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Archaeometry 57, 6 (2015) 966976

doi: 10.1111/arcm.12149

EL E M E N TA L CHARACT E RIZ AT IO N BY ED X R F O F I MPER I A L

LO N G Q UAN CE L ADON P ORCE LA I N EX C AVATED FR O M
FENGDONGYAN KIL N, D AYA O C O U N TY *
L. LI,1 L. T. YAN,1 S. L. FENG,1 Q. XU,1 L. LIU,1,2 Y. HUANG1,2 and X. Q. FENG1
1

Key Laboratory of Nuclear Radiation and Nuclear Energy Technology, Institute of High Energy Physics, Chinese Academy
of Sciences, 19 Yu Quan Lu, Beijing 100049, China
2
University of Chinese Academy of Sciences, Chinese Academy of Sciences, Beijing 100049, China

A mass of Longquan porcelain shards carved with Guan or the dragon patterns were
unearthed in the early Ming Dynasty layer of the Fengdongyan kiln site at Dayao County.
These celadon shards were fired in the Hongwu and Yongle eras of the Ming Dynasty. In order
to research the raw materials and firing technology of the imperial porcelain, 85 typical shards
were analysed by energy-dispersive X-ray fluorescence (EDXRF). The results indicate that the
contents of TiO2 and Fe2O3 in the body vary in the Hongwu and Yongle eras. Compared with
Longquan glazes in the Southern Song Dynasty, the average values of K2O, Fe2O3 and TiO2 are
higher, but that of CaO is lower in early Ming imperial porcelain glazes. Principal components analysis (PCA) shows that different degrees of elutriation of the same raw materials are
the main reason for this difference in the Hongwu and Yongle periods. However, the raw
materials of imperial porcelain glazes show no obvious changes and have inherited the earlier
tradition. The production and firing technology of imperial porcelain reached a higher level
and had not declined in the Early Ming Dynasty.
KEYWORDS: EDXRF, LONGQUAN KILN, IMPERIAL PORCELAIN, FENGDONGYAN
KILN, PCA

INTRODUCTION

Longquan celadons, with higher firing technology and greater artistic merit, play a significant
role in the history of ancient Chinese celadon. According to previous archaeological evidence (Li
1998), it is well known that the Longquan kilns, located in Longquan City in Zhejiang Province,
began to fire celadon in the Southern and Northern Dynasties (ad 420589), and developed in the
Southern Song (ad 11271279) and Yuan Dynasties (ad 12711368). It used to be thought that
the firing technology had declined in the Ming Dynasty (ad 13681644), as stated in several
references (Chou et al. 1973; The Light Industry Hall of Zhejiang Province 1989; Li 1998). But
did the firing technology of Longquan celadon really begin to decline in the Ming Dynasty? Were
the Longquan kilns still the famous kilns that made porcelain for the palace?
In the past, research interest was focused on the development history and the decorative arts of
the civilian porcelain of Longquan celadon (Li et al. 1984; Ye et al. 1999; Jin 2007). Due to the
lack of specimens, the raw materials and firing technology of the imperial porcelain of Longquan
celadon has been little investigated. But the excavation of the Fengdongyan kiln provides
physical evidence. From September 2006 to January 2007, the Fengdongyan kiln, located in
*Received 8 January 2014; accepted 8 September 2014
Corresponding author: email fengxq@ihep.ac.cn
2014 University of Oxford

Characterization by EDXRF of imperial Longquan celadon porcelain

967

Figure 1 The location map for the Dayao County kiln, amongst the Longquan kilns.

Dayao County, in Longquan City (see Fig. 1), was excavated by the Zhejiang Province Institute
of Cultural Relics and Archaeology, the School of Archaeology and Museology of Peking
University and the Longquan Museum. A mass of exquisite Longquan celadon shards of the Yuan
and Ming Dynasties were unearthed, including abundant civilian porcelain and a lot of official
wares carved with Guan or the dragon patterns in the Hongwu and Yongle eras of the Ming
Dynasty (Zhejiang Institute of Cultural Relics et al. 2009). The emergence of this imperial
porcelain has led to great repercussions in archaeology. Some scholars have published comparisons between the imperial porcelain of the Ming Dynasty and the Longquan porcelain of the
Southern Song Dynasty (Peng et al. 2009). However, what differences are there between the
imperial porcelain of the Ming Dynasty and the civilian porcelain of the Early Ming Dynasty? At
present, there is little research comparing imperial porcelain with civilian porcelain in the Ming
Dynasty.
In this paper, we have determined the chemical composition of imperial Longquan celadon
porcelain using energy-dispersive X-ray fluorescence (EDXRF). It is well known that the contents of major, minor and trace elements of the porcelain body and glaze are dependent on its raw
material and manufacturing technology (Li 1998; Kerr and Wood 2004; Artioli 2010), which can
be used to indicate the age of the porcelain and its provenance. From a statistical analysis of the
elemental data, the raw material and the development of porcelain firing technology are discussed. The information is used to display the inheritance relationship of the raw materials used
for the body and glaze in different periods.
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Figure 2 Photographs of imperial porcelain samples from the HWM and YLM periods.

