Polyvap /Analyst / SPESyncore®

en

Syncore® – an efficient, safe and environmentally sound tool for parallel sample processing

Syncore® comprises two instruments and a broad range of accessories suitable for all aspects of multiple sample processing. Its design concept allows one unit to perform as a parallel evaporator (Polyvap) which can be instantly converted into a parallel concentrator (Analyst). Thus, the field of applications includes fast parallel evaporation of multiple samples, the smooth concentration to predefined residual volumes and the sample preparation and purification with the SPE Module and the high quality Silica Prep cartridges from SiliCycle.

Polyvap page 6, 7

Analyst page 8, 9

SPE and support page 10, 11

Evaporation to dryness: Polyvap

The Polyvap is a unique parallel evapor-ator which allows fast safe environmentally sound reliable

evaporation of samples ranging in volume from 0.5 to 500 ml.

Concentration to residual volumes: Analyst

Chemical analysis often requires con-centration of big volumes to small resid-ual volumes. The Analyst performs this task with a locally cooled appendix. It further provides high recovery rates due to smooth sample processing.

Parallel preparation and purification of your sample: BUCHI SPE module and SiliCycle cartridges.

With the SPE module from BUCHI your SPE can be done directly into the evap-oration flask and your concentration can be proceeded without any additional step. You can save time and increase the quality of your results. SiliCycle is offering an excellent application support for SPE in combination with BUCHI.

Accessories page 13

Overview page 4, 5The modular concept

BUCHI Syncore® Line – the modular system for evaporation, concentration and sample preparation

The Platform is the core component of the three Syncore configurations. It provides basic functions like shaking, heating (150 °C) and cooling (–20 vapor °C) with an optional cooling plate.

Parallel evaporation: Syncore® Polyvap

Parallel evaporation of 4, 6, 12, 24, 48 and 96 samples ranging in volume from 500 to 0.5 ml.

Each rack has its own coated aluminum lid with individual vacuum connections.

Evaporation System

Recirculating ChillerThe recirculating chiller F-108/ F-114 provides the right cool-ing capacity for all Syncore configurations and accesso-ries.

Vacuum ControllerThe programmable Vacuum Controller V-855 can easily cope with complex solvent mixtures and allows auto-matic distillation.

Great time savingA refrigerated receiver re-duces the evaporation time by up to 30 %. Ideal for evapor ation of solvent mix-tures without cumbersome breaks.

Vacuum PumpThe Vacuum Pump V-700/ V-710 is optimally designed for use with V-855 and Syncore.

■ Heatable and chemical resistant vacuum cover

■ Individually sealed tube

■ Glass tubes for an individual observation of the evaporation stage (Crystal Rack)

■ Electronic controlled heatable rack (ambient to 150 °C)

The Platform

condenser

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@buchibest

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Installation, Operation and Performance of Syncore® Analyst for Environmental Analysis

www.buchi.com Information Bulletin Number 54/2009

5BUCHI Syncore® Line – the modular system for evaporation, concentration and sample preparation

Parallel concentration: Syncore® Analyst

Concentrate solutions in parallel to a cooled residual volume in formats of 4, 6 and 12.

Special glasswareBUCHI is offering a range of different glassware designed to optimize your processes and reduce sample transfer.

The Flushback Module – available in 6 and 12 positions – significantly increases recovery rates.

best@buchiThe scope of application in parallel evaporation, concen-tration and sample prepara-tion is show in several appli-cation notes.

SPE application support SiliCycle is offering a wide range of compatible SiliaPrepTM SPE cartridges in different formats, phases (such as reversed, polar, ionic, mixed mode and fluorinated phases) with specific characteristics and a broad application support.

SPE ModuleWith the SPE Module all essential work-up steps in-cluding evaporation are achieved without any sam-ple handling between the individual steps.

A horizontal orbital movement with a maxi mum rotational speed of 600 rpm produces a strong vortex in the sample tube thereby preventing bumping during operation. Temperature profiles can ei-ther be preprogrammed in timed stages or can be manually controlled.

cooling zone

H2O out

H2O in

H2O out

H2O in

residualvolume

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■ Optional Flushback Module which partially condenses the vapor at the top of the vessels.

