The following is a self-archived preprint version of S. Zhao, P. K. Bowen, J. W.

Drelich, and T. J. Scarlett, Reproducibility in rehydroxylation of ceramic

artifacts, J. Am. Ceram. Soc., DOI: 10.1111/jace.13745.

Reproducibility in Rehydroxylation of Ceramic Artifacts

S. Zhao,1 P. K. Bowen, 1, J. W. Drelich,1* T. J. Scarlett2
1
Department of Materials Science and Engineering
2
Department of Social Sciences
Michigan Technological University
Houghton, MI 49931, USA

Abstract
Since its introduction in 2009, application of the rehydroxylation (RHX) technique for dating
fired-clay ceramics has been controversial, with very few satisfactory dating results collected in
the interim. The stability and efficiency of this technique has been called into question by several
investigators in the last few years, who have struggled to reproduce and validate this new dating
method. Based on our new mass gain measurements for ca. 2000-7000 years old ceramic
artifacts, the reproducibility in the RHX process rate is analyzed and discussed. Timespan
analysis was performed, and age uncertainty related to RHX dating technique was evaluated by
considering the error propagation. The results show poor reproducibility of the RHX process in
the samples of the same origins, which give new evidence for a revision of the RHX protocols.

Keywords: rehydroxylation; fired clay ceramic; reproducibility; data scatter

*Authors to whom correspondence should be addressed, email: jwdrelic@mtu.edu and

shanzhao@mtu.edu

Introduction
Rehydroxylation (RHX) dating was proposed in 2009 as an easy and reliable technique in dating
sherds of unglazed archaeological pottery.

It relies on monitoring the rate at which water is

regained by refired ceramics through rehydration (Stage I) and rehydroxylation (Stage II)
1

processes, 2 and then modeling the Stage II process by a power law-correlation: 4 , where
is the change in sample mass and t is the time after firing or reheating of the ceramic.

3, 4, 5

The mass gain term, m, can be defined in terms of measured mass (in grams) or as a fractional
mass gain value relative to the starting mass of the sample (g/g); the latter is used here. The
roots of this power law correlation have been proposed to originate from a single file diffusion
mechanism

for water molecules migrating through the clay and meta-clay structures in

ceramics. Under these assumptions, the time elapsed since the last firing of the ceramic artifact
can be estimated from the accurate measurement of Stage II mass-gain kinetics. 1
Since its introduction, great effort has been invested in this new dating method by several
archeological and materials research groups. Unfortunately, only ten fired clay fragments have
been convincingly shown to be successfully dated,
Attempts by others have failed,

7, 8, 9, 10, 11

which is a surprisingly small number.

and major concerns about this new dating technique

continue to include: i) the stabilization of sample mass after the removal of physically bonded
water; ii) the universality of reheating conditions used to remove chemically bonded water; iii)
the stability and self-calibrating ability of the technique;

8
1

and iv) the validity of the single file

diffusion mechanism, which provides a basis for the 4 power law.

12

Very recent studies

demonstrate that appropriate chemical pre-treatment of archaeological material and/or the

theoretical limits to rehydroxylation dating could be helpful in optimizing instrument design.

13

Additionally, the relative insensitivity of the rehydroxylation rate to short-term humidity

2

fluctuations was demonstrated, providing strong, but still qualitative, experimental support for ceramic
artifacts dating through examination of the rehydroxylation process.

14

To succeed with the RHX dating method, at a minimum, the following conditions need to be met:
a)

the mass of non-refractory component from as-received samples must be negligible to

avoid the release of non-water constituents upon refiring;

b)

excess capillary water is removed during drying prior to re-equilibration at

experimental conditions specified under c;

c)

the sample is well equilibrated (attains a constant mass) in a constant humidity at a

temperature that represents effective lifetime temperature (ELT) of the artifact at the
archeological site;

d)

all water, including the hydroxyl water that is chemically bonded to clays, is totally
removed during refiring;

e)

the water gains are obtained for refired ceramic under constant humidity and
temperature (the same as in step d); and

f)

the rate water pick up fits the power law 4 .

