Metrohm Ion Chromatography The new UV/Vis generation – 886/887 Dr. Katinka Ruth Product Specialist Competence Center IC Metrohm International Headquarters UV/Vis generation 886/887

The new UV/Vis generation – 886/887 Outline New UV/Vis detector New heated reactor For post-column reactions As column department Applications UV/Vis generation 886/887

887 Professional UV/Vis Detector Hardware Diode array detector UV lamp (deuterium) + Vis lamp (halogen) Built in as in 844 8 data channels + 1 reference channel CH1/CH2 quotient channel omitted 887 = standalone detector Combination possible with 850, 881, 882 (≠ conductivity detector) Connection to PC via USB Analog out: up to 4 channels UV detector can basically be combined with all other IC devices UV/Vis generation 886/887

887 Professional UV/Vis Detector Features Same functionality as 844 MagIC Net T int, T out: New names for better understanding Tint = integration time Tout = measuring time Measuring time = multiple of integration time Records spectra at any point of the chromatogram Graphic frame in MagIC is not able to show 3D UV/Vis generation 886/887

Feature: Spectrum at any time point Retention time 19 min (bromide) Retention time 23 min (nitrate) Retention time 9 min (nitrite) 2 ppm nitrite, 4 ppm bromide, 50 ppm nitrate in artificial sea water (28 g/L NaCl) A Supp 10 - 250 5 mmol/L Na2CO3, 5 mmol/l NaHCO3 1.0 mL/min MSM MCS (step after 13.5 min) 218 ± 5 nm Sample volume 5 µL According to AW CH6-1027-012010 Range 1 means 1mV = 1mAU UV/Vis generation 886/887

Features Evaluate absorbance maxima Define start and end wave length Automatic evaluation of absorbance maxima Up to 10 automatic evaluations Range 1 means 1mV = 1mAU UV/Vis generation 886/887

Features Direct and indirect UV detection Change polarity via MagIC Net Range 1 means 1mV = 1mAU UV/Vis generation 886/887

Features New assembly of lamps Installation from the top Easy mounting Range 1 means 1mV = 1mAU 6.2804.050 Deuterium lamp (UV) 6.2804.060 Halogen lamp (Vis) UV/Vis generation 886/887

887 Professional UV/Vis detector Technical specifications Array with 512 diodes Channel λ 190 – 900 nm (increment 1) Bunching ± 0 – 100 nm (increment 1) Integration time 10 – 254 ms Measuring time 50 – 2000 ms Noise (expected) 0.1 – 0.2 mAU (similar to 844) Resolution 1.4 nm Metal free Leak sensor on tray PEEK detector cell Bunching bigger than with 844 Noise: tests with final device + software coming soon, lower noise with suppression Optical path UV/Vis generation 886/887

887 Professional UV/Vis Detector Possible combinations MagIC Net 2.2 = must Stand alone UV detector Controlled by MagIC Net Multi, Professional, and Compact 887 Professional UV/Vis Detector UV/Vis generation 886/887

887 Professional UV/Vis Detector Possible combinations 881 or 882 Compact IC 2.881.00X0 Compact IC pro 2.882.00X0 Compact IC plus 6.2061.120 System Connector ProfIC/Compact IC  2.887.0010 Professional UV/Vis Detector Connector Only UV detector Or UV detector + conductivity detector 887 Professional UV/Vis Detector 1 detector: MagIC Net Compact 2 detectors: MagIC Net Professional UV/Vis generation 886/887

887 Professional UV/Vis Detector Possible combinations 850 Professional IC 887 Professional UV/Vis Detector 2.850.XXXX Professional IC 2.887.0010 Professional UV/Vis Detector σ σ 1 detector: UV 2 detectors: UV + conductivity Needs MagIC Net Professional 3 detectors: UV + 2 x conductivity in series or parallel detection MagIC Net Professional UV/Vis generation 886/887

New heated reactor – general info Heating up to 150°C, increment 0.1°C Direct heat transfer, faster heating than 850, 881 <10 min (20°C to 40°C) Temperature stability: better than 0.05°C Temperature reproducibility: better than ± 0.2°C Temperature accuracy: <1°C MagIC Net 2.2 (Professional and Multi) Combinations possible with 850, 887, 881, 882 Host for further 872 Extension modules Robust design Two versions: a) 2.886.0110 Professional Reactor b) 2.886.0210 Professional Thermostat Replaces PCR box Heat-conductive paste, aluminium housing, aluminium core, spiral capillary For column heating UV/Vis generation 886/887

a) 2.886.0110 Professional Reactor For post-column-derivatisation (PCR) Intelligent reactor = iReactor (with chip on reactor plate) Temperatures up to 120°C Space to have 4 reactors Heated mixing-T Accessories (included) 6.2744.330 Y-connector 3 x UNF 10/32 6.2845.100 Reactor plate complete to PCR Module 6.2845.200 Reactor complete to 6.2845.100 6.1015.100 Metrosep BP 1 Guard/2.0 UV/Vis generation 886/887

