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Luminescence Dating Lab

UW Luminescence Dating Laboratory

The University of Washington Luminescence Dating Laboratory offers a dating service for ceramics, lithics, and sediments. The laboratory specializes in archaeological applications and is particularly interested in research projects in which luminescence can solve archaeological problems not assessable by other dating techniques. The current director, James Feathers, is a professionally trained archaeologist but has been involved in the luminescence field since 1986. The laboratory has produced more than 300 dates, almost all from archaeological contexts, since Dr. Feathers became director in 1993.

Luminescence dating is a rapidly expanding field. Recent advances in technique and instrumentation have improved both the accuracy and precision of the method, with the result that luminescence dating is becoming an important player in quaternary science. The advantage luminescence dating has over other techniques is the ability to date directly events of archaeological and geological interest: the last heating of ceramics and lithics and the last exposure of light for sediments. This often eliminates the need for associational arguments and the uncalibrated loss of accuracy involved therein. The technique is not as precise as radiocarbon, but errors of about 10 percent or better are commonly obtained.

Costs are negotiable, but generally we charge $400 per ceramic sample and $500 per lithic sample. An initial sediment sample costs $800, but additional samples from the same locality will be cheaper depending on the difficulty in dating. University indirect charges, currently 14.7 percent, are added to each project. Turn around times for ceramics and lithics are about 6 months, depending in part on sample queue, but quicker times can be negotiated in special circumstances. Sediment dating usually takes longer. In no case can we guarantee a successful date, although our past performance suggests that we achieve dates that agree with independent dating evidence (which itself is not always accurate) more than 85 percent of the time.

For researchers applying for grant money to fund luminescence dating, the laboratory will be happy to assist in writing the grant proposal at no charge.

Clients interested in using our dating service are advised to contact the laboratory before collecting samples for a feasibility assessment. For sediment dating, it is also advisable to have a luminescence specialist visit the site. Collection instructions are included as a link to this site. Also linked are a laboratory bibliography and current projects being undertaken by the laboratory. We also provide web site links to other luminescence laboratories throughout the world.

Instrumentation: The laboratory is equipped with three glow ovens: an automated Daybreak 1100 reader capable of measuring TL, OSL, and IRSL; an earlier Daybreak version reader for TL only; and a Littlemore reader capable of measuring TL, OSL and IRSL. We have two alpha counters, one high resolution gamma spectrometer and a flame photometer for measuring radioactivity. Other resources include two calibrated Sr-90 beta sources, one Am-241 alpha source, and an Applied Physics solar simulator.

James Feathers
University of Washington
Box 353100
Seattle, WA 98195-3100 USA
Ph: 206-685-1659 or 206-782-9421
FAX: 206-543-3285
Email: jimf@u.washington.edu

What is Luminescence Dating?

Luminescence dating is based on the accumulation of stored energy that occurs in some crystalline materials as a function of natural radioactivity. This energy may be released in the form of a luminescence signal by exposure to sufficient heat or light, which in effect act as zeroing mechanisms. The intensity of a luminescence signal is proportional to the amount of stored energy, which in turn is proportional to the amount of absorbed radiation. If the radiation dose rate is a constant function of time, the luminescence intensity can then be related to the time since the last zeroing event (exposure to heat or light). Since the major sources of natural radioactivity are radionuclides with exceptionally long half-lives, a constant dose rate can be assumed, except where geological processes have altered the radioactive concentrations. This latter situation can often be detected and sometimes corrected.

The following expression is used to derive ages in luminescence dating:

Age (t) = equivalent dose (Gy)/dose rate (Gy/t).

Gy stands for gray, the unit of absorbed radiation and t is unit time. The equivalent dose is the amount of radiation dose equivalent to what was necessary to produce the sample's natural luminescence signal. It is measured by calibrating luminescence sensitivity against artificial irradiation applied in the laboratory. It requires isolating signals that have been thermally stable over time and which increase with applied radiation. The luminescence signal can be stimulated in the laboratory by heating (thermoluminescence, TL) or by exposure to intense light, either from the visible spectrum (optically stimulated luminescence, OSL) or from the infrared (infrared stimulated luminescence, IRSL). The dose rate is the sum of alpha, beta, gamma and cosmic dose rates in the sample and its immediate environment.