■ Locally cooled appendix of the sample vessel to prevent evaporation under constant vacuum conditions.

Evaporation to dryness: Polyvap –efficient parallel evaporation of a wide sample range

Parallel evaporation of multiple samples is an essential prerequisite to increase productivity in parallel and multistage synthesis, extraction, quality control and chromatography. The Polyvap solves this problem quickly and safely even with high-boiling solvents. Interchangeable racks make it possible to evaporate samples ranging in volume from 0.5 to 500 ml. Optimal evaporation conditions are automatically adjusted using the optional Vacuum Controller V�855.

Syncore® Polyvap advantages No cross-contamination High chemical resistance Environmentally sound operation (ISO 14000) Automatic distillation with Vacuum Controller V-855 Evaporation of high-boiling solvents like DMSO and DMF Fully transparent racks in format 4 and 6 Compatibility with the Syncore Reactor and Syncore Analyst

Areas of application Evaporation of chromatography samples Evaporation after parallel extractions Gravimetric analyses in quality control Evaporation after parallel reactions

Extraction samplesHigh-pressure solvent extractions (Speed Extraction or ASE**) provide a considerable number of samples within a short period of time. With the Speed Extraction, ASE Rack up to 24 samples are evap orated simultaneously sustain-ing a high sample throughput in routine analysis.

Typical applications

Chromatography samples In chromatography a large number of samples are pooled in bigger flasks or evaporated individually. The workflow in sample work-up is significantly increased by simultaneous evaporation of multiple samples.

** ASE is a registered trademark of Dionex Corporation.

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With the help of the vacuum gradient function of the Vacuum Controller V-855 smooth adjustment to the end-vacuum is possible. This function is also ideal for evaporating off solvent mixtures which typically accumulate after chromato graphy. The settings can be saved in user-defined pressure profiles.

Order no.Vacuum Controller V-855 47232

Maximum flexibilityExchangeable racks provide maximum flexibility in both sample volume and sample numbers. The racks are avail-able in formats of 4, 6, 12, 24, 48, and 96 samples ranging in volume from 500 ml to 0.5 ml depending on the rack format.

High-boiling solventsHigh-boiling solvents, such as DMSO or DMF, are efficiently evaporated using the High-Temperature Insulation Kit. The kit comprises a rack and cover insulation with Woulff bottle and hose.

No cross-contaminationEach sample has its own vacuum connection via a vacuum cover. This design principle, together with the use of inert materials such as glass, coated aluminum and PTFE, prevents cross-contamination. The cover is heatable to 70 °C to prevent condensation.

Polyvap features

Schematic representation of a rack with two tubes individ-ually connected to the heated vacuum cover. The vapor is conducted to the condenser via grooved channels.

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Performance data

Evaporation rates Conditions: Parallel evaporation using temperature settings of 42 °C (rack) and 50 °C (vacuum cover). Optimized vacuum gradient for each solvent controlled by the Vacuum Controller V-855. The condenser is cooled with the Chiller F-114.

Rack 6 Rack 12 Rack 24 Rack 96

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Order information for Polyvap specific accessories Positions Working Number of Order no. Order no. Order no.

volume [ml] vessels incl. Rack Vacuum Cover High-Temp. Kit

4 50–500 4 47790 38245 6 25–250 6 47770 38246 12 5–120 12 40900 40910 50 test tubes 38188 24 2–30 for SpeedExtractor, 42660 40920 41922 ASE** tubes* 48 1–20 100 test tubes 42855 42850 96 0.5–10 100 test tubes 38277 40930 41923

* Tubes are not included in the rack. ** ASE is a registered trademark of Dionex Corporation.

Distillation of solvent mixtures

Concentration to residual volumes: Analyst –smooth concentration with high recovery rates

Efficient parallel concentration of large sample volumes to predefined residual volumes is a cornerstone of virtually every sample preparation technique in environmental analysis and quality control. In addition, smooth evaporation of thermosensitive compounds is crucial in preventing thermal decomposition. The Analyst copes with both tasks by cooling a small appendix at the bottom of the sample vessels. Sample adhesion to the glass wall is prevented by creating a gentle flushing action at the top of the glass wall with partially condensed vapor.