a) 2.886.0110 Professional Reactor Setup Base plate (iReactor) + 1 reactor (0.5 x 2000 mm PEEK-capillary) dimensions as previous PCR-Box + 2 reactor e.g. as preheating capillary for eluent or post column reagent Up to 4 reactors Setup depends on application/desired temperature Der Reaktor besteht aus einer spiralförmigen 0.5 x 2000 mm PEEK-Kapillare, welche auf einem Alu-Kern aufgewickelt ist. Die Wäme wird über eine Wärmeleitpaste vom Alu-Gehäuse auf die Kapillare übertragen. Die Dimensionen sind identisch mit der im PCR-Modul verwendeten Teflon-Mischkapillare von SeQuant. Bei der Reaktionsgeschwindigkeit und beim Rauschen wurden keine Unterschiede festgestellt. UV/Vis generation 886/887

b) 2.886.0210 Professional Thermostat Heated column department Compatible with intelligent columns Column length up to 150 mm Temperature up to 80°C Accessories (included) 6.1836.020 Preheating capillary with core, 1.44 m 6.2845.600 Column holder complete to PCR Module UV/Vis generation 886/887

2.886.0210 Professional Thermostat Setup Up to 2 columns in the thermostat e.g. column + pre-column or 1 x 150 mm + 1 x 100 mm 1 column is monitored Additional pre-heating capillary must be installed UV/Vis generation 886/887

Intelligent Thermostat / Reactor Name reactor plate Set to work Last change Comment Chip for reactors as at intelligent columns Monitoring / Traceability 1 Chip per reactor plate (iReactor) Data field for up to 4 reactors Reactor 1 mounted Reactor 1 order number Reactor 1 material Reactor 1 length Reactor 1 inner diameter Reactor 1 comment Reactor 2 mounted Reactor 2 order number Reactor 2 material Reactor 2 length Reactor 2 inner diameter Reactor 1 comment etc. UV/Vis generation 886/887

2.886.0110 Professional Reactor Possible combinations 881 or 882 Compact IC Transport of PCR-reagent: High pressure iPump of 872 Extension module Use of BP 1 Guard 2.881.00X0 Compact IC pro 2.882.00X0 Compact IC plus 6.2061.120 System Connector ProfIC/Compact IC  2.887.0010 Professional UV/Vis Detector 2.886.0110 Professional Reactor 2.872.0010 Extension Module IC Pump 6.1015.100 Metrosep BP 1 Guard/2.0 Connector 887 Professional UV/Vis Detector 886 Professional Reactor 872 IC Pump UV/Vis generation 886/887

2.886.0110 Professional Reactor Possible combinations 881 or 882 Compact IC Transport of PCR-reagent: 881 peristaltic pump + backpressure capillary Regeneration MSM: 800 Dosino Peristaltic pump of 872.0050 (for non-suppressed systems) 800 Connector aw ch6-1007-082009 Title[ Regeneration and Rinsing of the MSM suppressor with one Dosino ] 887 Professional UV/Vis Detector 886 Professional Reactor 2.881.00(2/3)0 Compact IC pro 2.882.00(2/3)0 Compact IC plus 6.2061.120 System Connector ProfIC/Compact IC  2.887.0010 Professional UV/Vis Detector 2.886.0110 Professional Reactor UV/Vis generation 886/887

2.886.0110 Professional Reactor Possible combinations σ σ Transport of PCR-reagent: 850 high pressure iPump (alternative : peristaltic pump) Use back pressure column together with iPump Flexible detector setup 850 Professional IC 887 Professional UV/Vis Detector 886 Professional Reactor σ σ UV in series or parallel 2.850.XXXX Professional IC 2.887.0010 Professional UV/Vis Detector 2.886.0110 Professional Reactor 6.1015.100 Metrosep BP 1 Guard/2.0 UV/Vis generation 886/887

2.886.0110 Professional Reactor Possible combinations Transport of PCR-reagent: 872 Extension Module IC Pump or 872 Sample Prep (peristaltic pump) Transport of eluent + injection: 872 Extension Module IC Module Bottle holder + tray 887 Professional UV/Vis Detector 886 Professional Reactor 872 IC Module IC Pump 2.887.0010 Professional UV/Vis Detector 2.886.0110 Professional Reactor 2.872.0030 Extension Module IC Module 2.872.0010 Extension Module IC Pump 6.2061.100 Bottle holder (ProfIC) 6.2061.110 Tray with sensor 6.1015.100 Metrosep BP 1 Guard/2.0 Backpressure capillary UV/Vis generation 886/887

