Archaeomagnetic researches and dating of burnt products from clay by the rehydroxylation method

Konstantin S.Burakov, Inga E.Nachasova Schmidts Institute of Physics of the Earth of the Russian Academy of Sciences, 123995, B. Gruzinskaya, 10, IFZ, Moscow, Russian Federation
ABSTRACT

Dating of products from the burnt clay by rehydroxylation method and archaeomagnetic researches of the burnt material from clay from three regions is spent: Great Britain, Spain and Black Sea Coast for the purpose of specification of dating of materials of the archaeological monuments used for carrying out of archaeomagnetic researches for data acquisition about elements of a geomagnetic field in last millenia. Carrying out archaeomagnetic researches has allowed to find out sources of a deviation of received datings from true values at work as a method rehydroxylation. These are aeration processes (transformation of magnetite in hydrooxides) or secondary magnetisation (for example, magnetisation at a fire). Ways of correction for reception of the datings close to true values are offered. The data about intensity of the geomagnetic field, received on magnetisation of investigated material, can be used as independent certificates in favour of correctness of the received dating. Application of rehydroxylation method opens data acquisition possibility about temperature around archaeological monuments in the last centuries in case of carrying out of researches of confidently dated burnt objects from clay; the already object dating, the is more exact temperature determination. Keywords: Archaeomagnetism, rehydroxylation dating, archaeointensity, ancient climatic temperatures 1. Introduction Paleo - and archaeomagnetic researches give the chance to obtain the data about an ancient magnetic field of the Earth. One of its main things are variations. In time and space, it is possible to receive the most detailed information on change of elements of a geomagnetic field as a result of carrying out the archaeomagnetic researches which object is magnetisation of the burnt materials of the archaeological monuments having ferromagnetic fraction. The method of definition of parameters of an ancient geomagnetic field on thermomagnetisation of the burnt material, developed in the middle of last century . and O.Thellier (Thellier, Thellier, 1959) has allowed to obtain the data about a terrestrial magnetic field of time of roasting with good approach to true values. Review the accuracy of the identification, assessment of possible biases and how their accounting was the subject of a number of studies (Coe, 1967; Coe, Gromme, 1973; Levi, 1975; Carmichael, 1977; Rogers et al., 1979; Aitken et al., 1981, 1986; Kono M. and Tanaka H., 1984; Genevey, Gallet, 2002; et all). To obtain the definitions of elements of the geomagnetic field with the smallest deviation from the true values of the authors developed a method of correction for magnetic anisotropy and the chemical changes occurring during laboratory heating at work using the Thellier method (Burakov, 1981; Burakov, Nachasova, 1985; Burakov, et al., 2005; Nachasova, Burakov, 2009). It is shown that one of the factors complicating and in some cases making it impossible to determine the tension of the ancient geomagnetic field on the remanent magnetization of the material is a chemical weathering which carry information about the magnetic field of the magnetite particles, in which they are covered with a film of iron hydroxide, identifies signs of weathering of magnetite and the degree of weathering of the magnetic fraction in the