Syncore® Analyst advantages Smooth concentration to small residual volumes No thermal decomposition High recovery rates No cross-contamination Complete solvent recovery

Areas of application Soil analysis Food-processing analysis Quality control Natural product extraction Environmental analysis

Extraction samplesThe extracts of the SpeedExtractor are collected in a special tube with an appendix and can be evaporated in a fast and reliable way on the parallel evaporator Syncore, without sample transfer, to a predefined volume. As a result 12 samples are processed in one run under the same conditions.

Concentration of PAH (best@buchi 51) The Extraction System B-811 and the Syncore Analyst par-allel concentrator as well as the Pressurized Solvent Ex-tractor were evaluated for the pretreatment of samples con-taining PAHs. Recoveries of extraction and subsequent concentration were 70–95% for 2 ring and 90–100% for 3–5 ring PAHs.

Typical applications

Determination of the pear content in apple juice (best@buchi 42) The Syncore® Analyst is scru-tinized for sample preparation in the determination of poly-cyclic aromatic hydrocarbons according to ISO 17025. The parallel evaporator excels in sample throughput, reliability and convenience. Within an evaluation period of six months, labor costs have been reduced by a factor of six.

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The Flushback ModuleThe Flushback Module is an optional accessory which is placed on top of the rack in formats of 6 or 12.

Left: without FlushbackRight: with Flushback

Tubes with appendixThe Analyst sample vessels feature an appendix with three different volumes all compat-ible with the same rack. There are two versions available: with and without graduated level indication.

Apart from the cooling zone at the appendix, there is an optional Flushback Module available which partially con-denses the vapor at the top of the vessels. Thus, the glass wall is continuously rinsed re-sulting in higher recovery rates.

Performance data

Recovery rates for concentration of polycyclic aromatic com-pounds (PAH) with the Analyst R-6 (3 ml residual volume) with-out (left) and with (right) Flushback Module in cyclohexane.

The Analyst is designed for applications in which a concen-tration step is required. This is typically the case in Food & Feed and environmental analysis, or quality control. Since the sample rests in the cooled appendix, the Analyst is also ideal for evaporation of temperature-sensitive compounds.In analysis high recovery rates are essential. For such appli-cations the Flushback Module is strongly recommended.

Conditions: Parallel evaporation using temperature settings of 40 °C (rack), 50 °C (vacuum cover), 5 °C (Flushback Module), 7 °C (residual volume). Vacuum gradient from 900 –150 mbar in 30 min. controlled by the Vacuum Controller V-855. Total time for evaporation process: 60 min.

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Local cooling zonesSchematic depiction of the locally cooled appendix of the sample vessel. The solvent evaporates above this cooling zone. The lower temperature in the appendix prevents evaporation under constant vacuum conditions.

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Order information for Analyst specific accessories

Analyst features

* Other volumes on request ** Tubes are not included in the rack.

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High recovery rate with Flushback

Positions Working Residual Tubes** Order no. Order no. Flushback volume [ml] volume* [ml] No graduation Graduated Rack Vacuum Cover Module

3.0 47797 47740 4 50–500 1.0 47798 47741 47794 38245 not available 0.3 47799 47742 3.0 38555 38557 6 25–250 1.0 38569 38575 47777 38246 48654 0.3 38485 38168 3.0 46014 46070 12 5–120 1.0 46015 46071 46000 40910 46036 0.3 46016 46072

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Parallel sample preparation: SPEImprove your workflow in work-up and evaporation

Conventional solid phase extraction (SPE), an essential step in many analytical procedures, includes a number of laborious steps. With the help of the modified parallel evaporator, Syncore®, all essential work-up steps including evaporation of the eluates are achieved without any sample handling between the individual steps.

The SPE modules offer the following benefits

Easy sample handling: conditioning, enrichment, washing, elution and evaporation are carried out without interruption, rendering high throughput.

