石测年方法进行过年代学研究。其中龙骨坡遗址历史上曾经是一个洞穴，上世纪80年代的早期发掘中曾出土两块疑似古人类化石、石制品和大量动物化石。在2003-2006年的中法联合考古发掘中又出土了大量的石器，并对遗址的地层进行了更为详细的描述。
本论文研究的17颗哺乳动物牙齿化石样品均采集自这次联合发掘。分析研究显示除遗址南壁两个样品中有铀的早期加入外（-0.7
本论文研究的另一处地点东谷坨旧石器遗址属于旷野遗址，发现于上世纪80年代初。后续发掘中出土了大量具有独特加工技术特征的石制品。论文测年研究分析的3颗化石样品来自遗址的早期发掘。对样品的铀系分析显示全部样品的牙组织铀系同位素比均超出了平衡值1，表明样品中存在铀的后期析出。由于无法通过单一的铀吸收参数定量重建样品中铀的加入过程，所以未能得到东谷坨遗址化石样品的US-ESR年龄。同时，采用传统ESR化石测年中的EU与LU模式计算得到的样品年龄也比遗址的古地磁参考年龄明显偏年轻。本论文研究表明东谷坨遗址的化石样品可能经历了反复加入与析出的复杂铀迁移过程。测年研究同时也反映了US-ESR测年法在早期考古遗址化石测年中存在的局限性。
本论文同时还对US-ESR测年法中的一些基础问题进行了研究：
（1）古剂量的测定:
本论文通过对三种不同的古剂量拟合函数（单饱和指数（SSE）函数、指数加线性（EPL）函数和双饱和指数（DSE）函数）的对比研究发现，采用DSE函数对实验剂量点拟合的偏差系统性的小于SSE函数拟合，同时采用DSE函数拟合外推得到的计算结果与已知参考剂量值的偏差均小于另外两种拟合函数。进一步研究显示DSE函数在不同剂量范围内的拟合结果基本一致，而SSE函数的拟合结果会随最大辐照剂量值的减小而明显减小。本论文研究表明目前ESR化石测年中普遍使用的SSE函数并不适合早更新世化石样品的古剂量拟合，而采用DSE函数对这类样品可能更为合理。
（2）样品外部γ剂量率的影响:
外部γ剂量率是本论文研究中龙骨坡遗址年代测定的一个难点。研究表明龙骨坡化石样品的外部γ剂量率在总剂量率所占比例超过了50%。由于龙骨坡遗址地层堆积环境中存在大量砾石、粘土和铀含量较高的动物骨化石碎片，成分极不均一，从而在样品周围形成一个不均匀的γ辐射场。而沉积物中γ射线的辐射半径约为30cm，所以野外实测的样品外部γ剂量率可能会与实验室分析结果存在差异。研究显示龙骨坡南壁附近化石样品的外部γ剂量率实验室分析数据平均高出野外实测数据约140%，由于实验室分析的仅是样品周边小范围内采集的沉积物，并不一定具有代表性，若采用实验室分析的数据进行计算会造成对样品年龄的严重低估。所以对遗址野外γ剂量率详尽而准确的测量是计算龙骨坡化石样品年代的关键之一。
（3）化石样品内部剂量率的重建:
采用ESR/铀系联合分析的方法进行化石测年需要通过计算铀吸收参数（p值）来还原样品中铀的加入历史。本论文研究显示东谷坨遗址的化石样品中存在铀的后期析出，而目前单一铀吸收参数的数学模式尚无法重建这类化石样品的内部剂量率，进而计算样品年龄。采用传统的EU与LU模式计算的ESR年龄明显小于遗址参考年龄也说明了东谷坨遗址化石样品经历了复杂的铀迁移过程，这很可能是与旷野遗址所经历的复杂地球化学变化有关。东谷坨遗址以及泥河湾盆地中其他早期遗址大都是由于近期侵蚀作用暴露于地表后被发现，遗址的水动力环境会随着侵蚀作用不断发生改变，进而引起铀活化作用的更新。对于经历了铀析出以及复杂铀迁移历史的化石样品的年龄测定还需要进一步研究。
本论文研究表明US-ESR测年法可以用于我国早更新世考古遗址的化石测年且与传统ESR化石测年相比具有明显优势。随着对该方法的进一步研究和完善，将为研究我国早期人类生存与演化的历史提供一种更可靠的年代学手段。
The study of Early Pleistocene archaeological sites in East Asia can help to solvethe questions of when hominins first left Africa and how they might have settled inAsia. Some earliest hominin evidence in China were not widely accepted mainly dueto chronological uncertainty, since most of them are beyond the classic radioisotopicdating range and lack of volcanic materials for K-Ar and Ar-Ar dating. CombinedESR/U-series dating could solve this problem, as its application to fossil tooth has apotential of dating the archeological sites older than1Ma, depending however on theaccuracy of reconstructing uranium uptake history. An U-diffusion parameter pshould be defined for each dental tissue and the obtained US-ESR model age is lessuncertain than the conventional EU (early uptake) and LU (linear uptake) ESR modelages.
In this work, combined ESR and U-series dating method of fossil tooth has beenused to date two Early Pleistocene sites of China, Longgupo, Chongqing, SouthwestChina and Donggutuo, Hebei, North China. These two sites may represent the earliesthuman settlement in each region of China. The Longgupo site, once a cave, has acomplex deposition environment which makes the previous dating work problematic.The purpose of this thesis includes establishing a precise chronological framework ofthe stratigraphic sequence of Longgupo which based on the recent joint Chinese-French excavation in2003-2006. For the Donggutuo site, the dating work of thisthesis was expected to be checked by the well-established paleomagnetic date in orderto evaluate the dating method used in this study.
