Investigation of samples dyed with Weld

1
Investigation of samples dyed with Weld Ioannis
Karapanagiotis and Violaine de Villemereuil    "OR
MYLIA" ART DIAGNOSIS CENTRE SACRED CONVENT OF THE
ANNUNCIATION IMSP EU-ARTECH meeting May
26-28, 2005, Ormylia
2
Protocol

• Sample treatment
• Sample (2-4mg) in H2OMeOH37 HCl (112, v/v)
  for 10 minutes at 1000C.
• Solution is evaporated to dryness by heating
  (60oC) under gentle nitrogen flow.
• Dry residue is dissolved in 300µl of DMF. If
  necessary, further dilution takes place.
• A volume of 20µl is submitted to HPLC analysis.

HPLC analysis ColumnXTerra C18 5µm 3.0 x 250mm,
thermostatted at 30oC. Reodyne 7725i Injector
with 20µl sample loop Gradient elution of
H2O-0.1TFA and CH3CN-0.1TFA. Flow rate 5ml/min

3
Results
Mordanted silk
Mordanted wool
4
Results
Sample2.9mg Dilution in DMF300µl Further
dilution Yes 1/3
Dyed wool Dye bath 1 (WITH potash)
250nm
5
Results
Sample3.7mg Dilution in DMF300µl Further
dilution Yes 1/3
Dyed wool Dye bath 2 (NO potash)
250nm
6
Results
Sample2.7mg Dilution in DMF300µl Further
dilution Yes 1/15
Dyed silk Dye bath 3 (WITH potash)
250nm
7
Results
Sample2.9mg Dilution in DMF300µl Further
dilution Yes 1/3
Dyed silk Dye bath 4 (NO potash)
250nm
20.54
100
80
60
Relative Absorbance
40
21.73
20
21.92
0
6
8
10
12
14
16
18
20
22
24
26
28
30
32
34
Time (min)
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Results
4 Samples1-2mg Dilution in DMF600µl Further
dilution No
Dyed wool (dye bath 1) quadruple analysis
270nm
270nm
270nm
270nm
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Results
Sample3.2mg Dilution in DMF500µl
Type 1 pigment lime water, then alum/CaCO3
10
Results
Sample4.2mg Dilution in DMF500µl
Type 2 pigment chalk/alum
11
Results
Type 3 pigment K2CO3/alum
Sample3.5mg Dilution in DMF500µl
12
Results
Plant material
1. NO HCl treatment
2. Standard HCl treatment