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Purospher® - High-purity HPLC columns

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Separation of explosives from drinking water

LiChroCART® 250-4 Purospher® RP-18 HC, 5 μm
Mobile phase A: Acetonitrile / Methanol; 20 / 80, v/v
B: Sodium dihydrogenphosphate buffer (c = 0.01 mol/L, pH 4.5)
Gradient 0 min 35 % A; 28 min 55 % A; 40 min 85 % A; 50 min 85 % A; 51 min 35 % A; 71 min 35 % A
Flow rate   0.8 mL/min
Detection DAD 210 and 235 nm
Temperature 36 °C
In. volume 40 μL
Sample

1. Octogen (HMX)
2. Picric acid
3. Hexogen (RDX)
4. Ethylene Glycol Dinitrate (EGDN)
5. Diethylene Glycol Dinitrate (DEGN)
6. 1,3,5-Trinitrobenzene
7. 1,3-Dinitrobenzene
8. Tetryl
9. Nitroglycerine


10. 2,4,6-Trinitrotoluene
11. 4-Amino-2,6-dinitrotoluene
12. 2-Amino-4,6-dinitrotoluene
13. 2,6-Dinitrotoluene
14. 2,4-Dinitrotoluene
15. 2-Nitrotoluene
16. 4-Nitrotoluene
17. 3-Nitrotoluene
18. Nitropenta (PETN)
19. Hexyl

LiChroCART® 250-4 Purospher® RP-18 HC, 5 μm
Sample preparation
Solid phase extraction with LiChrolut® EN (200 mg) (Cat. No. 1.19870):
Solvents A: Methanol (LiChrosolv® Cat. No. 1.06007),
B: Acetonitrile (LiChrosolv® Cat. No. 1.00030);
C: Water (LiChrosolv® Cat. No. 1.15333).
Sample pretreatment Filtrate if necessary and add approx. 5 g NaCl / 1L water sample.
Conditioning of extraction column: 3 mL A, 3 mL B, 10 mL C, do not allow column to dry out!
Sample application pass 1 L water sample through the extraction column within 1 hour by using LiChrolut® extraction unit (Cat. No. 1.19851) which is connected to the water sample reservoir with PTFE hose (Cat. No. 1.22143) and a steel capillary.
Drying step 10 min by means of nitrogen and LiChrolut® drying unit (Cat. No. 1.19852).
Elution step 1 x 2 mL, then 1 x 3 mL A/B (1:1), collect in a conical flask and gently evaporate the solvent by means of nitrogen up to a and volume of 0.5 mL. Fill up to 1.0 mL with C. Subsequently filtrate sample into a 1.5 mL sample vial through a 0.2 μm membrane filter.

© Merck KGaA, Darmstadt, Germany, 2013

All references to Merck refer to Merck KGaA, Darmstadt, Germany.


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