Difference between revisions of "CI 10305, Picric Acid, LC"

From CAMEO
Jump to: navigation, search
(Molecular Information)
(Chromatograms)
 
(8 intermediate revisions by the same user not shown)
Line 19: Line 19:
 
== Analytical instrumentation and procedures ==
 
== Analytical instrumentation and procedures ==
  
Dyes were extracted from textiles (silk or wool) using formic acid/methanol (5:95, v/v).
+
'''Extraction''':  The extraction was carried out as follows: a small sample of thread was extracted with the TFA 2M in 1.5ml eppendorfs for 30 min, in 60ºC water bath, with constant agitation. After extraction, each extract was dried in a vacuum system, where the resulting dry residues were reconstituted with 50 μl H2O: MeOH (80:20,v/v).  
  
HPLC column: Vydac 214TP52 analytical column (2.1 mm diameterX250 mm; 5-ím particle size).
 
  
HPLC-DAD-MS instrument: HPLC-DAD-MS analysis was performed with an Agilent 1100 liquid chromatography system consisting of an automatic injector, a gradient pump, a HP series 1100 DAD, and an Agilent series 1100 VL on-line atmospheric pressure ionization electrospray ionization mass spectrometer.  
+
'''HPLC system''': The dye analyses were performed in a Thermofinnigan Surveyor HPLC-DAD system with a Thermofinnigan Surveyor PDA 5 diode array detector (Thermofinnigan, USA), an autosampler and a pump.  
  
HPLC gradient profile: Separations were done on a  The column was eluted at a flow rate of 0.2 mL/min with a tertiary gradient of water (A),acetonitrile (B), and 1% (v/v) aqueous formic acid (C) with the following elution program: 0 min, 90% A, 5% B, 5% C; 0-55 min, a linear gradient to 35% A, 60% B, 5% C; 55-60 min, a linear gradient elution to 15% A, 80% B, 5% C; 60-62 min, isocratic elution at 15% A, 80% B, 5% C; 62-70 min gradient elution to 90% A, 5% B, 5% C; and reequilibration with the latter solvent for 15 min. The mass spectrometer was run both in the negative ion mode because metanil Yellow is negatively charged without Na+.
+
'''HPLC Column''': The separations were performed in Zorbax Eclipse Plus C18 (Agilent, USA) with 5μm particle size column (2.1 mm x 150 mm). The column was kept at controlled temperature (35ºC). The samples were injected onto the column via a Rheodyne injector with a 25μl loop.
 +
 
 +
'''LC program''': A solvent gradient of (A) TEA pH= 6,4 3mM and (B) pure methanolwas used at a flow rate of 0.3 mL/min; 0-0,01min A:B (95:5) isocratic, 5 min A:B (90:10) isocratic, 10 min A:B (70:30) isocratic, 15 min A:B (50:50) isocratic, 30 min A:B (45:55) isocratic, 35 min A:B (30:70) isocratic, 45-55 min A:B (5:95) linear, 60-70 min A:B (95:5) linear.
 +
 
 +
'''LC-DAD-MSn''': The analyses of dyes were performed on a LC-MS with ProStar 410 autosampler, two 212-LC chromatography pumps, a ProStar 335 diode array detector and a 500-MS ion trap mass spectrometer with an electrospray ionization (ESI) ion source (Varian, Palo Alto, CA, USA). Data acquisition and processing were performed using Varian MS Control 6.9 software.The separations were carried out using a Zorbax Eclipse Plus (Agilent, USA) with 5 μm particle size column (2.1 mm x 150 mm). The column was kept at controlled temperature (35ºC). The samples were injected onto the column via a Rheodyne injector with a 20 μL loop. The gradient adapted from and described in 2.3.1 was used at a flow rate of 0.2 mL/min. The mass spectra were acquired in negative and positive mode depending on the structures. The optimized parameters were as follows: ion spray voltage,  4,8 kV; capillary voltage, 20 V; RF loading 80%. Nitrogen was used as nebulising and drying gas, at a pressure of 35 and 15 psi; drying gas temperature, 300ºC. The multistage MS (MSn) spectra were obtained with an isolation window of 2.0 Da, excitation energy values of 0,9 to 1,5 V and an excitation time of 10 ms.
 +
 