Table 1

Detailed information on the celadon shards from the Fengdongyan kiln site

Group

Date

Number of shards

HWM
YLM
EM

Hongwu era of the Ming Dynasty

Yongle era of the Ming Dynasty
Early Ming Dynasty

32
53
48

Exterior characteristics
Celadon glaze, grey body
Celadon glaze, grey body
Celadon glaze, grey body

SAMPLES

In this work, 85 typical shards of imperial porcelain from the Fengdongyan kiln were provided
by Zhejiang Province Institute of Cultural Relics and Archaeology. These imperial porcelain
samples can be grouped into two cultural periods: the Hongwu (HWM group) and the Yongle
(YLM group) eras of the Ming Dynasty. Since Hongwu and Yongle are Early Ming, 48 shards
of civilian porcelain excavated at Fengdongyan dated to the Early Ming Dynasty (EM group)
were selected for comparison with the imperial porcelain. Some photographs of imperial porcelain shards are shown in Figure 2 and detailed information about the samples is listed in
Table 1.
THE EDXRF EXPERIMENT

A sample measuring 30 mm 10 mm was cut from the shard, and the cross-section was polished,
and then washed three times in an ultrasonic cleaner with deionized water and dried at 105C.
The EDXRF experiments were performed on an EDAX Eagle III spectrometer at the Institute of
High Energy Physics, CAS, Beijing, China. The spectrometer has a Mo tube and a 125 m Be
window with an incident beam angle of 65 and an emergence angle of 60. The detector is a
liquid-nitrogen-cooled Si(Li) crystal with a resolution of 160.3 eV at MnK. There is a vacuum
chamber and the diameter of the X-ray beam spot is selected to be 1 mm. The voltage and current
of the X-ray tube are 40 kV and 250 A, respectively. The software employed for spectrum
deconvolution and analysis is VISION32, which is associated with the instrument. A set
of standard reference samples with known chemical compositions, which were developed by the
2014 University of Oxford, Archaeometry 57, 6 (2015) 966976

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Characterization by EDXRF of imperial Longquan celadon porcelain

Table 2

Experimental
value
Certified
value

The quantitative results for the ancient ceramic samples

Na2O
(%)

MgO
(%)

Al2O3
(%)

SiO2
(%)

K2O
(%)

CaO
(%)

TiO2
(%)

MnO
(%)

Fe2O3
(%)

Cu
(ppm)

Zn
(ppm)

Rb
(ppm)

Sr
(ppm)

0.65

0.62

24.34

67.54

2.27

0.54

0.88

0.022

2.77

46

54

119

109

0.44

0.70

23.90

67.50

2.30

0.62

0.95

0.026

2.70

27

59

113

103

Institute of High Energy Physics, are used to calibrate the ceramic matrix in order to obtain
reliable experimental data. The homogeneity of elements in these ceramic reference samples met
the requirements for non-destructive quantitative analysis (Li et al. 2010).
The elemental abundances of Na2O, MgO, Al2O3, SiO2, K2O, CaO, TiO2, MnO, Fe2O3, CuO,
ZnO, Rb2O and SrO are quantified by the fundamental parameter (FP) method (He and Espen
1991; Sitko 2008). This method assumes that the unknown samples have approximate compositions, and then calculates the fluorescence intensities based on the Sherman equation (Sherman
1955) and compared to the measured intensities (Lachance and Claisse 1994). Successive
adjustments of the composition are carried out until the theoretical and measured intensities are
consistent. The final concentrations are assumed to represent the actual compositions. In order to
get a better measure of the precision and accuracy of the data in this work, ancient ceramic
samples of known composition are selected to compare the expected and observed elemental
concentrations measured on the ceramic reference samples used in the analysis. The results show
that the experimental values are well in agreement with the certified ones (see Table 2).
The average values of each elemental composition in the porcelain body and glaze are
displayed below, in Tables 3 and 5, respectively. In this paper, the data for Na2O and MgO are
provided as references because of the poor fluorescent yields and low counts obtained for the
characteristic X-ray radiation.
DISCUSSION