Although these conditions are quite well recognized by the research community working on the
RHX dating method, little was done to critically examine the effects these conditions have on
dating. Most of the research followed blind protocols of set time and temperatures during the
experimentation suggested in original publication by Wilson et al.,

and publications that

followed from the same research group. 3, 4, 5, 15, 16, 17, 18 Because no other research team was able
to successfully date ceramic artifacts through the protocols proposed by Wilson et al., the RHX
dating method remains controversial. Only poorly reproducible results were reported so far, 8, 9, 10,
3

14, 19

with many requiring variations on the original 4 power law. In our previous contributions,
1

we have used a generalized power law ( ) with a variable exponent (n), to describe the RHX
1

behavior of ceramics without identifying their ages. 10 The vs. curves produced for several
samples demonstrated improved linearity in RHX Stage II. 9, 12
The purpose of this contribution is to examine the reproducibility of the Stage II kinetics in the
RHX dating protocol for a group of small sherds from the same parent fragment after refiring at
500oC. The intragroup repeatability was examined for four such sets of ceramic artifacts, all
treated identically. Understanding the reproducibility of RHX dating raises new questions about
the validity of the dating protocol suggested in the past.

Experimental
In our study, four sets of sherds of fired clay ceramics from Mediterranean locations were
examined (Table 1). Ceramic samples were collected and provided for this research by
Prof.Kostalena Michelaki from Arizona State University. The sherds were cleaned to remove
loose debris and dirt, and washed with deionized water. Larger fragments, typically squareshaped cross sections, were cut into approximately 10 10 5 mm pieces with a water-cooled
diamond saw. Masses of the final samples varied from 0.4 to 1.0 g. One fragment of each set of
samples of the same origins was dried at 110C for 5 to 7 days as a control sample. Four to six
other samples were furnace dried overnight at 300C. This elevated drying temperature was used
here to speed up the drying process. We found previously (unpublished) that some ceramic
artifacts hold some amount of physically bonded water very strongly and drying them at 110120oC is not always sufficient to remove the totality of physically bonded water.

After drying, all samples were placed in a glove box (Coy Laboratory Products, Grass Lake, MI)
equipped with a Citizens CM-11 microbalance (Citizen Scale Inc., Edison, NJ) having 1 g
precision. The glove box was set for 202% RH (relative humidity) for the duration of the whole
experiment and located in a lab with an average ambient temperature of 202C. The mass of
each sample was recorded for several days until it reached its equilibrium mass, previously
defined as 2 by Wilson et al.,

15

characterized by measurement-to-measurement mass changes

no larger than 0.01%. Then all samples were fired in a box furnace at 500C for 1 to 3 days and
placed back into the glove box, again at 20C and 20% RH. Samples were labeled with their
drying temperature and refiring times; for example, 300C-2a would mean that the sample was
heated at 300C, equilibrated to find 2 , and then fired for two days at 500C. The refired
ceramic mass 0 was critical to all other experimentation, as it was the value to which changes
in mass were normalized to yield a fractional value of . Sample weight was monitored
periodically after refiring; every 15 min in the first couple of hours, then every 1-2 hours, and
finally at least once a day for several weeks. X-ray diffraction (XRD) measurement was
performed on a small sample surface by using Scintag XDS2000 / X-ray diffractometer with
Cu K radiation ( = 1.540562 ). The scans were performed continuously from 15 to 70o in 2
at a speed of 0.6o/min with a step size of 0.02o. The XRD instrument was operated at a tube
potential of 45 kV and 35 mA filament current. Peaks were identified using the DMSNT (Scintag
Inc.) software package in concert with the Powder Diffraction Database Search (PDDS) software
(Scintag Inc. and Radicon Ltd., St. Petersburg, Russia). The PDDS software was used to search
the Joint Committee on Powder Diffraction Standards-International Center for Diffraction Data
(JCPDS-ICDD) database.