 +
[1]
  
 
= Chromatograms =
 
= Chromatograms =
  
  
[[File:Picric Acid LC.PNG|center|frame|Absorbance at 347nm (mAU)[1]]]
+
[[File:Picric Acid LC.PNG|center|frame|Absorbance at 347nm (mAU), By Cátia Souto, University of Lisbon, Portugal 2010.[1]]]
  
  
 
== Results ==
 
== Results ==
  
[[File:Picric acid result.PNG|center|frame|compounds identified]]
+
[[File:Picric acid result1.PNG|center|frame|compounds identified]]
  
 
== References ==
 
== References ==

Latest revision as of 09:59, 4 October 2017

Usage History

Picric acid

Synonyms

C.I. 10305; 2,4,6-trinitrophenol; 1,3,5-Trinitrophenol.

Molecular Information

Picric acid Hazards

Molecular Formula C6H3N3O7

Molecular Weight 229.1 g/mol

Picric acid.png

Analytical instrumentation and procedures

Extraction: The extraction was carried out as follows: a small sample of thread was extracted with the TFA 2M in 1.5ml eppendorfs for 30 min, in 60ºC water bath, with constant agitation. After extraction, each extract was dried in a vacuum system, where the resulting dry residues were reconstituted with 50 μl H2O: MeOH (80:20,v/v).


HPLC system: The dye analyses were performed in a Thermofinnigan Surveyor HPLC-DAD system with a Thermofinnigan Surveyor PDA 5 diode array detector (Thermofinnigan, USA), an autosampler and a pump.

HPLC Column: The separations were performed in Zorbax Eclipse Plus C18 (Agilent, USA) with 5μm particle size column (2.1 mm x 150 mm). The column was kept at controlled temperature (35ºC). The samples were injected onto the column via a Rheodyne injector with a 25μl loop.

LC program: A solvent gradient of (A) TEA pH= 6,4 3mM and (B) pure methanolwas used at a flow rate of 0.3 mL/min; 0-0,01min A:B (95:5) isocratic, 5 min A:B (90:10) isocratic, 10 min A:B (70:30) isocratic, 15 min A:B (50:50) isocratic, 30 min A:B (45:55) isocratic, 35 min A:B (30:70) isocratic, 45-55 min A:B (5:95) linear, 60-70 min A:B (95:5) linear.

LC-DAD-MSn: The analyses of dyes were performed on a LC-MS with ProStar 410 autosampler, two 212-LC chromatography pumps, a ProStar 335 diode array detector and a 500-MS ion trap mass spectrometer with an electrospray ionization (ESI) ion source (Varian, Palo Alto, CA, USA). Data acquisition and processing were performed using Varian MS Control 6.9 software.The separations were carried out using a Zorbax Eclipse Plus (Agilent, USA) with 5 μm particle size column (2.1 mm x 150 mm). The column was kept at controlled temperature (35ºC). The samples were injected onto the column via a Rheodyne injector with a 20 μL loop. The gradient adapted from and described in 2.3.1 was used at a flow rate of 0.2 mL/min. The mass spectra were acquired in negative and positive mode depending on the structures. The optimized parameters were as follows: ion spray voltage,  4,8 kV; capillary voltage, 20 V; RF loading 80%. Nitrogen was used as nebulising and drying gas, at a pressure of 35 and 15 psi; drying gas temperature, 300ºC. The multistage MS (MSn) spectra were obtained with an isolation window of 2.0 Da, excitation energy values of 0,9 to 1,5 V and an excitation time of 10 ms.

[1]

Chromatograms

Absorbance at 347nm (mAU), By Cátia Souto, University of Lisbon, Portugal 2010.[1]


Results

compounds identified

References

[1] Cátia Susana da Costa Nogueira Souto, "Analysis of Early Synthetic Dyes with HPLC-DAD-MS An important database for analysis of colorants used in cultural heritage", Thesis, Master Degree in Conservation and Restoration of Textiles. UNIVERSIDADE NOVA DE LISBOA, 2010.