AN 360: Rapid Determination of Azo Dyes in Textiles Using ... - Dionex

asE condItIons
Preheat: 20 min (purge closed)
Pressure: 1500 psi
Static Time: 5 min
Temperature: 100 °C
Cycles: 2
Purge Time: 100 s
Flush Volume: 30%
Solvent: 90% MeOH with 10% 1 M KOH
Extraction Time
per Sample: 40 min
Solvent Amount Used
per Sample: 17 mL
analytIcal condItIons
Column: Acclaim ® 120 C18 3 µm 120 Å
2.1 x 150 mm
Eluent: H O/5%, CH CN/4%, CH OH
2 3 3
H O/40%, CH CN/45% CH OH
2 3 3
Column Temperature: 30 °C
Flow Rate: 250 µL/min
Injection Volume: 10 µL
UV: 240 nm, 278 nm
Ionization Mode: APCI, positive polarity
Nitrogen: 3 bar
Corona Current: 10 µA
Source Temperature: 400 °C
Cone Voltage: Varies by analyte (See Table 1.)
SIM Mode: m/z by analyte (See Table 1.)
Dwell Time: 0.3 s
Span: 0.3 m/z
Sample Prep
Soak 1 g of material in 3 mL citrate buffer
(pH 6.0) and 3 mL sodium dithionite (200 mg/mL) for
2 min. Transfer the mixture and solution to an ASE 11 mL
cell containing a glass fiber filter.
Extraction
Place the extraction cells into the ASE 200 carousel,
and extract using the ASE conditions listed above. Record
total volume of the extract, and inject 10 µL onto the
UltiMate 3000 HPLC/MS/UV system.
LC Conditions
Time Flow
Rate
(µL/min)
30 mM
Ammonium
Acetate, pH 4
Acetonitrile Methanol Curve
0.00 250 91 5 4
25.00 250 69 27 4 5
40.00 250 52 40 8 5
45.00 250 15 40 45 5
48.00 250 15 40 45 5
48.10 250 91 5 4 5
30 mM Ammonium Acetate, pH 4.0
Weigh 2.31g NH OAc (FW 77.0825 g/mol). Add 1000
4
mL H O. Adjust pH to 4.0 with acetic acid.
2
2 Rapid Determination of Azo Dyes in Textiles Using Dionex ASE and UltiMate 3000 HPLC Systems