Statistical Analysis
Linear regression analysis was used in this study to analyze the linear, Stage II portion of the
1

versus 4 curves.
1

Timespan analysis was performed by comparing the RHX rate () against the 4 . The RHX rate
1

() was calculated by the slope of the fractional RHX mass gain with respect to 4 , and was
calculated at intervals that began with the last data points and was gradually expanded to include
data back to t = 0 (using the slope from the end approach).

In this presentation, values

calculated near the end of the experiment experience large perturbations due to the small number
of data points considered; as the timespan analysis approaches the transition to Stage II mass
gain the value of becomes more statistically robust.
Random error propagation analysis

20

was used to estimate the error associated with the RHX

dating outcome. It was assumed that the archaeological age of the sample (ta), is described by
Equation 1:
2 4 4

= (

(1)

where = 2 4, 2 is the equilibrium fractional mass (normalized with respect to 0 ),

4 is the y-intercept of the linear segment of the vs. t1/4 plot according to Wilsons et al.15
Then, the uncertainty associated with ta was estimated by the root of the sum of the square of
each terms associated standard error multiplied by the partial derivative of ta with respect to the
same term. This is shown in Equation 2:

2 + ( )2 2
= ( )2 2 + (m )2 m
m2
4
m
4

(2)

The standard error values for the coefficients and 4 were determined by using the "LINEST"
function in Microsoft Excel. Standard error for 2 was estimated as the fractional measurementto-measurement deviation of the equilibrium mass (0.01%). Sources of systematic-type error
are not included in this approach.

Results and Discussion

All ceramic artifacts selected were multiphase. Mineralogical analysis via XRD revealed quartz
as the dominant phase and at least 4-5 secondary phases (Figure 1). For all samples, the peaks of
quartz are high and narrow (especially at 2=20.90 and 26.66), indicating that a relatively large
amount of highly crystalline material was present. The clay mineral illite-2M1 (JCPDS-ICDD
No. 26-0911) and illite-2M2 (43-0685) were confirmed by the presence of characteristic peaks at
19.8, 23.9, 29.9 and 30.3, 34.7, 37.4 respectively. Plagioclase feldspar was recognized by the
presence of its two end phases: albite (09-0466) and anorthite (41-1481), which were identified
by small peaks at 22.0, 23.5, 27.9 and 27.8, 33.8, 35.7, respectively. Apart from the quartz
phase, sample RLG 007 showed large amount of calcium carbonate (85-1108) identified by the
peaks at about 29.5, 39.5, 47.6, 48.6. Since our sample is not in the pulverized form so there
might be the possibility of accidentally deposition of a large amount of weathering
product/concretion on the surface. From XRD results, it can be seen that the high crystallinity of
ceramics coming from the non-RHX active components (quartz, feldspars) while there was
relatively little evidence of crystalline RHX-active components (i.e. illite).
As shown in Figures 2 to 5, results from all four sets of samples illustrate different RHX
behaviors. The values of linear regression variables describing Stage II RHX fractional mass
gainthe intercept, 4 , and the RHX rate, are summarized in Tables 2 to 5.

