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Evaporative Light Scattering Detector Product Range.

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Presentation on theme: "Evaporative Light Scattering Detector Product Range."— Presentation transcript:

1 Evaporative Light Scattering Detector Product Range

2 Introduction PL-ELS 1000 Routine GPC and HPLC using high boiling point solvents PL-ELS 2100 Regular HPLC with low temperature operation for volatile compounds Polymer Laboratories ELSD portfolio includes 2 models, each offering high sensitivity for a wide range of applications

3 Application Areas of PL’s ELSDs PL-ELS 1000 GPC analysis Ambient High Temperature HPLC of non volatiles Lipids Sugars (Microbore LC) PL-ELS 2100 Low temperature analysis HPLC of volatiles & semi-volatile analytes Pharmaceuticals Nutraceuticals Combinatorial libraries Ambient GPC analysis SFC

4 Solvent resistance enclosure Clear Display of Detector Output and Exhaust temperature Status LEDs Removable handset allows instrument control both on and off the unit PL-ELS 1000 High Temperature ELSD


6 The eluent “droplet” is sheared from the needle by the gas supply (cross-flow nebulization) Eluent Inlet Gas Inlet PL-ELS 1000 Nebulizer

7 A large thermal mass ensures accurate and constant temperature control The chamber is independently temperature controlled The PL-ELS 1000 can operate up to 300°C PL-ELS 1000 Evaporator

8 Light Source Detector (via fiber optic cable to Photodiode detector) (tungsten halogen lamp) PL-ELS 1000 Optics

9 Safety Features Vapour sensors Independent temperature sensors Gas flow safety Electrical surge protection CE compliant

10 Solvent Trap and Waste Nebulizer waste Drain from solvent trap To extraction system Waste drain

11 Control features and Modes of Operation Modes of operation Run –Instrument is fully operational Standby –Power on, instrument parameters can be modified Sleep –Instrument shut down Gas Save –Heaters at operational temperature – Gas flow rate and heaters at operational levels – Gas flow set at zero, lamp and heaters off – Gas flow closed, lamp and heaters off – Gas flow at low flow (0.1 SLM)

12 Control features and Modes of Operation Control features Control parameters stored as method. –10 locally –unlimited via software System automation Instrument diagnostics Operational log Computer software Removable handset System performance testing

13 PC Control Software and System Performance Testing Runs a series of diagnostic checks on the detector When used in conjunction with the log can be used to diagnose errors. Can be used to validate detector performance OQ, IQ and PQ feature

14 Computer Interface

15 Columns : 2 x PLgel 5um 50Å Eluent : THF + 0.1% diethanolamine Flow rate : 1.0ml/min 620minutes Chimasorb 944 Irgafos 168 Irganox 1010 Tinuvin 622 Tinuvin 770 Tinuvin 327 Most additives are non-volatile and do not possess a UV chromophore. The and universality and high temperature range of the PL-ELS 1000 provides a sensitivity detection technique. Polymer Additive Analysis

16 Separation of PEG Using GPEC Samples: Narrow polyethylene glycol standards (Mp 600 and 1470) Columns: Zorbax 300 SB-C18 5µm, 150x4.6mm Eluent: ACN: Water Flow rate: 0.5mL/min Detector: PL-ELS 1000 Evap 140°C, neb 100°C, gas flow 0.5SLM The PL-ELS 1000 can be operated at high temperature for polymer analysis, such as GPEC.

17 Benefits of the PL-ELS 1000 Operating Temperature range from 40 to 300°C Extremely low dispersion for high resolution separations Highly Sensitive and Stable High eluent flow rates, up to 3ml/min Low gas consumption Compatible with High Temperature GPC Remote control Easy to use software Extremely small footprint, stackable

18 PL-ELS 2100 Compact, modern design Flat top Small footprint, stackable Operation via control panel and simple keypad Column connection at front of detector One exhaust tube at rear, one liquid waste port at front 200mm 450mm 200mm Column Connection Liquid Waste Keypad 415mm Display 450mm