Individual control: each sample has its own stopcock to control the flow, therefore achieving safe operation and high recovery rates.

No cross-contamination: no risk of contamination from adjacent samples due to individual sample sealing.

Efficient evaporation: elimination of sample transfer allows for fast parallel evaporation in an environmentally sound way.

Operation principle of the SPE stopcock

a “Waste” position: Cartridge is conditioned, enriched with the analyte, and

washed. All liquids are transferred to a waste vessel.

b “Stop” position: Closure of the cartridge to prevent from running dry or to

close the system during evaporation.

c “Elute” position: Elution of the analyte into the collecting vessel, followed by

concentration to a residual volume.

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SPE Method for Pesticides Detectionin Drinking Water

N

N

N

NH

Cl NH

Atrazine

N

O

Cl

O

Alachlor*

SiliCycle P/N: SPEC-R31930B-06S

SiliaPREP CleanENVI, 6 mL, 1 g

SiliaPrep CleanENVI Conditioning 2x5 mL of MeOH and 2x5 mL of H2O

Loading10 mL of drinking water through the cartridge

Washing 2x5 mL of H2O on manifold at 5˝ Hg vacuum

Elution2x3 mL of acetone on manifold at 5˝ Hg vacuum

ReconstitutionEvaporate under stream of nitrogen (30 min at 25 °C)

& reconstitute with 1 mL of reconstitution solution(H2O/ACN, 60/40)

*Alachlor is unstable at high temperature

N

N

N

NH

Cl NH

Simazine

Syncore SPE work-up accessoriesThe Syncore® SPE work-up accessories are available in two different config-urations. With the SPE Basic setup, the sample is transferred directly into the collecting vessel for subsequent evaporation. The flow of each position can be individually controlled. In contrast,

the SPE Advanced setup allows separa-ting the liquid passed through a SPE cartridge into either a waste vessel or a collecting vessel, respectively. The eluate is then evaporated to dryness (Polyvap) or to a predefined residual volume (Analyst). The accessories are available as MODULE to upgrade a standard Syncore vacuum cover, or as fully equip-

ped COVER. The accessories are com-patible with standard Luer-tipped SPE columns or filter discs. For further infor-mation please visit our homepage at:

www.buchi.com parallel evaporation

The SPE Basic MODULE intended to up-grade an existing Syncore vacuum cover comprises a coated aluminum plate, flow-control valves (PEEK) and flanged tubes (FEP). The corresponding SPE Basic COVER consists of a complete vacuum cover equipped with the SPE Basic Module.

SPE Basic accessories

The SPE Advanced MODULE intended to upgrade an existing Syncore vacuum cover comprises a coated aluminum plate, 3-way stopcocks (PTFE, FEP) fitted on a support, a waste vessel and tubes (FEP). The corresponding SPE Advanced COVER consists of a complete vacuum cover equipped with the SPE Advanced Module.

Accessories and spare parts

SiliCycle Application

Item Order no.

Set of 12 flow-control valves 051453

Set of 12 three-way stopcocks 051457

Tube cutter 019830

FEP tube (OD 1/8”, ID 1/16”, L 5 m) 044354

SPE Advanced accessories

Item Order no.

Set of 6 flanged FEP tubes 051459

Set of 4 x 3 FEP waste tubes, length adjusted 051455

Set of 25 tube fittings (1/8”, green) 040956

Set of 25 ferrules (1/8”, green) 040961

SPE Basic setup Order no.

MODULE COVER

Format 12 051440 051438

Format 24 051463 051439

SPE Advanced setup

Order no.

MODULE COVER

Format 6 11055465 11055466

Format 12 051164 051448

Pesticides Mean Recoverywith Relative Standard Deviation (RSD)

PesticidesFortification

Levels (ng/mL)

Recovery

(% for N = 6)RSD (%)

Atrazine

1 83 6

20 84 3

100 85 2

Simazine

1 85 7

20 84 2

100 83 2

Alachlor

1 72 7

20 70 2

100 67 3

Optimal operation with other BUCHI products

V-850: Simple Vacuum Con-troller for manual operation.V-855: Programmable Vac-uum Controller with gradient function and automatic distil-lation (stage probe).