The elemental characteristics of imperial porcelain with a Longquan celadon body

There are no evident differences between the average concentrations of SiO2, Al2O3 and MnO in
the imperial porcelain body for the HWM and YLM groups, as shown in Table 3. It can be seen
that the K2O contents in the Hongwu era of the Ming Dynasty are a little higher than those of the
Yongle era of the Ming Dynasty, while the CaO contents are lower, as can be seen in Figure 3.
The average TiO2 content in the HWM group is 0.21 0.03 % higher than that (0.14 0.02 %)
in the YLM group. The abundance change of Fe2O3 in the imperial porcelain body is similar to
that of TiO2, as shown in Figure 3. It is clearly observed that few differences exist in the major
elements of the porcelain body between the HWM and YLM groups. It is well known that in the
past, the raw material for making porcelain was obtained in the vicinity of the kiln sites.
According to the available documents (The Light Industry Hall of Zhejiang Province 1989), the
composition of Fe2O3 in the porcelain clay in the Longquan district is 0.331.24 %, which is less
than that (1.812.10 %) in the imperial porcelain body; however, the Fe2O3 content in Zijin clay
is greater than 8%, as shown in Table 4. Therefore, it seems that some Zijin clay was added: not
2014 University of Oxford, Archaeometry 57, 6 (2015) 966976

MgO (%)

0.48 0.06
0.46 0.06
0.45 0.06

Na2O (%)

0.56 0.08
0.65 0.10
0.64 0.11

Group

HWM
YLM
EM

2014 University of Oxford, Archaeometry 57, 6 (2015) 966976

20.5 0.5
20.6 0.5
20.8 0.9

Al2O3 (%)
70.4 0.7
70.7 0.8
70.6 1.2

5.36 0.31
5.20 0.42
5.19 0.48

K2O (%)
0.045 0.016
0.078 0.019
0.059 0.021

CaO (%)

0.21 0.03
0.14 0.02
0.13 0.03

TiO2 (%)
0.053 0.006
0.053 0.008
0.051 0.010

MnO (%)

2.10 0.10
1.81 0.12
1.82 0.13

Fe2O3 (%)

The average values of each composition in the bodies of the samples

SiO2 (%)

Table 3

59 6
58 5
57 6

CuO
(ppm)

101 10
107 21
104 22

ZnO
(ppm)

353 20
324 22
325 26

Rb2O
(ppm)

49 7
37 5
34 6

SrO
(ppm)

970

L. Li et al.

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Characterization by EDXRF of imperial Longquan celadon porcelain

Figure 3 The histogram of the elemental contents in K2O, CaO, TiO2 and Fe2O3 by EDXRF.
Table 4 The chemical composition of porcelain clay and Zijin clay in Dayao County of Longquan City (The Light
Industry Hall of Zhejiang Province 1989)

Porcelain
clay
Zijin clay
of Dayao
County

SiO2 (%)

Al2O3 (%)

Fe2O3 (%)

TiO2
(%)

65.4175.75

16.0023.00

0.331.24

55.70

25.24

8.18

0.69

CaO (%)

A few
per cent
1.64

MgO (%)

K2O (%)

Na2O (%)

Trace amounts

2.715.35

0.021.12

A few per cent

2.61

0.82

only can it improve the strength of the body, but it can also increase the colour density of black
or grey in the porcelain body. The average contents of the trace elements Cu, Zn, Rb and Sr were
close to each other in the HWM and YLM periods.
In this work, principal components analysis (PCA) was used to study the raw material used
for the body in different cultural periods. The main objective of PCA is to reduce the dimensionality of the observations. Figure 4 shows a factorial analysis diagram from the composition
of the imperial porcelain bodies made in the Hongwu and Yongle periods. The data for K2O,
CaO, TiO2, Fe2O3, Rb and Sr are used and the eigenvalue sum of Factors 1 and 2 accounts for
81.12% of the total variance. Factor score 1 (F1) mainly includes the changes in TiO2 and
Fe2O3, while Factor score 2 (F2) represents the K2O content. In Figure 4, the data are divided
into two clusters by variation in F1, which shows that they clearly belong to the HWM and
YLM groups, respectively. The samples of the YLM group are situated in the lower region,
while most of samples in the HWM group are located in the upper region, and only a few
overlap with the YLM samples. This also shows that the difference between the porcelain
bodies of the Hongwu and Yongle periods is mainly caused by changes in the TiO2 and Fe2O3
contents in the imperial porcelain body. However, it can be seen from F2 that the samples in the
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Figure 4 The distribution of the celadon body from the HWM and YLM periods by PCA: a plus sign (+) indicates the
celadon body of the Hongwu era of the Ming Dynasty and a triangle () represents the celadon body of the Yongle era.

