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HAL Id: jpa-00219640

https://hal.archives-ouvertes.fr/jpa-00219640

Submitted on 1 Jan 1980

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MÖSSBAUER SPECTROSCOPY STUDY OF IBERIAN POTTERY

J. Gancedo, M. Gracia, A. Hernández

To cite this version:

J. Gancedo, M. Gracia, A. Hernández. MÖSSBAUER SPECTROSCOPY STUDY OF IBERIAN POTTERY. Journal de Physique Colloques, 1980, 41 (C1), pp.C1-401-C1-402.

�10.1051/jphyscol:19801154�. �jpa-00219640�

(2)

JOURNAL DE PHYSIQUE

Colloque

C l

, supplkment au n

O 1,

Tome

41,

janvier

1980,

page

C1-40 1

&SBAUER SPECTROSCOPY STUDY OF IBERIAN POTTERY

J.R. Gancedo, M. G r a c i a and A. ~ e r n ~ n d e z *

I n s t i t u t o de Quimica F i s i c a "RocasoZano" C.S.

I . C.

C/Serrano,

119,

Madrid-6, Spain

x

I n s t i t u t o GeoZ6gico y Minero de Esp&

C/

Rios Rosas,

23,

Madrid-3, Spain

I n t r o d u c t i o n . - Mossbauer Spectroscopy (MS) has o f Fe2+ and a magnetic s e x t e t w i t h a h y p e r f i n e f i - been used w i t h good r e s u l t s f o r t h e s t u d y o f archaeo e l d of 491 t 4 KG, weaker than found the l o g i c a l ceramics, because t h e parameters o b t a i n e d I t G I 1 and UP11 groups.

from t h e s p e c t r a can be c o r r e l a t e d w i t h t h e prove-

nance (11, f i r i n g technique (2,3) and d a t e o f manu- llP1l P o t t e r y "GV P o t t e r y "H" P o t t e r y ( 5 s a m p l e s ) ( 5 s a m p l e s ) (5 samples) f a c t u r e of t h e sherds (1, 4 ) .

The aim of t h i s work i s t o e s t a b l i s h evidence o f Fe3+(non-mag.)

p o s s i b l e d i f f e r e n c e s i n p r o v e n a n c e a n d f i r i n g t e c h - QS (mm/s) 0 , 9 9 ? 0 , 0 9 1,OOf 0,03 1,13'0,08 n i q u e f o r t h r e e types o f I b e r i a n ceramics ( 4 t h ten- I S (mm/s) 0,34

?

0901 0934 0902 0 9 3 6 0702 t u r y BC) p i c k e d up from t h e same l a y e r o f the a r - Fe2+(si t e I )

c h a e o l o g i c a l e x c a v a t i o n o f Lora d e l R i o (Sevi 1 le )

.

QS (mm/s) 2,19

f

0,03 2,30

2

0,04 2,36

2

0,06 Two more techniques, Atomic A b s o r p t i o n Spectroscopy IS (mm/s) 1,12

t

0,03 1,17 f 0,02 1,10

+

0,03

(AAs) and X-Ray D i f f r a c t i o n (X-RD), were used i n o r F e Z + ( s i t e 11)

-

QS (mm/s) 1,89 1,74

f

0,14

der t o complement t h e MS.

-

I S (mm/s) 0,98' 0,87

f

0,08

-

Three groups o f ware have been s t u d i e d , two o f

thrown p o t t e r y ( r e d p a i n t e d ("P") and g r e y ( 1 1 ~ 1 ~ ) ) Magnetic part

and one o f hand-made p o t t e r y ("H1l). QS (mm/s) -0,04 ? 0,06 0,03

2

0,06 -0,14 f 0,04 IS (mm/s) 0,43 f 0,03 0,35 ",05 0,39 2 0,04 Experimental

.-

Transmission s p e c t r a were o b t a i n e d H e f f (KG) 509

'