This thesis presents the feasibility of applying combined ESR/U-series method ondating Chinese early Pleistocene sites, and the result of this study places thechronology of the Longgupo site between1.4and1.8Ma. With respect to thetechniques development of the stone artifacts unearthed from the site, Longgupo isstill one of the earliest evidence of human settlement in southern China.
This study shows that this combined method provides the availability of dating theold archaeological sites, but some challenges are also brought forward and addressed:
(1) Paleodose determination
The paleodose reconstruction is the main problem not only for tooth dating but alsofor quartz minerals studied by the ESR method. In combined ESR/U-series dating, theuncertainty on DEis the main error source of the final result. The determination of DEof the samples from old sites is more difficult because of the high dose valueaccumulated during the history. As regeneration protocol used in luminescence studiescannot be applied on tooth enamel without the destruction of the ESR traps, theextrapolated additive dose method is used for DEdetermination, and the dose responsecurve is simulated with certain fitting functions. Which function is morerepresentative and close to the true value of paleodose of the sample, especially forthe old tooth samples were studied in this thesis.
Three different fitting functions were investigated: single saturation exponential(SSE), exponential plus linear (EPL) and double saturation exponential (DSE), inorder to find the better solution for DEdetermination of old tooth samples. This studyshow that conventional SSE function is unambiguous not suitable for fitting doseresponse curves of old tooth samples from Longgupo and Donggutuo sites and itsfitting curve shows a large deviation with analytical points and higher fitting errorsthan the other two functions. EPL and DSE fittings are the extensions of SSE, ofwhich both have their own possible physical meanings, and have been appliedpreviously to some other dating materials. EPL function was used to provide higherDEvalues than DSE one, but the results are in general close to each other in the errorrange. The DSE function gives the lowest DEamong the three fitting but relative largeerrors because more fitting parameters were introduced in this function. The adjustedcoefficient of determination (adjusted R2) which indicates the fitting effect shows thatthe DSE function fit best to the experimental dose points. According to the work ofthis thesis, it could conclude that the conventional paleodose fitting method (SSE) isnot applicable to date the old tooth. Double saturation exponential function is more acceptable and exponential plus linear one is sometimes a compromise solution in thecase that the number of aliquots is not enough to reduce the uncertainty of DES.
(2) External gamma dose rate
The importance of external gamma dose rate was addressed in this study, especiallyfor the Longgupo site. This issue is quite essential to ESR and TL dating studies ofarchaeological sites, which are often enriched with fossils and stone artifacts andcorrespond then to typical “lumpy” site. The external gamma dose rate measuredtoday has always a discrepancy with the past value because of the complex variationsof sedimentological history and hydrological environment changes.
In some cases, when the sample layer is full of bone fragments, the external doserate is variable because the surrounding bones would absorb uranium from theenvironment. In this study, the external dose rate contributes greatly to the total doserate of Longgupo tooth samples (more than50%in general) and the measuredexternal dose rate values have a big influence on the age calculation. Unfortunately,the in situ gamma dose rate was not available for some of the studied samples leadingto an inverse correlation of the calculated ages with the stratigraphic sequence and toa discrepancy with biostratigraphy evidence. In view of the above-mentioned facts, Iwent to Longgupo again in October,2011in order to make a more precisemeasurement of the external dose rate on the field. Although this work is moredifficult nowadays after five years of previous excavation when the samples werecollected, it is necessary not only for the dating study but also may have animplication of the depositional environment changes of the site.
(3) Uranium uptake history
The uranium uptake history in the tooth is the key issue for the determination of thedose rate. The advantage of combined ESR/U-series dating is to reconstruct it by theuse of a diffusion parameter rather than by artificial assumptions. In the present workthe uranium uptake was not the main problem for Longgupo samples because the dominant contribution of the external dose rate was related with the recent uptakehistory. In contrary, uranium uptake and/or leaching have a key effect on the agecalculation of Donggutuo samples. This is partly due to the high uranium content ofthe samples and to the high isotopic230Th/234U ratios.
The two old sites studied here correspond to two types of sites: a cave site(Longgupo) and an open site (Donggutuo). The difference of uranium uptake historybetween these two sites can probably be explained by the different depositionalhistories. Longtupo was systematically excavated after its discovery and, although thestratigraphy of the site is complicated, the sedimentary stack was not disturbed a lotbecause of the protection of the carpeted breccias on the slope. In contrast, theDonggutuo site and a couple of other localities in the Nihewan basin were exposed inthe open air by recent erosion. With a changing erosion system, there is also a changein the hydrological environment and the erosion process is commonly accompaniedby drainage re-activation and lowering of the ground water table. This goes alongwith renewed uranium mobilization. Uranium leaching always makes a difficulty foruranium reconstruction. For the moment, there is no better solution for dating thefossil tooth with uranium leaching, and a practical solution is to check systematical U-series mapping to identify the most promising domains for combined ESR/U-seriesdating.
Dating Early Pleistocene sites is always a challenge, the combined ESR/U-seriesdating method provides a possibility and it has the best potential for dating old fossilsamples from old sites. For the estimation of a reliable dating result, a number ofquestions have to be addressed other than the issues mentioned above, such as theestimation of large dose values and the difference between natural and laboratoryirradiation. The environmental dose rate is always a problem for dating “lumpy” sites,and it should be measured in situ when such measurements are possible. This studymay provide a choice of dating the old sites in China. In combination with otherdating methods, such as the paleomagnetism or cosmogenic nuclides method, thecombined ESR/U-series fossil dating technique will help to create a more precisechronological framework of ancient human settlement in China.
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