For introductions to the method, the reader can consult two books by Martin Aitken, Thermoluminescence Dating (1985, Academic Press), which provides an overall discussion of luminescence and is still the best reference for pottery dating, and An Introduction to Optical Dating (1998, Oxford University), which is a more current review of sediment dating. More specialized reviews on a number of topics can be found in a special volume of Radiation Measurements (1997, Vol. 27 #5/6), edited by Ann Wintle. A review of archaeological applications can be found in an article by Richard Roberts in that same issue and also in Journal of Archaeological Method and Theory (1997, Vol. 4) by the director of this laboratory.

Sample Collection Instructions

Luminescence dating is applied to nonmetallic materials. Two classes of materials can be dated: heated materials (primarily ceramics and burned lithics) and buried sediments. The former is dated to the last heating to about 500°C or so. The latter is dated to the last exposure to light.

Heated Materials

Selection Criteria:

Any coherent ceramic material that has been heated to at least 500°C is potentially suitable. Incidental ceramics (e.g., house daub, hearth fragments) may be variable in this regard even though often ideal subjects. Consequently, select pieces most likely on contextual and physical grounds to have been heated to the highest temperatures.

Lithics are more problematic. There are at least two concerns. One is the possibility for translucent pieces to be optically bleached. When samples are being collected specifically for luminescence dating, they should immediately be placed in opaque containers upon excavation to minimize this problem. For surface finds or lithics exposed to light for long periods after excavation, restriction to opaque specimens is recommended. The other concern is selecting samples that have been heated to at least 450°C. Burned chert or flint can be recognized by discoloring or the appearance of luster, crazing or pot-lid fractures, although none of these can indicate how high the sample has been heated. Unfortunately, a sufficient heating can only be ascertained by the luminescence measurements themselves. While the physical characteristics can be used to select samples, a good precaution is to submit several samples, only some of which may prove to be suitable for dating. It should be noted that flaking properties optimized by heat treatment require temperatures around 370°C, too low for luminescence. Better prospects are lithics that have been accidentally fired in hearths or heat treatment failures (fired too high). Suitable lithics for dating do not have to be flints or cherts. Fire cracked rocks from fire pits have been successively dated.

Finally, luminescence can be a destructive technique. The laboratory will do what it can to save valuable portions of the sample, but in general do not expect to have anything returned. In special cases, dating can be performed on only very small portions of samples.

Size

The outer 2 mm layer of the sample must be removed in the laboratory to eliminate effects of light exposure and influence from environmental beta radiation. After removal, enough material must be left over for analysis. While improved techniques have reduced the amount of sample required for luminescence measurements, larger pieces are still advantageous since more can be done with them. Ceramics at minimum should be about 5 mm thick and 3 cm in diameter; better precision is obtained with larger pieces. Flint or chert artifacts need to be at least 10 mm thick and 5 g in weight.

Context

Samples should be selected from contexts that maximize two parameters: 1) compositional homogeneity within a sphere of 30cm radius around the sample, and 2) contextual stability over the post-depositional period. Both requirements stem from facility in measuring the sample dose rate. Gamma radiation has a range in soils of about 30 cm, so determining the gamma dose rate requires knowledge of the radioactive composition of the environment within 30 cm. This is more difficult the more complicated the environment is. Numerous clasts or stratigraphic boundaries can create a geometric complexity that can frustrate an accurate dose rate measure. Also composition that has changed through time (for example, by leaching or other movements that redistribute the radioactive impurities) will complicate the dose rate assessment. Less than optimal conditions, however, should not deter dating. Often it is possible to account for the uncertainties, although the precision may be less and the cost more. Some complicated contexts, moreover, are not necessarily complicated in terms of radioactivity. If all the different strata and clasts have a similar radioactivity, the dose rate is quite easy to determine. It is always advisable to contact the laboratory before collecting samples to discuss environmental complications and the probability for successful dating.

Treatment

Avoid excessive heating of the sample (do not heat above 100°C) and exposure to ionizing radiation (ultraviolet, infrared, x-rays, gamma-rays) above ambient levels. Any such treatment can reduce the luminescence signal and produce too young ages. Airport and postal inspection X-rays are usually not of significant dosage, but avoid them if possible.

Do not perform any unnecessary treatment of the samples. Particularly avoid contact with materials of unknown composition that may be absorbed by the sample (e.g., glues, preservatives, detergents). Supply a list of treatments that have been applied. Contaminants can affect both the luminescence signal and the radioactive assay. Washing with distilled water is okay.