499 ? 2 491

f

4

a t room temperature i n a double-symmetrical-ramp 'mag'' t o t 0,21 f 0,02 0,16 2 0,06 0,19 2 0,03 512-channel spectrometer, and computer f i t t e d t o IFn2+/IFe3+ 0 , 3 2 2 0,26 1 , 5 5 + 0,43 0,20

f

0,13

. - . -

sum o f L o r e n t z i a n l i n e s . The absorber w e i g h t was

250-300 mg o f ground ceramic, s u f f i c i e n t t o y i e l d ,

-

Table I . - Mossbauer parameters f o r samples o f I b e approximately, 5 mg/cmz de Fe. r i a n p o t t e r y ( I S r e l a t i v e t o i r o n m e t a l ) .

The c o n c e n t r a t i o n s o f t h r e e c a t i o n s , A l , Fe and

Mg, were determined by AAS, by means o f a 360 Per- I n s p e c t i o n o f t a b l e I a l l o w s one t o conclude t h a t kin-Elmer spectrometer. t h e c l a y o f t h e hand-made ceramics i s w e l l d i f f e r e l l

The X-RD m i n e r a l o g i c a l study was done w i t h a P h i - l l i p s d i f f r a c t o m e t e r , model PW 1130/00.

R e s u l t s and d i s c u s s i o n . - The most r e l e v a n t MS pa- rameters a r e i n c l u d e d i n t a b l e I.

A l l t h e llP1l ceramics b u t one y i e l d s p e c t r a which can be f i t t e d t o a Fe3+ ( o c t a h e d r a l ) d o u b l e t , a mas n e t i c s e x t e t ( ~ r o b a b l ~ o f o x i d e ( 3 ) ) and a FeB(oc- t a h e d r a l ) d o u b l e t . One o f these s p e c t r a i s shown i n f i g u r e 1.

The o t h e r "P" sample, w i t h t h e h i g h e s t Fe2+ con-

t i a t e d from t h a t o f t h e thrown p o t t e r y . The sample w i t h "black-core1' i s s p e c i a l l y r e v e a l i n g because

i t s parameters (Fe2+si t e I : QS = 2,32 IS = 1,23;

~ e ~ + s i t e l I : QS = 1 ,89 mm/s, 1 S = 0,98 mm/s; 1 Fe2+/

IFe3+ = 0,68) appear t o be between those o f t h e "GI1 and "P" samples. I t can be suggested t h a t t h e n o t t o o l a r g e d i f f e r e n c e s between t h e s p e c t r a o f t h e g r e y and p a i n t e d samples i s due t o t h e d i f f e r e n t f i r i n g technique; p r o b a b l y t h e g r e y samples were f i - red i n a high1 y reducing atmosphere ( 2 ) .

The AAS a n a l y s i s ( t a b l e I I ) c o n f i r m t h i s hypothe- t e n t and a marked "black-core", and t h e whole group s i s , as t h e r e a r e no s e n s i b l e c o n c e n t r a t i o n d i f f e - o f "G" ceramics show s p e c t r a ( f i g u r e 2) which can rences between t h e "Pat and "GI' groups, w h i l e t h e be f i t t e d t o a Fe3+ d o u b l e t s i m i l a r t o t h a t o f t h e c o n c e n t r a t i o n s f o r t h e "Hal samples a r e q u i t e d i f f e

"P" samples, a magnetic s e x t e t and two Fe2+ s i t e s . r e n t .

The "H" group e x h i b i t s one s i t e o f Fe3+, another The X-RD r e s u l t s ( t a b l e I I I ) show t h e presence o f

Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:19801154

(3)

C

1

-402

JOURNAL DE PHYSIQUE

m a g n e t i c s e x t e t

I I I I I I

:

-

Fez*

-8 - 6 -4 - 2 0 2 4 6 8

I I I I I I I I I

m m l s F i g u r e 1.- Spectrum o f r e d p a i n t e d ceramic.

c a l c i t e among o t h e r m i n e r a l s i n t h e "P" and "G1' sa!