HWM and YLM groups are distributed in the same area, so the concentration of K2O is not
significantly different according to the PCA results. The reason for this difference is the use of
different raw materials or differing degrees of elutriation of the same raw materials. In view of
the slightly different major element contents and the similar trace element contents, we conclude that differing degrees of elutriation of the same raw materials are the main reason for the
differences between the Hongwu and Yongle periods.
The EDXRF values for civilian porcelain bodies are also shown in Table 3. It can be seen that
the values for TiO2 and Fe2O3 in the HWM period are higher than those of the Early Ming
Dynasty (EM period), whereas the contents of other elements are similar. However, there are no
evident differences in the elemental features of the porcelain bodies in the YLM and EM groups.
Figure 5 shows the PCA factor analysis based on the chemical components in the porcelain
bodies of the HWM, YLM and EM groups. The same elements are selected as shown in Figure 4.
The eigenvalue sum of Factors 1 and 2 accounts for 77.5% of the total variance. Most of the data
in the HWM group are independently distributed in the upper region, while the samples from the
YLM and EM groups are situated in the lower region. This shows that the degree of elutriation
of the raw materials used for making imperial porcelain bodies in the Hongwu period was
different from that for the civilian porcelain bodies. The sample plots overlap each other in the
YLM and EM periods, and the data plots for the YLM period form a relatively concentrated
distribution. This means that similar processing of raw materials was used in the imperial
porcelain bodies of the Yongle period and the civilian porcelain bodies in the Early Ming
Dynasty.
The elemental characteristics of imperial porcelain with a Longquan celadon glaze
As shown in Table 5, there are no evident differences in the average concentration of each
composition in the porcelain glaze of the Hongwu and Yongle periods, and the elemental
2014 University of Oxford, Archaeometry 57, 6 (2015) 966976

Characterization by EDXRF of imperial Longquan celadon porcelain

973

Figure 5 The analytical results of PCA on porcelain bodies of the HWM, YLM and EM periods: a plus sign (+) indicates
the celadon body of the Hongwu era of the Ming Dynasty, a triangle () represents the celadon body of the Yongle era
and an asterisk (*) represents the civilian porcelain body of the Early Ming Dynasty.

values of the porcelain glaze are close to each other in the imperial and civilian porcelain.
According to the documentary evidence (Peng et al. 2009), the recipe for the glaze is made up
from plant ash and porcelain stone. From the perspective of the chemical composition of the
glaze, there are no obvious differences in the imperial porcelains, so the raw materials of the
imperial porcelain glaze of the Hongwu and Yongle periods are unchanged and have an inheritance relationship.
The quality and formula changes of the Longquan celadon glazes varied over time (Li 1998).
During the Southern Song Dynasty, the quality of the celadon glaze had been significantly
improved, and the very famous Fen ching (lavender grey) and Meizi ching (plum green) had been
created (Li 1998). However, the colour of the Longquan imperial porcelain in the Ming Dynasty
was mainly yellowgreen (see Fig. 2). So, what changes in the imperial porcelain glaze had taken
place as compared with that of the Southern Song Dynasty? The formation of the glaze colour is
related to many factors, and the major influences are the recipe, the glazing craft and firing
temperature, and so on. In this paper, the data of Fen ching and Meizi ching (Li 1998; Xiong et al.
2004) for the Longquan glazes dating from the Southern Song Dynasty are compared with the
analytical results obtained by EDXRF for the imperial porcelain samples of the Ming Dynasty.
As shown in Table 6, the average K2O contents of the Fen ching and Meizi ching glazes
(4.005.36 %) were lower than those for the imperial porcelain samples (5.785.83 %) in the
Ming Dynasty, while the change of concentration for CaO was opposite to that for K2O. In the
ceramics, K2O and CaO are often referred to the flux, which was used to reduce the firing
temperature of the body and glaze. The difference is that the fluxing ability of K2O is stronger
than that of CaO. In addition, the glossiness of the glaze is closely related to the oxide content
with a high refractive index, the content of the flux and the glass phase (Zhang 1998). Increasing
the chemical composition of K2O is advantageous for improving the refractive index of the glaze
layer, reducing the firing temperature and the high-temperature viscosity of the glaze and
2014 University of Oxford, Archaeometry 57, 6 (2015) 966976