Sediment Sample

At least 100 g of sediment representing that in which the sample was buried, or on which it was resting in the case of surface items, should be supplied in a plastic bag. Care should be taken to avoid any sorting as different size fractions will typically differ in composition as well. If there is a scatter of small stones (pebble size) or small artifacts, these should be included and larger sample submitted. Exposure of the soil to sunlight, ultraviolet, x-rays, etc., does not matter.

The sediment sample is required for assessment of the environmental gamma dose rate to which the sample has been exposed (up to 30 cm). The sediment should come from within 30 cm of the sample but will be representative of the full environment of the sample only to the extend the latter is homogeneous. In complicated environments different samples for each area of suspected different composition (clasts, different strata, features, etc.) will need to be supplied, assuming the geometry is not too complicated. In exceeding complex environments, in situ measurements of the environmental dose rate is preferred. A common procedure is to bury a small copper capsule (about 1 cm in diameter by 3 cm long) containing a sensitive dosimeter (calcium sulfate is commonly used) for a full year in the same location from which the sample was extracted. The laboratory supplies the capsules. On the day they are to be buried, the capsules must be heated to 400°C, or until they begin to glow red (avoid going too high at risk of melting the solder sealing the ends). This zeroes the dosimeter. Heating can be done with a propane torch, camp stove or other portable heat source. The capsule can be inserted in the sediment by driving a 30cm long plastic conduit (of slightly larger diameter than the capsule) into the profile at the sample location. A string or wire is tied around the capsule, which is pushed to the back of the conduit with the string extended out the front for easy retrieval in a year's time. A full year is recommended to account for annual changes in moisture content (if this varies greatly from average during the time of burial, such information should be provided). On the day of retrieval an accompanying "travel monitor" capsule is heated to 400°C. The monitor accompanies the capsule retrieved from the ground to record the gamma dose received en route to the laboratory. An alternative to dosimeters is to use a portable gamma spectrometer. The laboratory does not have one at present, but access to one is possible under special circumstances. A problem with in situ radiation measurement is that the sample environment is destroyed to some degree in the acquisition of the sample, so that the dosimeter never measures the radiation from the exact same environment as the sample, only something close to it, the significance of which varies directly with the complexity of the environment. Nevertheless, on-site measurements are beneficial for corroboration of laboratory derivations.

In selected cases ceramics or lithics can be dated without a sediment sample. This works only where the samples all come from the same environment so that the external radiation is effectively constant. If all the samples can be assumed to be of the same age, a ratio scale date for them can be obtained by a technique called isochron dating. If the samples are of different ages, only interval scale dates can be obtained. In either case several samples need to be dated, so costs are higher. The laboratory should be consulted for feasibility of dating without sediment samples.

Water Content

Because the radiation absorption coefficient of water differs from than of sediments or pottery, a correction must be made for the water content of the sample and its surroundings. Some approximation must be made of the average water content, how this varies between contexts and with respect to surface conditions, how it might vary seasonally and whether any long term variation is known. The location of the water table with respect to the sample is also desirable. If current water conditions are representative, a sample can be collected in an air tight container and sent to the laboratory for measurement. Other information that might be useful in making an approximation are seasonal and long-term climatic variation and grain size distribution of the sediments (clay, silt, sand, etc.). While usually not precisely known (except in permanently saturated or permanently dry conditions), any information related to water content is useful in improving the precision of the dates. Water content of lithics is much less important than ceramics because of much lower absorption capabilities.

Other Information

  1. Drawings and, if possible, photographs of the contexts from which the sample was taken. The former should roughly show sample locations and approximate distances to any boundaries, such as change in soil type, and whether stones or other clastics are within 30 cm. This information is useful to judge the appropriateness of the sediment sample for the environmental radiation dose rate and other context related matters.

  2. Latitude, longitude and altitude of the site, and depth of burial of the sample. This data is necessary to compute the cosmic ray contribution to the dose rate.

  3. Anticipated ages of the samples, if known. This helps select procedures and appropriate artificial irradiation exposures. While knowing the expected age will not influence our results, it does prompt us to look for explanations when our date does not correspond with expectations.