ceramic archaeological sites to account for confounding factors when determining the ancient geomagnetic field (Nachasova, Burakov, 2009). The most widely burnt archaeological material is ceramic. Investigation of magnetization provides data on the strength of the ancient geomagnetic field in different parts of the globe over several millennia. Authors obtained data on changes in the geomagnetic field over the past several thousand years for the areas of the Iberian Peninsula, the Caucasus, Eastern Mediterranean and Black Sea, Central Asia and Siberia (Nachasova et al., 2002, 2007; Nachasova, Burakov, 2008; Nachasova et al., 2007). Established that there are variations of the geomagnetic field of varying duration from decades to millennia. To study the temporal and spatial variability characteristics of geomagnetic field variations must be as accurate as possible picture of the changes in the field. One of the defining moments of the sharpness of the picture changes of the geomagnetic field along with the accuracy of obtaining data on the field strength is the accuracy and reliability of the data binding to the timeline. There are various kinds of errors in the implementation of the interim data binding of the geomagnetic field. The dating of the material, the magnetization is investigated, conducted by archaeologists - the researchers of the monument on the basis of a number of different types of research. Most-date development stages of the monument, the accumulation of cultural backgrounds, stages of construction. Possible errors due to the fact that for the construction of buildings could be used material from earlier buildings, and for the restoration of the buildings could receive material of a later time. The last time the firing of the material may vary from time to time create archaeological sites from which these materials are selected. In the event that archaeological site was subjected to fire, the residual magnetization of the material from this object will contain information about the magnetic field, which is precisely the time the last fire. To obtain independent criteria correctly timing study burned archaeological materials can be used archaeomagnetic results of research. The authors used for this purpose a comparison of data on the geomagnetic field derived from studies with data obtained by the material from this area with reliable accurate dating. The authors also proposed a method of dating archaeological ceramic material on the porosity of the material, successfully used in the study of ceramic multilayer archeological monuments of Spain: Cendres Cave, La Motilla del Azuer, El Molon (Nachasova et al., 2002, 2007; Burakov et al, 2005). Importance of obtaining the most accurate dating of archaeological materials for the development of studies of the history of human cultures, and studies Earths magnetic field, i.e. the processes in the Earths core, defines a great interest in various dating methods, integrated application that allows you to significantly increase the reliability of obtained datings. 2. The method of rehydroxylation In the School of Engineering Aerospace and Civil Mechanics Manchester team of researchers led by M. Wilson (Wilson et al., 2009) developed a method for dating of burnt materials of archaeological sites using the rehydroxylation, which allows timing the moment of firing of the material. The physical basis of the method is the fact that crystals of clay minerals such as montmorillonite, kaolinite, illite clay during firing at temperatures of 450-900C are losing their constituent water molecules. After cooling water from the environment through the capillaries in the clay gets to dehydrated minerals and connects with them. The rate of accumulation of such water does not depend on the ambient humidity, but depends on the temperature, the mass of the associated water depends on the time to degree 1/4. Accumulated over time, water is easily removed when re-heated to a temperature of 450550C.

Thus, the method rehydroxylation based on the properties of the ceramic reacts with atmospheric moisture after baking. As a result of this reaction, the weight of ceramics increased slowly during its existence. To determine the age of ceramics to determine the weight of accumulated moisture and its rate of accumulation must be known to the average temperature during the existence of pottery. The authors conducted a comprehensive study (method rehydroxylation dating and arhaeomagnetic research) baked clay products from three regions: the UK (London), Spain (Mlaga and Granada) and the Black Sea (Kerch, Taman). Fragments of ancient bricks from London (1b - 4b) were kindly provided by M. Wilson. To carry out the dating by the rehydroxylation we used fragments products weighing from 3 to 30 grams. Procedure for laboratory studies same as described in (Wilson et al., 2009), but has a number of features associated with the type of equipment used and method of measurement. In the first stage, we measured the weight P(t) samples at room temperature T = 25 2C and the natural humidity RW (t) (Fig. 1). To measure the weight scales used Adventurer AR1530 sensitivity of 1 mg, the humidity was measured with the hair hygrometer. Weight change of samples due to the change in mass of the capillary water in the ceramic, its amount in the sample is reversible depends on the humidity. According to the measurements we find the dependence of the weight of images from moisture dP/dRW, which is later used to amend the humidity in the measurement of the weight of the samples. At the second stage of capillary water is removed from the samples by keeping them at 105C for 12 hours. As a result, the weight of sample P(105C) without water, not related chemically to the substance of the sample. Note that the weight of the sample without the capillary water Pextr can also calculate by extrapolation of direct P(RW) to RW = 0. In the third stage the samples were heated to 500C and maintained at this temperature for 4 hours, then cooled with furnace to 120C. At this temperature, the samples were placed in an airtight container, and after the samples were cooled to room temperature, measured by the weight of P(500) and began the countdown. At a temperature of 500C is removed chemically bound water, and its mass in the sample is defined as Pm = P(105)-P(500). The fourth stage - the longest of the order of several months. During this time the samples were stored in a container, the thermostat inside which the temperature was maintained at 25 0.2C and the humidity was maintained within 63-72% and was measured with an accuracy of 0.3%. In the fourth stage is an increase in sample mass as a result of leakage of the two processes. First, the capillaries are filled with water. Depending on the size of the sample time required to reach the equilibrium content of capillary water and humidity is required from one to several days. As shown in (Tosheva et al., 2010), this time also depends on the firing temperature of ceramics. During this time, been a rapid increase in the mass of the sample 2a. The second process - the actual chemical hydration begins immediately after the occurrence of water in the capillaries. Calculations needed for the dating of samples were carried out by us in accordance with (1), (2). The process of increasing the weight of the sample over time, depending on the linear part P(t) (t>7 days) can be described by the formula:

P(t)=P0+k t 0.25 ,

(1)

where P0 represents the sum of weight of sample P (500) plus weight of the capillary water which have reached saturation at set humidity, - a kinetic constant, k factor at 25. If for temperature 25 to accept 25=1, for other temperatures it can be calculated according to the data received in (Wilson et al., 2009), under the formula:

ln(/25 )=18.5716-5537.3/Tk ,

(2)

where 25 a kinetic constant at temperature 25, size of a constant for temperature of endurance of sample Tk in Calvin's degrees. In this formula temperature Tk is, generally speaking, the unknown person, and it changes during existence of the ceramic sample, that, certainly, affects accuracy of dating.. Application of a method of rehydroxylation has allowed to reveal a material of archaeological monuments which time of roasting essentially differs from time of creation of a monument, to specify dating an investigated material. So results of dating of fragments of bricks (3s, 6s, 7s), selected in territory of a fortress of VIIIth century Castillo de Gibralfaro in Malaga (Spain), have shown, that all bricks are restoration, and concern to XVIIIth-th centuries AD. In the Table results of the researches lead on samples from burnt materials of archaeological monuments of England, Spain and Black Sea Coast are resulted. Research of the sample 121 (a fragment of a brick) from Granada has allowed to specify its dating. Archaeological dating - 1600100 AD, the dating received by means of rehydroxylation method - 153535 AD. However in some cases at work by a method rehydroxylation there are complexities. Some divergence of result of dating by a method rehydroxylation and archaeological dating has turned out at research of the sample 1b from London. Archaeological dating I th century AD, received by means of rehydroxylation method 385 BC. As a result of research of the sample 3b from London which is not having archeological dating, date of its manufacture 11000 BC has turned out., which is unreal, since the sample is a fragment of a brick. Similar unreal datings have been received and for other samples. Attraction of results archaeomagnetic researches has allowed to make a number of the conclusions concerning these cases. 3. Archaeomagnetic researches For carrying out archaeomagnetic researches specimens with the basis 10x10 mm and height 510 mm have been cut, how much it thickness of ceramics allowed. Determination of intensity of an ancient geomagnetic field was spent by means of modified Thellier method of double heatings with introduction of correction on magnetic anisotropy of samples and chemical changes of magnetic fraction during heatings (Burakov et al., 2005). A study was conducted of the magnetic properties of the samples. It turned out that the sample 3b (from London) is very different magnetic properties from other English samples. The magnetic properties of the sample showed that it is strongly magnetic, its magnetic susceptibility is 0.015 units SI, i.e. bricks made of clay containing a large (up to 10%) of magnetite. Weathering of magnetite, i.e., fraction of magnetite in this sample is transformed into hydroxides Wa = 20.3%, while in other British samples, an order of magnitude less magnetic, weathering does not exceed 5%. When the sample is heated, these hydroxides are transformed into magnetite with the release of water. The calculation shows that the mass of the released water is up to 40 mg. Thus, if we assume that the 65 mg released from the sample when heated to 500C water of 40 mg are hydroxides, then the share of the actual clay fraction is 25 mg. Then, taking Tk equal to 11C, according to the adopted in (Wilson et al., 2009) for London, we obtain for him the production date in 1725 AD. To determine the error of this dating is difficult, we can assume that the time of manufacture of the bricks - XVIIth-XVIIIth centuries AD. Similar magnetic characteristics inherent in the pattern of 1s Castillo de Gibralfaro (Malaga, Spain). He also strongly magnetic and the odds of weathering, i.e, proportion of magnetite, turned it into hydroxides, is about 25%. If we assume that half of the emitted when heated to 500C the amount of water is associated with iron hydroxides (like the 3b), we find that his date of manufacture is 1935 AD, i.e. you can assign it to the nineteenth and twentieth centuries. Thus, the magnetic properties of baked material reveals one of the reasons for obtaining false dating at work by rehydroxylation, the introduction of the correction of an estimate of the time interval to which the firing of the material, which may also be of interest in the case of the need

