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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction resin-based sorbents.

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Presentation on theme: "ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction resin-based sorbents."— Presentation transcript:

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2 ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction resin-based sorbents

3 Resin vs. Silica Sorbents * Methacrylate - ester hydrolyzes at high pH Silica Resin Stability (pH)limited (2-8) broad (0-14) * Interactionsmultiple primarily hydrophobic Capacity1-5% up to 50% Selectivityhigh low Conditioningrequired sometimes required

4 Why Use Resin-Based Sorbent? v Increased surface area ( ~ 1100 m 2 /g ) v Decreased bed size v Extract a wide range of polarities v Resistant to pH extremes

5 Types of ISOLUTE Resins ISOLUTE ENV+ Hydroxylated Polystryrene Divinylbenzene OH CH-CH 2 - -CH-CH 2 -CH-CH 2 - C-CH 2 - CH-CH 2 - -CH-CH 2 - HO OH HO C-CH 2 - CH-CH 2 - -CH-CH 2 -CH-CH 2 - CH-CH 2 - -CH-CH 2 - ISOLUTE 101 Polystryrene Divinylbenzene HO

6 PolyvinylpyrrolidonePolyvinylpyrrolidone N CH - CH 2 O N O

7 Polyamide (Nylon) R NHNH R’ NHNH R NHNH NHNH O O O O

8 MethacrylateMethacrylate C=O CH 2 - CH O CH 3 CH 2 - CH O=C O CH 3

9 WettabilitiesWettabilities NameWettability sinks (5-10 sec) sinks (20-30 sec) sinks (>1 min) sinks (<5 sec) floats (5-10 sec) floats (>1 min) floats (<5 sec) floats (5-10 sec) ISOLUTE ® ENV + (Hydrox PSDVB) Lichrolut EN (Hydrox PSDVB) MCI CQP (methacrylate) ISOLUTE ® 10Y (Polyamide) Tosohaas HW (methacrylate) Spe-ed RP105 Reillex HP (Polyvinylpyrrolidone) ISOLUTE ® 10Z (PSDVB) Bond-Elut ENV ISOLUTE ® 101 (PSDVB) Oasis HLB (divinylbenzene co) ISOLUTE ® 10W (PSDVB) Bond-Elut PPL (PSDVB bromin) ISOLUTE ® 10X (PSDVB)

10 SwellingSwelling Swelling (acetone) none observed 20-30% none observed 20-30% 5-10% 20-30% 5-10% 20-30% 10-20% none observed Name ISOLUTE ® ENV + (Hydrox PSDVB) Lichrolut EN (Hydrox PSDVB) MCI CQP (methacrylate) ISOLUTE ® 10Y (Polyamide) Tosohaas HW (methacrylate) Spe-ed RP105 Reillex HP (Polyvinylpyrrolidone) ISOLUTE ® 10Z (PSDVB) Bond-Elut ENV ISOLUTE ® 101 (PSDVB) Oasis HLB (divinylbenzene co) ISOLUTE ® 10W (PSDVB) Bond-Elut PPL (PSDVB bromin) ISOLUTE ® 10X (PSDVB)

11 Physical Characteristics Name Avg Particle Size Surface Area ENV+ Lichrolut EN MCI CQP (methacrylate) ISOLUTE 10Y Tosohaas HW (methacrylate) Spe-ed RP105 Reillex HP (PVP) ISOLUTE 10Z Bond-Elut ENV ISOLUTE 101 Oasis HLB ISOLUTE 10W Bond-Elut PPL ISOLUTE 10X >

12 Capacity versus Surface Area Surface Area (m 2 ) Caffeine Capacity mg/g Reillex HP (PVP) 10 Z BondElut PPL 10 X 101 ENV+ Lichrolute BondElut Env Oasis HLB

13 ISOLUTE ENV+ Sorbent v Polystyrene Divinylbenzene Polymer v High Surface Area ( ~ 1100 m2/g ) v Highly Crosslinked v Narrow Particle Size Distribution ä Reproducible flow characteristics ä High sample flow rates v Fines Free (trouble-free analysis)

14 Problem Analytes v Polar v Water soluble v Unretained on non-polar silica based sorbents v Applications requiring “salting out”

15 PhenolsPhenols Average recovery of phenols on C18(EC)... < 50 % !

16 Extraction of Phenols 1. Sample pre-treatment 2. Column solvation 3. Column equilibration 4. Sample application 5. Interference elution 6. Analyte elution pH = 2 Methanol Water at pH = 2 One liter Deionized water Methanol ISOLUTE ENV+, 150 mg / 3 mL and 200 mg/6 mL

17 Recovery of Phenols Flow Rate Analyte Phenol Chlorophenol ,4-Dichlorophenol ,4,6-Trichlorophenol mL / min 60 mL / min (150 mg/3 mL) (200 mg/6 mL)

18 Extraction of Explosives Sample pre-treatment Column conditioning Column equilibration Sample application Interference elution Analyte elution None THF ( 2 mL soak 4 min, then 4 mL) 4 mL water 30 mL/min + Bottle Rinse (10 mL MeOH, 10 mL water) (10 mL MeOH, 10 mL water) 10 mL water, 10 min N 2 or CO 2 Two x 1.5 mL ACN

19 Recovery of Explosives 1,3-Dinitrobenzene Tetryl Nitrobenzene TNT 2-Nitrotoluene 4-Nitrotoluene 3-Nitrotoluene Average Sample volume: 1 liter Analyte conc: 0.04 ppb

20 Recovery of Herbicides Recovery Std Dev Recovery Std Dev Dicamba823 Dichloroprop844 Chloramben736 Dacthal, MA695 Norflurazon736 Silvex905 Dinoseb72 14 MCPA803 Acifluorfen714 Bentazon893 2,4-D833 AVG 78 5 Conc: 500 ppt Volume: 1 Liter ISOLUTE ENV+ (500 mg, 6 mL) on AutoTrace

21 Recovery of Carbamates and Urea Pesticides Conc: 500 ppt Volume: 1 Liter ISOLUTE ENV+ (500 mg, 6 mL) on AutoTrace Recovery Std Dev Recovery Std Dev Methiocarb847 Fluometuron909 Linuron791 Propoxur854 Neburon755 Carbaryl92 9 Barban85 13 Carbofuran884 Diuron856 AVG 85 6

22 C8 / ENV+ Layered Columns A layered column approach has been applied to the extraction of a broad range of organic pollutants from drinking water and surface water (EEC directives 80/778 and 75/440) to form an efficient multiresidue extraction approach. Analyte classes extracted: Base neutral herbicides Acidic herbicides Phenols PAHs Phthalate esters Ref: Davi et al, Intern. J. Environ. Anal. Chem 74 (1-4)

23 Multiresidue SPE Method 1. Sample pre-treatment 2. Column solvation 3. Column equilibration 4. Sample application 5. Interference elution 6. Analyte elution 10 ml methanol 10 ml water 1L sample – 60 ml / min Dry 10 mins under vacuum 10 ml acetone / ethyl acetate (1:1, v/v) Acidify to pH2 with HCl Add 10 ml methanol C8 / ENV+ layered column 700 mg / 6 ml

24 Base-Neutral Herbicides

25 Acidic Herbicides and Phthalates

26 Phenolic Compounds

27 PAHsPAHs

28 ENV+ vs. Carbopack Recovery Std Dev Recovery Std Dev Dichlobenil763 Chlorothalonil574 Conc: 500 ppt Volume: 1 Liter NOT RETAINED ON CARBOPACK! ISOLUTE ENV+ (500 mg, 6 mL) on AutoTrace


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