Buried Sediments

Selection Criteria

Since the dating event is last exposure to light, the most important consideration in selecting sediment samples for dating is the likelihood that the sample was exposed to sufficient light prior to deposition and burial. Sufficient light may be as little as a few minutes of direct sunlight, although complete bleaching usually takes several hours. Aeolian deposits have a high likelihood of long exposures because of airborne time. The bleaching of fluvial deposits depends on the sediment load and the turbity of the flow, deposits from meandering streams generally being well bleached while glacial outflow tending to be less so. Colluvial deposits can be problematic, depending on the nature of the deposition and the grain size of the sediments. Buried soils have been successfully dated because of cycling of A-horizon sediments to the surface by pedoturbation. Bleaching is also affected by shade conditions and cloud cover.

Any kind of crystalline material is potentially datable, but most research has been conducted on quartz and feldspars. The latter tends to have a longer dating range than quartz but can suffer from anomalous fading. Use of other material will require more basic research and thus entail a higher cost. Analysis can be done on coarse grains (generally 90-125µm for quartz, 125-250µm for feldspar) or fine grains (usually 4-11µm), but other sizes have been used as well.

Where sediments down a profile are being selected, it can be useful to have one sample from the surface that represents a "zero-age" sample that can be used to test for extent of bleaching.

Sample Size

Any single sample should be a minimum of 250g, but larger samples are desirable. If the same sample is to be used for radioactivity measurements, at least 350g is needed. More optimal size is 500 to 1000g. In special circumstances very small samples may be sufficient. The vertical extent of the sample will affect resolution depending on the rate of deposition. For example, a sample drawn from a 10cm profile section that accumulated in 1000 years will not be able to resolve at a scale less than 1000 years. The number of samples depends on the specific problem to be addressed and financial resources, but more than one sample from any given context will certainly increase precision.

Collection Procedure

Exposure of the sample to light must be avoided at all costs to avoid an underestimation of the age. This means the sample must be collected under conditions that minimize light and must be stored in opaque containers. There are several solutions to the collection problem. One way is to collect the samples at night, preferably with no moon, aided by low intensity red/orange filtered flashlights. Red to orange light causes insignificant reduction to the luminescence signal. Exposure to within 1 cm of the sample can be done in daylight; then under night light the overlying cm is scraped off and the sample excavated. More convenient are collections in daylight. A common daylight solution is to drive an opaque pipe (plastic or stainless steel) into the sediment and cap both ends. The ends, which will have been exposed, can be removed in the laboratory. It is important to make sure the sediment is secure, not loose. Otherwise mixing of the exposed ends with the unexposed center will occur during transport. If the sample does not fill the entire pipe, some kind of stopper is needed to keep the sediment from moving around. In capping the ends or stopping, do not use material that will oxidize or decompose when in contact with the sample (often damp) and thus contaminate it. Aluminum foil, for example, will oxidize when in contact with wet soil for long periods of time. In sediments that are too hard to drive a pipe in, a block of sediment can be removed as long as it keeps its integrity. The outer surfaces are then removed in the laboratory. Samples can also be collected by coring. Various split-core samplers with light tight sample containers are available. In general, the procedure is to take one core that will be exposed to light in order to define the stratigraphy and the depth of the desired sample. Then core down to just above where the sample will be collected and attach the split core sampler to retrieve the sample.

Radioactivity

Where the sample comes from a very homogeneous deposit, the sample itself can be used to measure radioactivity. Where the environment is more complex, considerations similar to those for heated materials must be taken into account. In a sediment profile where movement through time of radionuclides, either up or down, is suspected, several 70-100g samples down the profile will be useful to model the distribution of radioactivity. No special precautions are needed for these "radioactivity" samples, except to avoid altering their composition.

Other information

For context considerations, treatments, moisture contents, data for cosmic ray dose, drawings, and age estimations, the same procedures as for heated materials should be followed. Moisture contents are somewhat more critical for sediments since they have a larger influence on the dose rate than for pottery or lithics.

Laboratory Bibliography

Readhead, M. L., Dunnell, R. C., and Feathers, J. K., 1988, Recent addition of potassium: a potential source of error in calculating TL ages. Ancient TL 6(1):1-4.

Feathers, J. K., 1993, Radioactive disequilibrium in the TL dating of southeast Missouri pottery, Radiation Protection Dosimetry 47:655-658.

Feathers, J. K., 1993, Thermoluminescence dating of pottery from southeastern Missouri pottery and the problem of radioactive disequilibrium. Archeomaterials 7:3-20.