19 Nebulization Eluent flow mixed with N 2 /Air Concentric nebulizer gives efficient nebulization, stable droplet plume, uniform droplet size Narrower cone of spray plume allows a smaller nebulizer chamber, which minimizes band broadening Better recovery of semi-volatile solutes compared to cross-flow nebulizer Easier to align, reproducible from one detector to another Temperature independently controlled

20 Evaporation Solvent removed by heating Temperature independently controlled PL-ELS 2100 has an additional gas input that aids evaporation (patent pending) Small volume evaporator Fast thermal equilibration Diffuser reduces turbulence inside evaporator tube which minimizes band broadening (patented)

21 Detection Blue LED light source (480nm) Intensity controllable by user Photomultiplier detector tuned to same wavelength for increased sensitivity Feedback control for light source provides constant output Detector mounted directly onto the optics which eliminates stray light loss and increases sensitivity Reduced volume in the optics chamber, minimizes band broadening Digital gain control to optimize full scale sensitivity Digital signal smoothing to optimize S/N ratio

22 Digital Signal functions are accessed via the down arrow key in main menu screen Parameter Screen allows you to change - PMT output or gain (1-250) - Smoothing (1-50) - LED intensity (0-100) Digital Signal Processing

23 Simple Operation Two modes of operation : STANDBY Power on LED off Heaters off Gas at minimum flow rate (1.2 L/min) - Gas shuts off after 15 minutes RUN Power on LED on Temperatures and gas flow controlled to set values

24 Operating the PL-ELS 2100: Onboard Instrument Control Keypad Interactive menu bar Current method Mode Detector output Status Actual values of set parameters

25 PL-ELS 2100 Control Software  Select mode of operation  Control parameters  Evaporator & Nebulizer temp  Gas flow (0-3.25 L/min)  Monitor output  Gain setting (0.1-250)  Signal smoothing (0-5) Log instrument conditions over time Load / Edit methods - 10 programmable methods

26 PL-ELS 2100 Control Software To use the control software simply connect the PL-ELS 2100 to a PC via a serial connection (RS232) on selectable COM port Where no serial port is available, a USB serial connector can be used Supplied as standard with the PL-ELS 2100 Select 1 of 10 different temperature programs according to analysis Also available as a Software Development Kit for third party system integration

27 Method Manager Software Used when the instrument is to be controlled via the onboard instrument control (rather than software control) This is a simple software utility designed to set up, edit and log defined methods which can then be downloaded to the PL-ELS 2100 Method Manager Software supplied as standard with the PL-ELS 2100 To use this software utility, simply connect the PL-ELS 2100 to a PC via a serial connection (RS232)

28 PL-ELS 2100: Routine Operation When running with the “XXX” method, the User has complete flexibility to change parameters via the PL-ELS 2100 keypad and display (e.g. for method development) Once standard methods for operation of the PL-ELS 2100 have been established, these can be stored using the PL-ELS 2100 Method Manager software utility and downloaded to the unit These downloaded parameters are stored as numbered methods (1-10) and cannot be edited through the keypad, only by running the PL-ELS 2100 Method Manager software

29 A New Approach to ELS Detection Operating conditions of the PL-ELS 1000 is based on the properties of the eluent (e.g. high boiling point solvents require high evaporator temperatures) However, the PL-ELS 2100 operating conditions are determined by the properties of the analyte (e.g. semi- volatile or non-volatile) The PL-ELS 2100 can evaporate water at ambient temperature, unlike the PL-ELS 1000.

30 Manipulating the PL-ELS 2100 Parameters FOR NON-VOLATILE SOLUTES Nebulizer and evaporator can run hot to increase signal to noise ratio Gas flow is set as low as possible to maximize signal FOR RELATIVELY VOLATILE SOLUTES Nebulizer and evaporator run cold to increase signal Gas flow is increased to control baseline noise

31 Samples: 1. Acetanilide, 2. Indapamide, 3. Ibuprofen, 4. Dibutylphthalate Column: C 18 5µm, 150x4.6mm Eluent A: 0.1% TFA in Water Eluent B: 0.1% TFA in ACN Gradient: 60-90%B in 5 mins Flow Rate: 1.0mL/min Detector: PL-ELS 2100 (neb and evap set at the same temperature, gas 1.8 L/min) Note: peak 2 is non-volatile, peaks 1, 3, 4 are relatively volatile Volatile Applications: Effect of Changing Evaporator Temp