to identify the material, the production time is differs greatly from the establishment of an archaeological monument. Research of magnetization of samples has shown, that almost all the investigated samples have unicomponent magnetization which has been created during their roasting, and were not exposed to secondary heatings to heats. Exception is only the sample 1b from London, dated as Ith century AD. Dating of this sample by a method rehydroxylation gives date - 385 BC. Research of magnetization of this sample has shown, that secondary heating takes place. On the diagramme of Arai-Nagata it is visible that there are two magnetisations (fig. 3), and secondary magnetisation has a direction, the return primary (fig. 3b). Apparently, at packing in a building the brick has been turned concerning that position which it had at roasting. Its magnetisation has appeared directed back to a magnetic field. Then the building has undergone to a fire in which the brick has heated up to order temperature 330, and in it was created secondary partial magnetisation in a direction of an operating magnetic field. Having heated up to such temperature leads to disappearance of the most part of the saved up moisture. Modelling of the processes occurring during secondary heating has been spent on the sample 610 of a monument of Hermonassa. Short-term heating to 330 has been carried out. During heating the sample has lost all capillary water and 90% of chemically connected water. In this case the dating error essentially increases, apparently, archaeological dating more close to true. The intensity of a geomagnetic field received on primary high-temperature magnetisation of the sample on a temperature interval 400-560 - 66.52.2 mkT, on secondary magnetisation of time of a fire - 60.95.2 mkT. The divergence of values of intensity is insignificant, most likely both primary and secondary roastings concern I century AD. Use of the data about intensity of a geomagnetic field at the moment of roasting of an investigated material has shown that received on samples from monument Castillo de Gibralfaro (Malaga) the data about intensity of a field is close to the data received on direct supervision for time of manufacturing of samples, defined by means of dating by a method rehydroxylation (Table). Dating of the sample 1s has been received taking into account influence of process of aeration (date is shown in brackets). On fig. 4 definitions of intensity of the ancient geomagnetic field, received on magnetisation of bricks from London, and also definitions of intensity of a field known at present for England (Barraclough et al., 2000; Casas et al., 2005). . The magnetization of the sample 2b, dated archaeologically 1275 25AD, obtained a value 61.0 0.3 mkT, and the sample 4b, having a dating 1400 100AD, - 58.90.8 mkT. Investigation of changes in the geomagnetic field at the interval of the last two millennia in Eastern Europe, Bulgaria, Caucasus (Kovacheva, 1997; Nachasova, Burakov, 2009), Western Europe (Genevey et al., 2009) and Central Asia (Nachasova, Burakov, 1995) showed that in general terms the nature of the stress field is the same. Changing the field strength at this time interval has the form of a wave with a characteristic time of about six thousand years, to which imposes more short-period oscillations (Nachasova, Burakov, 2000). The minimum of this wave occur within the first century AD, the maximum - at the end of the first - the beginning of the second millennium AD. The magnetization of the sample 3b was obtained value of the geomagnetic field of 50.10.2 mkT. Based on the fact that this sample - a brick, we can assume that most likely it was made in the second millennium AD. The value of the resulting magnetic field practically coincides with that obtained in (Casas et al., 2005). You can take that and the time of manufacture of both the material at hand. Obtained for UK data broadly consistent with the pattern of changes in the geomagnetic field from other areas of Eurasia (Suttie et al., 2011). In the second millennium AD