Kaylor, R., Feathers, J. K., Gottfried, M., Hornyak, W. F., and Franklin, A. D., 1993, Important date/strange material.Ancient TL 10:40-44.

Vandiver, P. V., Feathers, J. K., Kaylor, R., Gottfried, M., Yener, K. A., Hornyak, W. F., and Franklin, A. D., 1993, Thermoluminescence dating of a crucible fragment from an early tin processing site in Turkey. Archaeometry 35:295-298.

Feathers, J. K., 1995, Optically stimulated luminescence of heated materials. In Ceramic Cultural Heritage, proceedings of the International Symposium of the 8th CIMTEC-World Ceramic Congress and Forum on New Materials, edited by P. Vincenzini, pp. 368-374. Techna, Faenza

Dunnell, R. C., and Feathers, J. K., 1995, Thermoluminescence dating of surficial archaeological material. In Dating in Surface Context, edited by C. Beck, pp. 115-137. University of New Mexico Press, Alburquerque.

Kaylor, R., Feathers, J. K., Hornyak, W. F., Franklin, A. D.,1995, Optically stimulated luminescence in Kalahari quartz: bleaching of the 325°C peak as the source of the luminescence. Journal of Luminescence 65:1-6.

Roosevelt, A. C., Lima da Costa, M., Lopes Machado, C., Michab, M., Mercier, N., Valladas, H., Feathers, J. K., Barnett, W., Imazio da Silveira, M., Henderson, A., Sliva, J., Chernoff, B., Reese, D. S., Holman, J. A., Toth, N., and Schick, K., 1996, Paleoindian cave dwellers in the Amazon: the peopling of the Americas. Science 254:1621-1624.

Feathers, J. K., 1996, Luminescence dating and modern human origins. Evolutionary Anthropology 5:25-36.

Feathers, J. K., 1997, The application of luminescence dating in American archaeology. Journal of Archaeological Method and Theory 4:1-66.

Feathers, J. K., 1997, Luminescence dating of early mounds in northeast Louisiana. Quaternary Science Reviews (Quaternary Geochronology) 16:333-340.

Feathers, J. K., 1997, Luminescence dating of sediment samples from White Paintings Rockshelter, Botswana. Quaternary Science Reviews (Quaternary Geochronology) 16:321-331.

Saunders, J. W., Mandel, R. D., Saucier, R. T., Allen, E. T., Hallmark, C. T., Johnson, J. K., Jackson, E. H., Allen, C. M., Stringer, G. L., Feathers, J. K., Frink, D. S., Williams, S., Gremillion, K. J., Vidrine, M. F., and Jones, R., 1997, A mound complex in Louisiana at 5400-5000 years before present. Science 277:1796-1799.

Feathers, J. K., and Rhode, D., 1998, Luminescence dating of protohistoric pottery from the Great Basin. Geoarchaeology 13:287-308.

Michab, M., Feathers, J. K., Joron, J.-L., Mercier, N., Selos, M., Valladas, H., Valladas, G., Reyss, J.-L., and Roosevelt, A. C., 1998, Luminescence dates for the paleoindian site of Pedra Pintada, Brazil. Quaternary Science Reviews 17:1041-1046.

Feathers, J. K., in press, Why luminescence dating deserves wider application in American archaeology. In It's About Time, edited by Stephen Nash, University of Utah Press.

Feathers, J. K., and Bush, D. A., in press, Luminescence dating of Middle Stone Age Deposits at Die Kelders, Journal of Human Evolution.

Feathers, J. K., and Migliorini, E., Luminescence dating at Katanda – A reassessment. Quaternary Geochronology, submitted.

Feathers, J. K., Dating the Howiesons Poort assemblages at Diepkloof, western Cape, South Africa, by luminescence methods. South African Journal of Science, submitted.

Feathers, J. K., Thermoluminescence of Southwestern United States ceramics: a date list. Ancient TL, in preparation.

Feathers, J. K., Thermoluminescence of Eastern North American ceramics: a date list. Ancient TL, in preparation.

Dykeman, D. D., Towner, R. H., and Feathers, J. K., Tree-ring and thermoluminescence dating techniques: methods for confidently dating early Navajo sites, American Antiquity, in preparation.

Feathers, J. K., Brooks, A., and Yellen, J. Reassessing dating evidence at Katanda. Science, in preparation.

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