2.886.0210 Professional Thermostat Possible combinations Simple stand-alone UV-system 886 as column department Bottle holder + tray 887 Professional UV/Vis Detector 886 Professional Thermostat 872 IC Module 2.887.0010 Professional UV/Vis Detector 2.886.0210 Professional Thermostat 2.872.0030 Extension Module IC Module 6.2061.100 Bottle holder (ProfIC) 6.2061.110 Tray with sensor UV/Vis generation 886/887

suppressed or non-suppressed UV detection – suppressed or non-suppressed +MSM +MCS +MSM-MCS –MSM-MCS N = 8 500 ppb NO2, Br, NO3; A Supp 15 -150 (4.0 mm); 0.7 mL/min 5mM Na2CO3 0.3 mM NaOH, 45°C, 20ul loop Noise 0.05 – 0.075 mAU Noise 0.05 – 0.075 mAU Noise 0.15 – 0.2 mAU 500 ppb NO2-, Br-, NO3- Mean (n = 8) 20 µL loop 218 ± 15 nm 45°C Integration time 13 ms A Supp 15 – 150/4.0 Measuring time 1 s 0.7 mL/min 5 mM Na2CO3 + 0.3 mM NaOH UV/Vis generation 886/887

suppressed or non-suppressed UV detection – suppressed or non-suppressed NO2 +MSM +MCS +MSM -MCS –MSM Full width at half maximum 0.40 0.35 Height 1.8 Area 0.79 0.80 0.70 Noise 0.09 0.18 S/N 21 10 Theoretical plates 1619 1362 2041 Br +MSM +MCS +MSM -MCS –MSM Full width at half maximum 0.53 0.52 0.62 Height 0.7 0.5 Area 0.38 0.39 0.27 Noise 0.09 0.18 S/N 8 3 Theoretical plates 1782 1709 3068 NO3 +MSM +MCS +MSM -MCS –MSM Full width at half maximum 0.65 0.66 Height 1.5 1.1 Area 1.02 1.07 0.80 Noise 0.09 0.18 S/N 17 6 Theoretical plates 1533 1324 2335 Noise has influence on integration, and thus theoretical plates can change Conclusion Area, height, noise, S/N = suppressed better Theor. Plates = non-suppressed better UV/Vis generation 886/887

suppressed or non-suppressed UV detection – suppressed or non-suppressed Recommendation Chemical suppression (MSM) Improvement for Noise → S/N System peak Injection peak No MCS Peak broadening costs + MSM + MCS + MSM - MCS - MSM - MCS UV/Vis generation 886/887

Applications All existing applications published with 844 or Lambda 1010 (reactor dimensions identical to previous PCR-Box) Direct UV/Vis detection Indirect UV/Vis detection Pre column derivatisation + UV/Vis detection Post column derivatisation + UV/Vis detection UV/Vis generation 886/887

Applications Examples for Post column reactions (PCR) Transition metals Chromate Bromate Silicate Cyanide, cyanogen chloride Aluminium ... Potential new applications for PCR Amino acids Ammonium next to high amounts of sodium Au, Ag, Hg, Pt, Pd UV/Vis generation 886/887

Applications 887 Professional UV/Vis detector Cl- NO2- NO3- 500 ppb NO2-, NO3- in artificial sea water (28 g/L NaCl) A Supp 10 – 250/4.0 5 mmol/L Na2CO3, 5 mmol/l NaHCO3 0.7 mL/min 5 µL MSM MCS 218 nm ± 15 nm T int 13 ms, T out 1 s AW CH6-1027-012010 NO2- No dilution; Cl influence NWG Interface, hard to judge, ~50 ppb NO3- UV/Vis generation 886/887

UV detection of nitrite and nitrate Calibration 50 ppb – 20 ppm Ion Relative standard deviation Correlation coefficient Nitrite 1.163 0.999986 Nitrate 1.113924 0.999987 UV/Vis generation 886/887

Applications Transition metals 10ppm Cu, Ni, Zn, Co, Mn, 20ppm Cd, 50ppm Pb Metrosep C 5 – 150/4.6 15 mmol/L oxalic acid pH 3.5 (NH3) 1.0 mL/min (eluent) 0.5 mL/min (PCR) 10 µL 510 nm ± 11 nm PCR-reagent 0.15 mmol/L PAR 0.4 mol/L NH3 80 mmol/L HNO3 More info/details presentation “columns” NWG ~1 ppb expected UV/Vis generation 886/887

Applications Amino acids USP 27 norm for amino acids Requires 120°C Possible with new PCR reactor 0.5 mM amino acids (20 compounds) Metrosep Amino Acids 1 – 100/4.0 USP eluent 570 nm PCR-reagent Ninhydrin, hydrindatin dimethylsulfoxid, lithium acetate, acetic acid (N2 purged) UV/Vis generation 886/887

Applications Bromate Bromate 4.8 min According to draft norms ISO/DIS 11206 + EPA 326 PCR, tri-iodide method UV absorbance at 352 nm Metrosep A Supp 16 – 100/4.0 0.5 – 5 ppb Bromate UV/Vis generation 886/887

Summary UV/VIS generation – 886/887 Professional UV/Vis detector MagIC Net 8 channels (wavelength + bunching) spectra at any time point functionality as 844 Professional Thermostat / Reactor Faster heating + higher temperatures (direct heat transfer) iReactor 2 MPa backpressure for smooth adding of reagent Available in summer 2010 (depending on MagIC Net 2.2) Faster heating + higher temperatures compared to 850, 881, and Dionex specs UV/Vis generation 886/887