p l e s ; i t i s h i g h e r i n t h e "G1' samples. I n t h e "P"

sample w i t h ' l b l a c k - c o r e " t h e i n n e r p a r t c o n t a i n s a h i g h e r c o n c e n t r a t i o n o f c a l c i t e w h i c h c o r r e l a t e s w i t h t h e h i g h e r c o n c e n t r a t i o n o f ~ e seen by MS. ~ +

"PI1 P o t t e r y "GI1 P o t t e r y "H" P o t t e r y

% Fe 3,98 f 0,16 3,96

f

0,15 4,5 f 0,8

% A1 7,52

2

0,67 7,47 f 0,68 9,6 f 1,2

% Mg 1,28 f 0,12 1,24 f 0,06 1,3 f 0,6 T a b l e I 1 . - AAS a n a l y s i s r e s u l t s ( i n r e l a t i v e con- c e n t r a t i o n ) .

"P" P o t t e r y "6" P o t t e r y "HI1 P o t t e r y

Micas 1 1 v h

Q u a r t z v h v h v h

C a l c i t e 1 h

-

K - f e l de:;p. h h v h

P l a g i o c l . h h v h

( v h = v e r y h i g h , h = h i g h , 1 = low,

-

= n o t found) T a b l e 1 1 1 . - X-RD m i n e r a l o g i c a l a n a l y s i s .

References

( 1 ) KOSTIKAS, A., SIMOPOULOS, A. and GANGAS, N. H., J. Physique Col l o q . 35 (1974) C6-537.

(2) BOUCHEZ, R., COEY, J . M. D., COUSSEMENT, R., SCHMIDT, K. P., VAN ROSSUM, M., APRAHAMIAN, J. and DESHAYES, J., J. Physique C o l l o q . 35 (1974) C6-541.

, >

I

I

0 : ~ e ~ + ( s i t e I ) C : ~ e ~ * ( s i t e 11) 0 : magnetic sixtet

-8 -6 -4 -2 0 2 4 6 8

I I

m m l s F i g u r e 2.- Spectrum o f g r e y ceramic.

On t h e o t h e r hand, a p i e c e o f g r e y c e r a m i c h e a t e d a t 850°C c o v e r e d w i t h c h a r c o a l i n N2 atmosphere l o s t t h e c a l c i t e c o m p l e t e l y i n a c o u p l e o f h o u r s w i t h a s u b s t a n t i a l i n c r e a s e o f t h e b l a c k c o l o u r .

A l l t h e e v i d e n c e s exposed l e a d t o t h e c o n c l u s i o n s t h a t t h e "Go' and "Pol c e r a m i c s were f i r e d a t tempe- r a t u r e s around 800°C w h i c h i s a compromise between t h e e x i s t e n c e o f c a l c i t e and t h e v a l u e o f ~ e 3 + QS (2, 3 ) .

The "HI1 samples do n o t c o n t a i n c a l c i t e b u t con- t a i n i l l i t e , m i n e r a l w h i c h decomposes a r o u n d 850°C ( 5 ) . The low Heff = 491 f 4 KG can be a s c r i b e d t o s u b s t i t u t i o n a l i m p u r i t i e s o f t h e m i n e r a l

( 3 ) ,

w h i c h c o n f i r m s t h e d i f f e r e n t provenance o f t h e c l a y s .

Acnow1edgement.- One o f us (M.G.) has been suppo_r t e d by a Fundaci6n Juan March g r a n t . We a r e indeb- t e d by Dr. J. Remesal who p r o v i d e d us w i t h t h e sherds.

(3) JANOT, Ch., and DELCROIX, P., J . Physique C o l l o q . 35 (1974) C6-557.

(4) GANGAS, N. H., SIGALAS, I . and MOUKARIKA, A., J. Physique Col l o q . 37 (1976) C6-867.

(5)

The X-ray i d e n t i f i c a t i o n and c r y s t a l s t r u c t u - r e s o f c l a y m i n e r a l s . Brown G. ( E d i t o r ) (Ja r r o l d and Sons L t d . , ~ o r w i c h ) (1963) p.232.

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