there is a tendency to reduce the field strength and field strength in the early first millennium AD is not much different from the average level of the first half of the second millennium. For the dating method rehydroxylation need to know the temperature of the area of manufacturing calcined material. Direct measurements of temperature in the past began in the eighteenth century, so that in fact the temperature in the previous century is unknown, extrapolation of the known for the present data in antiquity can lead to deviations from the true values. When dating of samples from sites Pantikapeum (Kerch) 1063, Hermonassa (Taman) 610 and the Cartuja (Granada) 123 by using published data on the temperature in these regions (11.1C for the Kerch and Taman, and 15,5C for Granada) dates obtained by rehydroxylation sharply at odds with the archaeological (Table). The date obtained for sample 123 - 10000 years BC, it is unrealistic (sample - a fragment of brick). Geomagnetic field, obtained from samples from the Black Sea, 65.5 0.94 mkT - on sample 1063 and 94.50.4 mkT - on 610, does not contradict the pattern of change of the geomagnetic field over the past two millennia in the Caucasus. In the first centuries of the first millennium AD, the tension was about the same as in the tenth century - has increased significantly (Nachasova, Burakov, 2009). At the same time in the second millennium BC (the date obtained by the method rehydroxylation on the sample 610) of high field strength values do not. This can be considered as evidence in favor of the correctness of archaeological dating. Thus, it is possible that the source of errors in determining the dates of calcined material may be ignorance of the temperature in the firing of the material. 4. Determination of ancient climatic temperatures. Get information about the temperature in the archaeological site in the past century by using the application of the method rehydroxylation in the case studies confidently fired narrowly dated objects from clay. Figure 5 shows a curve showing the relationship of time and sintering temperature of ceramics according to the equations (1), (2) for sample 4b.This dependence makes it possible, knowing the date of manufacture, the object of investigation, to determine the temperature in the vicinity of the archaeological monument. Due to the nonlinearity of the growth of the accumulation of water in the sample (Fig. 2a), the main mass of water accumulated in the first stage after the firing of ceramics, and where the temperature is precisely for this stage, the duration of which is likely no more than a hundred years. In order to determine the temperature in the area of the archaeological monument Panticapeum (Kerch) studies were carried out by rehydroxylation fragment sintered clay coating of kiln (model number 1063), dating from the end of the IIth century AD. Obtained temperature 12.50.3C, close to the average temperature of the district, which according to the literature was 11.1C. Research conducted on another sample from this region, fragments of pottery (sample number 610) from a layer of cut archaeological site Hermonassa (Taman), dated archaeologically ~86060 year AD, gave temperature of 16.9 0.3 C. Does the resulting discrepancy between the actual temperature change in temperature is unknown. It is possible that we have studied the effect of the material conditions of existence for the first time after firing. Since ceramics first time since production could be used at elevated temperature (indoors). That might influence the second factor seems to indicate, and the difference in temperatures obtained by studying samples of a ceramic shop in Granada (Spain). Modeled on the clay (123) from the inner coating kiln, excavated in a ceramic shop, dated archaeologically 100 AD, was obtained by the temperature of 22.6C. Study of the fragment of ceramic vessel

(125), selected from the filling between the furnaces in the pottery workshop, gave the temperature of 24.7C. While its production is close to the late functioning workshop. According to archaeologists opinion vessel was made several years before the end of the workshop, i.e. date of its production ~ 90AD, it was soon broken, and a shard found in the earth backfilling between the furnaces. Determination of temperature on the samples from the Black Sea (1063 and 610) and Spain ( 123), conducted on the basis of archaeological dating of the samples (Table) gave a temperature different from the modern to the 17C. Moreover, the greater was the deviation in temperature, the greater the discrepancy in dating. By joining this series and samples 1b, 2b and 4b from London. Apparently, if the dating of ancient materials to more accurately know the temperature of the environment, the firing time of the material. Using the confidence and narrowly dated annealed material of archaeological sites using the rehydroxylation, you can get data on temperature, time of manufacture of this material and to construct the curves of temperature change over the last millennium in a certain area. Such studies are very relevant and promising. In conclusion, we note that in this study, we did not count on getting accurate data on the age of the samples. However, even with the precision instruments that we used, the application of the method of rehydroxylation eliminates errors in the dating of the materials used for arhaeomagnetic research. It is obvious that the use of more accurate instruments and, in particular - balances of a sensitivity of at least 10 micrograms, and will increase the accuracy of determining the age of the samples of baked clay. 6. Conclusions. Conducted a comprehensive study (dating products, in baked clay by rehydroxylation and arhaeomagnetic research) calcined material of clay (ceramics and bricks) from three regions:Britain, Spain and the Black Sea, has allowed: 1) to date material from the archaeological site of "Castillo de Hibralfaro" and to clarify the dating of material from the monument Alhambra (Spain); 2) get some data on changes in the geomagnetic field in London in the past two millennia 3) identify sources of deviations from the true values of the results obtained by the method of dating rehydroxylation, and suggest methods of correction for dating, close to the true values; 4) obtain information about the temperature in the past, conducting research method rehydroxylation on dated material that is of great importance, because knowledge of temperatures very important when working method rehydroxylation, besides the temperature data in the past are in themselves of great value. Thus, the application of the method in conjunction with rehydroxylation arhaeomagnetic method allows us to solve the problem of dating objects made of baked clay, to obtain information about the ambient temperature and the ancient geomagnetic field in the past. Increasing the accuracy of timing of archaeological sites and materials which are used to study variations in the geomagnetic field, will move in the representation of the mechanism of emergence and existence of the geomagnetic field and its role in the functioning of the whole Earth system. Acknowledgements This work was supported by RFBR grant 09-05-00329. References Aitken M.J., Alcock P.A., Bussel G.D. and Shaw C.J., 1981. Archaeomagnetic determination of the past geomagnetic intensity using ancient ceramics: allowance for anisotropy. Archaeometry. 23, 53.

