Evaporative Light Scattering Detector Product Range

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

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

PL-ELS 1000 High Temperature ELSD Solvent resistance enclosure Clear Display of Detector Output and Exhaust temperature Status LEDs Display – detector output, exhaust temp Status LED - green light = ready, red light = standby/error Handset – mode of operation, methods, temp and gas control, auto zero, clear errors Removable handset allows instrument control both on and off the unit

PL-ELS 1000 High Temperature ELSD

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

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

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

Drain from solvent trap Solvent Trap and Waste Nebulizer waste To extraction system Drain from solvent trap PTFE narrow bore exhaust tubing Glass collection vessel 99.5%+ recovery for aqueous based solvents Safe and environmentally friendly Waste drain allows constant pressure Waste drain

Control features and 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)

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

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

Computer Interface Monitor available giving view of output, temperatures and gas flow

Polymer Additive Analysis 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. Columns : 2 x PLgel 5um 50Å Eluent : THF + 0.1% diethanolamine Flow rate : 1.0ml/min Chimasorb 944 Irgafos 168 Irganox 1010 Tinuvin 622 Tinuvin 770 Tinuvin 327 6 minutes 20

Separation of PEG Using GPEC The PL-ELS 1000 can be operated at high temperature for polymer analysis, such as 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

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

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 Column Connection Liquid Waste Keypad 415mm Display

Nebulization Eluent flow mixed with N2/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

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)

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

Digital Signal Processing 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)

Two modes of operation : 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 LED on Temperatures and gas flow controlled to set values

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

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

PL-ELS 2100 Control Software 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 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

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 To use this software utility, simply connect the PL-ELS 2100 to a PC via a serial connection (RS232)

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

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.

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

Volatile Applications: Effect of Changing Evaporator Temp Samples: 1. Acetanilide, 2. Indapamide, 3. Ibuprofen, 4. Dibutylphthalate Column: C18 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 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

Environmental Application:Herbicides Sample: Mixture of 10 Phenylurea herbicides Column: C18 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)

Environmental Application: Herbicides

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

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

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

Non-Volatile Application: Triglycerides in Natural Oils Sample: 2mg/ml Starflower Oil Column: C18 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)

Advantages of ELSD: Uniformity of Response Comparison of UV and ELS traces show that ELSD allows for a more uniform response than UV detection 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

Comparing PL-ELS 1000 & 2100 response PL-ELS 2100 gives better mass response due to lower temperature operation 80°C Small response for UV peak 1 – not as strong a chromophore as 2 ELS gave very similar response – mass response 30°C

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

PL-ELS 2100: DMSO Transparency Sample: Pharmaceutical Mixture in DMSO Column: C8 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)

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

Ideal for High Throughput Screening 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

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

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