Seven fragments from sample RLG 019 show a typical two-stage progression of mass with t1/4 .16
Neither drying at 300C, nor prolonged firing time showed a significant effect on the RHX rate.
The timespan analysis of the RHX curve (shown in solid lines) indicates that a trend is present
for the RHX rate () throughout the experiment. Instead of reaching an ideal plateau near the
Stage II transition, appears to increase systematically as the interval of analysis increases up to
the time where Stage II presumably begins. The observed scattering and fluctuations of over
the entire timespan analysis could be argued to increase uncertainty in the calculated age.
For sample RLG 024, evolution of fractional mass gain does not strictly follow the two-stage
pattern; it displays both concave and convex behavior at different times. As the observed
curvature for all six specimens does not occur at the same time, it is likely that the disturbance
comes from the intrinsic instability of the sample and the RHX technique. It is rather unlikely
that this could be attributed to perturbation of the environment, as all samples within the set were
simultaneously submitted to concurrent temperature and humidity fluctuations. With respect to
the RHX rate over time, samples 300C-1c and 100C-1 show a plateau in from 3.0-4.0 and 3.54.2 hr1/4, respectively, while the others do not appear to stabilize at all in the timespan analysis.
Because external conditions were identical, the different RHX behavior of samples from the
same sherds [300C-1 (a, b, c, d, and e)] indicates the poor reproducibility of the technique.
Overall, the RHX rates of RLG 024 specimens appear to scatter more than those from RLG 019,
and lead to larger average age uncertainties. The vast scattering can also be evidenced from the
wide range of 4 and value listed in Table 3. The higher drying temperature, again, had no
discernable effect on the RHX rate. The change in drying conditions appeared to both increase
the RHX rate from 96 g/h1/4 to 400 g/h1/4, as well as decrease it to 47 g/h1/4. The fact that

values nearly ranged over a full order of magnitude is worrisome; in principle, this value should
be practically constant.
Fractional mass gain for sample RLG 007 resembles sample RLG 019, in that both sets of
samples exhibit a typical two-stage progression of mass with time1/4. The timespan analysis over
the entirety of Stage II (Figure 4) shows RHX rates that are relatively flat with a narrow
spreada better outcome than for other samples. Also like RLG 019, the value of in the
timespan analysis appears to depend strongly on the time at which Stage II is assumed to begin.
The timespan and linear regression analyses indicate that the scattering for a family of specimens
cut from the same larger sherd differs from sherd-to-sherd, which is in agreement with recent
results shown by LeGoff and Gallet.

Separation in 4 between 300C-1a and 300C-1c is as

wide as 25%, but samples 100C-1 and 300C-1e, they exhibit nearly identical RHX behavior.
Taken in whole, results in RLG 007 again indicate poor stability in the RHX process.
For sample RLG 014, a plateau in the RHX rate () was observed in Stage II at 2.5-3.5 h1/4. Even
though relatively constant values were observed, their magnitudes vary widely, by as much as
82%. Again, the poor sample-to-sample consistency cannot be explained by random error or
fluctuations in either temperature or RH conditions. The poor reproducibility instead points to
intrinsic instabilities in the RHX process. It should be mentioned that samples 110C-1 and 300C2a exhibited an unexpected mass decrease near the end of the experiment. It is thought that this
was a result of sample disintegration.
For all four sets of samples, the scattered nature of the RHX process introduce 10-40% of
random uncertainty in the calculated ages and the estimated ages are much younger than their
documented ages (Table 1). (However, in the case of RLG 007, the absolute calculated dates

should be much shorter due to RHX measurements being performed at temperatures substantially
higher than the parent sherds ELT. In this case, the sample ages cannot be compared to the
documented age.) This consistent outcome points to some source of systematic error (>99%) in
the RHX dating process that caused a mismatch between the calculated and archaeological ages.
There was also a noticeable amount of scatter within each family of samples, especially RLG
007 and 014, which had calculated ages that spanned two orders of magnitude. The scatter could
be explained, in part, by the pronounced scatter behavior of in Stage II as well as the
subjectivity involved in selecting a Stage II transition in samples that did not show a RHX rate
plateau. If one desired, dates could be made to appear older or younger by arbitrarily selecting a
cut-off point along the timespan analysis that gave the desired RHX rate () and value of 4 .
The data illustrate the troubling scatter in RHX rates and calculated dates between samples cut
from the same parent sherds, and processed in an identical manner.