MgO (%)

0.67 0.16
0.67 0.11
0.63 0.14

Na2O (%)

0.47 0.13
0.59 0.13
0.50 0.13

Group

HWM
YLM
EM

2014 University of Oxford, Archaeometry 57, 6 (2015) 966976

12.3 1.2
13.0 1.1
12.7 1.2

Al2O3 (%)
69.4 3.4
69.2 1.9
69.7 2.6

SiO2 (%)

Table 5

5.78 0.82
5.83 0.32
5.84 0.69

K2O (%)
7.80 2.05
7.25 1.79
7.31 2.10

CaO (%)

0.18 0.03
0.18 0.04
0.17 0.03

TiO2 (%)
0.31 0.09
0.35 0.07
0.32 0.08

MnO (%)

2.16 0.13
2.17 0.26
2.06 0.30

Fe2O3 (%)

The average values of each composition in the sample glaze

73 8
74 8
68 9

CuO
(ppm)

140 40
124 36
112 44

ZnO
(ppm)

291 18
296 16
286 24

Rb2O
(ppm)

547 125
509 95
568 144

SrO (ppm)

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Characterization by EDXRF of imperial Longquan celadon porcelain

975

Table 6 The data of Fen ching and Meizi ching for Longquan glaze
dating from the South Song Dynasty (Li Jiazhi 1998; Xiong Yingfei 2004)

K2O (%)

CaO (%)

TiO2 (%)

Fe2O3 (%)

Fen ching (lavender grey)

4.87
8.39
5.06
9.94
4.53
7.95
4.25
10.7

0.07
0.06

0.95
1.1
1.54
1.29

Meizi ching (plum green)

4.41
9.88
5.36
9.05
4.12
9.21
4.00
9.99

0.06
0.08

0.91
1.32
0.82
1.68

increasing liquid formation at high temperature. Compared with Fen ching and Meizi ching in the
Southern Song Dynasty, the increased K2O content in the imperial porcelain glaze of the Ming
Dynasty gives a glaze with good transparency and gloss.
In Tables 5 and 6, it can be also seen that the TiO2 and Fe2O3 contents of the imperial porcelain
glaze of the Ming Dynasty are higher than those of the Southern Song Dynasty. The colour of
celadon glaze mainly depends on the Fe2O3 content and on the firing temperature and atmosphere.
The high levels of Fe2O3 in imperial porcelain make the glaze take on a yellowgreen colour, as
shown in Figure 2.
According to the available documents, imperial porcelain began to be fired at the Fengdongyan
kiln in the Hongwu era (ad 13681398) of the Ming Dynasty (Zhejiang Institute of Cultural
Relics et al. 2009). As is known, in ancient times the best-quality porcelain was dedicated for
palace use. In this work, the results of the analysis show that the raw materials for both the body
and the glaze of the imperial porcelain are similar to those of civilian porcelain. Therefore, we can
conclude that the production and firing technology of Longquan celadon had reached a higher
level and did not decline in the Early Ming Dynasty.

CONCLUSION

In this paper, EDXRF has been applied to analyse the elemental composition of Longquan
imperial porcelain that was fired at the Fengdongyan kiln in the Hongwu (ad 13681398) and
Yongle (ad 14021424) eras of the Ming Dynasty. The elemental contents of TiO2 and Fe2O3 in
the body vary in the different cultural periods. Compared with Longquan glaze dating from the
Southern Song Dynasty (ad 11271279), the average values for K2O, Fe2O3 and TiO2 are higher,
but the CaO content is lower in the imperial porcelain glaze. The PCA results show that the degree
of elutriation of the raw material used for making the imperial porcelain body in the Hongwu
period was different from that of the civilian porcelain, but the Yongle body is similar to that of
the civilian porcelain in the Early Ming Dynasty. However, the raw materials of the imperial
porcelain glaze of the Hongwu and Yongle periods show no obvious change and show an
inherited relationship. The production and firing technology of Longquan imperial celadon had
not declined in the Early Ming Dynasty.
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ACKNOWLEDGEMENTS

The authors greatly appreciate the Zhejiang Province Institute of Cultural Relics and Archaeology, which provided ancient Chinese celadon excavated from the Fengdongyan site of the
Longquan kiln. This work was financially supported by the National Natural Science Foundation
of China (11205167, 11305183 and 11175190).
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2014 University of Oxford, Archaeometry 57, 6 (2015) 966976