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Suttie, N., Holme, R., Hill, M.J., Show, J., 2011. Consistent treatment of errors in archaeointensity implies rapid decay the dipole prior 1840. Earth Planet. Sci. Let. 304, 1321. Thellier, E., Thellier, O., 1959. Sur Lintensit du champ magntique terrestre dans le pass historique. Ann.Gophys. 15.285-376. Tosheva, L, Mihailova, B., Wilson, M.A., Carter, M.A., 2010. Gravimetric and spectroscopic studies of the chemical combination of moisture by as-fired and reheated terracotta. Journal of the European Ceramic Society. 30,18671872. Wilson, M.A., Carter, M.A., Hall, C., Hoff, W.D., Ince, C., Savage, S.D., McKay, B., Betts, I.M., 2009. Dating fired-clay ceramics using long-term power law rehydroxylation kinetics. Proc. R. Soc. A, doi: 10.1098/rspa.2009.0117, 1-9.
Table. Results of determinations of time of roasting of ceramics and bricks

from Malaga, Granada, Taman and London and intensity of a geomagnetic field during roasting. Data on the average temperature which obtained from meteorological observations in the regions of research and the geomagnetic field according to observatory data are shown in italics. The error of determination of temperature is calculated taking into account limits of dating of object and accuracy of determination of factor k. Sample Archaeol weight Weight k, Date Average Geomag , ogical of the loss mg/mi of tempera netic site data of sampl P(105) n0.25 rehydr ture T, field B, object e oxylati C mkT AD years P(105) P(500) on, , mg , mg AD years 3s ? 35311 147 2,683 1901 18,5 41,50,3 Malaga, 0,05 15 42,7 Castillo de Gibralfaro 6s -17431 50 1,157 1958 18,5 38,90,3 Malaga, 0,019 2 42,1 Castillo de Gibralfaro 7s -1747 182 2,427 1715 18,5 46,50,1 Malaga, 0,07 35 Castillo de Gibralfaro 121, 16-17 cc. 5761 204 2,991 1535 15,5 53,90,6 Granada, 0,058 35 Alhambra, brick 1b c.I AD 5963 71 -385 11 60,95,2 London, 0,941 0,025 2452 9010 11,80.4 Opus spicatum brick paving 2b 127525 2906 27 0,221 -14460 11 61,00,5

London, Westminster, brick 4b London, Canterbury, brick 1063 Panticape um, plaster of furnace 610 Hermonas sa, ceramic 123, Granada, Cartuja, brick 125 Granada, Cartuja, ceramic 3b, Greenwich brick sample 1s Malaga, Castillo de Gibralfaro

0,009 3727 1400100 20 0,2724 0,025

1275 22,80,3 -13990 1400 15,71,4 11 58,90,8

190 10

6828

111 1,394 0,022

-880 190

11,1 12,50,3

65,50,94

860 60

8121

181

1,903 0,037

-1450 860

11,1 16,90,3

94,50,4

100 10

8399

181

1,182 0,020

-10050 15,5 100 22,60,3 15,5 22,95 0,4

53,30,8

90 10

3353

66

0,4212 0,011

-11210 90

55,40,6

14196

65 (25)

0,5645 0,025

11 -10980 (1725) 11 18.5 18,5 (1935) 50,1 0,2

35526

722 (360)

6.77 0.35

790 25 0

43.6 0.2 41.9