Conclusions
By examining the RHX rate for all the four series of samples, few examples of consistent RHX
rates, with respect to both time and other samples within a family, were identified. Replicate
experiments show striking scatter at two drying conditions (110C and 300C) and different
refiring conditions (500C for 1 to 3 days), with no discernable effect of either condition on
RHX kinetics. High intragroup variation of RHX rate within a batch of specimens cut from the
same parent sherd is indicative of poor intrinsic Stage II stability when analyzed in the t1/4 power
law framework. The poor stability and the scattered nature of the RHX process introduce 10-40%
of random uncertainty in the calculated ages. This is in addition to unidentified systematic errors
(in some cases corresponding to >99% error) that result in shorter-than-actual calculated ages for

10

all specimens examined here. All the results are indicative of inherent, unexplained complexities
in applying the RHX dating technique to archaeological fired-clay ceramics.

Acknowledgements
We thank Kostalena Michelaki from Arizona State University for providing the fragments used
in the current study, and our collaborator Carl Lipo and Elizabeth Niespolo from California State
University at Long Beach for helpful discussions over the course of RHX experiment. This
project was supported by an Archaeometry Research Award from the United States National
Science Foundation (No.1219540).

References
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Betts, "Dating fired-clay ceramics using long-term power law rehydroxylation kinetics,"
Proc. R. Soc. London, Ser. A, 465[2108] 2407-15 (2009).
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Ceram. Soc., 95[9] 2673-78 (2012).
3. M. A. Wilson, W. D. Hoff, C. Hall, B. McKay, and A. Hiley, "Kinetics of Moisture Expansion
in Fired Clay Ceramics: A (Time)1/4 Law," Phys. Rev. Lett., 90[12] 122503-1-03-4
(2003).
4. S. D. Savage, M. A. Wilson, M. A. Carter, W. D. Hoff, C. Hall, and B. Mckay, "Moisture
expansion and mass gain in fired clay ceramics: a two-stage (time)(1/4) process," J. Phys.
D: Appl. Phys., 41[5] 055402(4pp) (2008).
5. S. D. Savage, M. A. Wilson, M. A. Carter, B. McKay, W. D. Hoff, and C. Hall, "Mass Gain
due to the Chemical Recombination of Water in Fired Clay Brick," J. Am. Ceram. Soc.,
91[10] 3396-98 (2008).
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6. P. S. Burada, P. Hanggi, F. Marchesoni, G. Schmid, and P. Talkner, "Diffusion in confined

geometries," ChemPhysChem, 10[1] 45-54 (2009).
7. M. Le Goff and Y. Gallet, "Evidence for Complexities in the RHX Dating Method,"
Archaeometry DOI: 10.1111/arcm.12137 (2014).
8. M. Le Goff and Y. Gallet, "Evaluation of the rehydroxylation dating method: Insights from a
new measurement device," Quat. Geochronol., 20 89-98 (2014).
9. P. K. Bowen, J. W. Drelich, and T. J. Scarlett, "Modeling Rehydration/Rehydroxylation MassGain Curves from Davenport Ceramics," J. Am. Ceram. Soc., 96[3] 885-91 (2013).
10. P. K. Bowen, H. J. Ranck, T. J. Scarlett, and J. W. Drelich, "Rehydration/Rehydroxylation
Kinetics of Reheated XIX-Century Davenport (Utah) Ceramic," J. Am. Ceram. Soc., 94[8]
2585-91 (2011).
11. K. S. Burakov and I. E. Nachasova, "Archaeomagnetic study and rehydroxylation dating of
fired-clay ceramics," Izv. Phys. Solid Earth, 49[1] 105-12 (2013).
12. M. Le Goff and Y. Gallet, "Experimental variability in kinetics of moisture expansion and
mass gain in ceramics," J. Am. Ceram. Soc., In press (2014).
13. V. J. Hare, "Theoretical constraints on the precision and age range of rehydroxylation
dating," Vol. 2: Royal Society Open Science DOI: 10.1098/rsos.140372, (2015).
14. J. W. Drelich, P. K. Bowen, and T. J. Scarlett, "Effect of Humidity Instability on
Rehydroxylation in Fired Clay Ceramics," J. Am. Ceram. Soc., 96[4] 1047-50 (2013).
15. M. A. Wilson, A. Hamilton, C. Ince, M. A. Carter, and C. Hall, "Rehydroxylation (RHX)
dating of archaeological pottery," Proc. R. Soc. London, Ser. A, 468[2147] 3476-93
(2012).