32 At high temperature peak 2 has better S/N but peaks 1,3,4 are not detected At 30°C all four peaks are detected

33 Environmental Application:Herbicides Sample: Mixture of 10 Phenylurea herbicides Column: C 18 5µm, 250x4.6mm Eluent A: Water Eluent B: Acetonitrile Gradient: 10-80%B in 40 mins Flow Rate: 0.7ml/min Inj Vol:20µl Detector: PL-ELS 2100 (neb=25°C, evap & gas flow varied)

34 Environmental Application: Herbicides

35 Non-Volatile Applications: PEG 400 Separation Sample: PEG 400 Column: PLRP-S 100Å 5µm, 150x4.6mm Eluent A: Water Eluent B: ACN Gradient: 10-30% B in 12 mins Flow Rate: 1.0mL/min Inj Vol: 10µl

36 PEG 400: Effect of Changing Temperature Evap 30°C Neb 30°C Gas 1.6 L/min Evap 90°C Neb 90°C Gas 1.6 L/min Higher temperatures increase S/N, no risk of loss due to evaporation

37 PEG 400: Effect of Changing Gas Flow Evap 70°C Neb 50°C Gas 1.2 L/min Evap 70°C Neb 50°C Gas 2.4 L/min Sensitivity is improved as gas flow is reduced

38 Non-Volatile Application: Triglycerides in Natural Oils Sample: 2mg/ml Starflower Oil Column: C 18 5µm, 250x4.6mm Eluent A: ACN Eluent B: DCM Gradient: 30-50% B in 40 mins; 50-90% in 2 mins, hold for 3mins Flow Rate: 1.0ml/min Inj Vol: 20µl Detector:PL-ELS 2100 (neb=40°C, evap=70°C, gas=1.4 L/min)

39 Column: PLRP-S 100Å 5µm, 150 x4.6mm Eluent A: 50% 0.1% TFA in Water : 50% 0.1% TFA in ACN Flow Rate: 1.0ml/min Inj Vol: 10µl Detector: PL-ELS 2100 (neb=30°C, evap=30°C, gas=1.4 L/min) UV-VIS @ 280nm Comparison of UV and ELS traces show that ELSD allows for a more uniform response than UV detection Advantages of ELSD: Uniformity of Response

40 Comparing PL-ELS 1000 & 2100 response 80°C 30°C PL-ELS 2100 gives better mass response due to lower temperature operation

41 PL-ELS 2100: Fast Gradient, Fast Flow Rate Capability 2ml/min 3ml/min 4ml/min 5ml/min Stable baseline throughout the gradient PL-ELS 2100 can operate in 100% up to 5ml/min min

42 PL-ELS 2100: DMSO Transparency Sample:Pharmaceutical Mixture in DMSO Column:C 8 5µm, 50x4.6mm Eluent A:Water Eluent B:Acetonitrile Gradient:5-100% B in 5 mins Flow Rate:1.0ml/min Inj Vol:20µl Detector:PL-ELS 2100 (neb=25°C, evap & gas flow varied)

43 Ideal for High Throughput Screening Loss of volatile species occurs as temperature is increased

44 The design of the PL-ELS 2100 makes it transparent to DMSO at 25-30°C Great potential in the High Throughput Combichem market Unique to the PL-ELS 2100 due to its use of evaporation gas PL-ELS 2100: neb=25°C, evap=30°C Ideal for High Throughput Screening

45 Benefits of ELSD Universal detector: independent of the optical properties of the solute Compatible with gradient elution Ideal for fast gradient elution:- no solvent front. Removes the need for derivatization Compatible with chromatographic techniques such as MS and SFC Wide application area

46 Additional Benefits of the PL-ELS 2100 Operation in 100% water at 25°C DMSO transparency at ambient temperature Extremely low dispersion for high resolution separations (e.g. SFC) High sensitivity to volatile compounds Compatible with eluent flow rates, up to 5ml/min Rapid thermal equilibration Easy to use Extremely small footprint, stackable

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