12

16. M. A. Wilson, S. Clelland, M. A. Carter, C. Ince, C. Hall, A. Hamilton, and C. M. Batt,

"Rehydroxylation of Fired-Clay Ceramics: Factors Affecting Early-Stage Mass Gain in
Dating Experiments," Archaeometry, 56[4] 689-702 (2014).
17. C. Hall, M. A. Wilson, and W. D. Hoff, "Kinetics of Long-Term Moisture Expansion in
Fired-Clay Brick," J. Am. Ceram. Soc., 94[11] 3651-54 (2011).
18. C. Hall, A. Hamilton, and M. A. Wilson, "The influence of temperature on rehydroxylation
[RHX] kinetics in archaeological pottery," J. Archaeol. Sci., 40[1] 305-12 (2013).
19. G. T. Barrett, "Rehydroxylation dating of fired clays: an improved time-offset model to
account for the effect of cooling on post-reheating mass gain," J. Archaeol. Sci., 40[10]
3596-603 (2013).
20. Y. Beers, "Introduction to the Theory of Error." Addison-Wesley Publishing Company, INC.:
Massachusetts, Palo Alto, London, (1957).
21. J. Robb, L. Foxhall, and D. Yoon, "Bova Marina Archaeological Project survey and
excavations: Preliminary Report. ," pp. 33-35. in. Department of Archaeology, University
of Cambridge, The soprintendenza archeologica della Calabria., 2003.
22. K. Michelaki, R. G. V. Hancock, and G. V. Braun, "Using provenance data to assess
archaeological landscapes: an example from Calabria, Italy," J. Archaeol. Sci, 39[2] 23446 (2012).
23. K. Michelaki, G. V. Braun, and R. G. V. Hancock, "Local Clay Sources as Histories of
HumanLandscape Interactions: a Ceramic Taskscape Perspective," J. Archaeol. Method
Theory (2014).

13

24. J. B. Auban, T. O. Kohler, A. D. Castillo, M. G. Puche, and F. J. M. Hernandez, "Mas dIs

(Penguila, Alicante): aldeas y recintos monumentales del Neoltico Inicial en el valle del
Serpis," Trabajos de Prehistoria, 60[2] 39-59 (2003).
25. J. B. Auban and T. O. Kohler, "Mas d Is (Penaguila, Alicante): un recinto monumental del VI
milenio cal BC," pp. 485-96. in. Universidad de Cantabria, Santander,Espaa., in Actas
del III Congreso del Neoltico en la Pennsula Ibrica, 2005.

14

Table 1. Sample Information

Sample

Site and
Archaeological
Context

Location

ELT/ oC

RLG007

Mas D'Is; D4;

Sherd #100405

Penguila,
Alicante,
Spain

10.9

RLG014

Umbro Greek/
T2 N73 E45
Context 237
Bag 2348

Bova Marina,
Calabria, Italy

19.520.5

RLG019

Umbro
Neolithic
T6 N6 E59
Sherd #142158

Bova Marina,
Calabria, Italy

19.520.5

Age:
Achaeometric
or
Calendrical
and RHX
target in
Years before
2014
Neolithic
5,590 +/-40
BP,
TRHX: 5,6145,694
Classical
Greek
425-350 BC
TRHX: 2,4392,364

Main Phases

Quartz, illite2M1,
calcite
Quartz, illite2M1,
anorthite, albite,

Early to
Quartz, illiteMiddle
2M1,
Neolithic
anorthite, albite
5,500-5,000
Cal BC
TRHX: 7,5147,014
RLG024
Penitenzeria;
Bova Marina,
19.5Early/Middle
Quartz, illiteT4; E40 N46
Calabria, Italy
20.5
Neolithic
2M1(2),
Sherd #20385,500-5,000
anorthite, albite
66
Cal BC
TRHX: 2,4392,364
Sample dates include expected dates expressed as calibrated or uncalibrated radiocarbon dates or using
the known date range of cultural phases at the specific site. These dates are then converted into RHX
Target Age (TRHX) understood as years before A.D. 2014. Samples RLG014, RLG019, and RLG024
were recovered during excavations by the Bova Marina Archaeological Project team. Details about the
excavation contexts for the sample sherds have been reported elsewhere 21, 22, 23. Sample RLG007 is from
the site of Mas DIs which has also been described in the literature 24, 25.

15

Table 2. Time RHX parameters for RLG 019

Sample
RLG 019
100C-1

Nominal
Mass
0.780520

m4105[g/g]

105[(g/g)/h1/4]

Age/year

1053 9

160 2

2.1 0.2

300C-1a

0.693347

932 10

156 3

1.6 0.1

300C-1b

0.762487

956 9

161 2

1.3 0.2

300C-2a

0.520244

936 10

163 3

2.2 0.2

300C-2b

0.814421

949 9

157 2

1.7 0.2

300C-3a

0.895630

929 11

156 3

2.1 0.3

300C-3b

0.504413

873 1

156 3

1.7 0.2

16

Table 3. Time RHX parameters for RLG 024

Sample
RLG 024

Nominal
Mass

m4105[g/g]

105[(g/g)/h1/4]

Age/year

100C-1

0.80787

698 7

10 2

74

300C-1a

0.684012

807 14

54

31

300C-1b

0.624774

664 16

19 4

1.3 0.4

300C-1c

0.92682

849 10

20 3

0.5 0.1

300C-1d

0.886827

610 8

31 2

1.4 0.5

300C-1e

0.811570

834 10

40 3

43

17

Table 4. Time RHX parameters for RLG 007

Sample
RLG
007

Nominal
Mass

m4105[g/g]

105[(g/g)/h1/4]

Age/year

100C-1

0.635143

864 11

130 3

38 1

300C-1a

0.591287

990 13

135 3

0.5 0.1

300C-1b

0.750737

782 10

137 3

24 2

300C-1c

0.622529

739 9

133 2

23 2

300C-1d

0.603122

754 11

119 3

290 30

300C-1e

0.577538

870 11

121 3

33 4

18

Table 5. Time RHX parameters for RLG 014

Sample

Nominal

RLG 014

Mass

100C-1

m4105[g/g]

105[(g/g)/h1/4]

Age/year

252 8

55 3

685 27

300C-1a

0.659297
0.622409

257 5

59 1

34 9

300C-1b

0.656815

336 12

35 2

91

300C-2a

0.458795

237 7

59 2

600 200

300C-2b

0.682371

200 6

62 2

15 3

300C-3a

0.629391

242 6

11 4

157 23

19

Figure 1. X-Ray diffraction results for each parent sherd.

20

Figure 2. RHX mass gain and RHX rate of RLG 019. After drying at 110C (100C-1) and 300C,
they were fired at 500C for 1, 2, or 3 days samples denoted as 300C -1a(b), 300C -2a(b),
300C -3a(b), respectively.

21

Figure 3. RHX mass gain and RHX rate of RLG 024. After drying at 110C (100C-1) and 300C,
they were fired at 500C overnight samples denoted as 300C-1 (a, b, c, d, e)).

22

Figure 4. RHX mass gain and RHX rate of RLG 007. After drying at 110C (100C-1) and 300C,
they were fired at 500C overnight, which was denoted as 300C-1 (a, b, c, d, e)).

23

Figure 5. RHX mass gain and RHX rate of RLG 014. After drying at 110C(100C-1) and 300C,
they were fired at 500C for 1, 2, 3 days, which was denoted as 300C -1a(b), 300C -2a(b), 300C
-3a respectively.

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