Order no.V-850 47231V-855 47232

Chemical resistant PTFE dia-phragm pump with a final vacuum of < 10 mbar. Recom-mended configuration with sec. condenser, Woulff bottle and Vacuum Controller V-855. Order no.V-700 71000

V-700, V-855, condenser 71311

V-700, V-855, cold trap 71312

Recirculating chillers for oper-ation with type S condenser, Analyst Rack, Refrigerated Receiver, Reflux- and Flush-back Module.

Order no.F-108, 230 V; 50/60 Hz 800 W 11056464F-108, 115 V; 50/60 Hz 800 W 11056465F-114, 230 V; 50/60 Hz 1400 W 11056466F-114, 115 V; 50/60 Hz 1400 W 11056467

Four head diaphragm pump with a final vacuum of 2 mbar. Recommended configuration with secondary condenser, Woulff bottle and Vacuum Controller. Order no.V-710 72000

V-710, V-855, condenser 72311

V-710, V-855, cold trap 72312

Order information for general Syncore® accessories

Basic platform for indi-vidual combination to meet personal de-mands.

Order no.230 V 1P3000000120 V 1P2000000100 V 1P1000000

Carrier for Analyst or Polyvap vessels in for-mats of 4, 6 and 12.

Order no.Format R-12 40077Format R-6 40076Format R-4 40075

Standard condenser (type S) for tap water with rod, clamps, 1 or 2 liter flask.

Order no.Type S, 1 l flask 37690Type S, 2 l flask 40146

Dry ice condenser (type C) with rod, clamps, 1 or 2 liter flask.

Order no.Type C, 1 l flask 38371Type C, 2 l flask 40147

Receiver with integrated cooling loop used in conjunction with a type S condenser.

Order no.Refr. receiver 48640

Crystal Rack R-4 for working volumes of 50–500 ml, incl. 4 tubes.

Order no. 47790

Crystal Rack R-6 for working volumes of 25–250 ml, incl. 6 tubes.

Order no. 47770

Rack R-12 for working volumes of 5–120 ml, incl. 12 tubes.

Order no. 40900

Rack R-24 for working volumes of 2–30 ml.

Order no.with 50 tubes 38188for PSE tubes 42660for Falcon tubes 38440

Rack R-48 for working volumes of 1–20 ml, incl. 100 test tubes.

Order no. 42855

Rack R-96 for working volumes of 0.5–10 ml, incl. 100 test tubes.

Order no. 38277

Vacuum Cover for all rack formats R-4.

Order no. 38245

Vacuum Cover for all rack formats R-6.

Order no. 38246

Vacuum Cover for all rack formats R-12.

Order no. 40910

Vacuum Cover for all rack formats R-24.

Order no. 40920

Vacuum Cover for rack format R-48.

Order no. 42850

Vacuum Cover for rack format R-96.

Order no. 40930

Lid for R-12 and R-6 Analyst and Polyvap tubes. The set com-prises 12 or 6 pieces, respectively.

Order no.Set format 12 48690Set format 6 48689

Platform Sample vessel carrier Vessel lid Condensers

4 Positions 6 Positions 12 Positions 24 Positions 48 Positions 96 Positions

Refrigerated receiver

Vacuum Controller Vacuum Pump V-700 Vacuum Pump V-710 Recirculating Chiller

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Voltage1 100 V 50/60 Hz2 120 V 50/60 Hz3 230 V 50/60 Hz

Condenser0 NoneS Type S, Standard for chiller or tap water, P+G coatedC Type C, Cold trap for dry ice cooling, P+G coated

Round receiving flask, KS 24/20, P+G coated0 None1 1 l volume (suggested formats: 24, 96)2 2 l volume (suggested formats: 4, 6, 12)

Rack type (incl. vacuum cover)1 Crystal Rack R-42 Crystal Rack R-63 Rack R-124 Standard Rack R-246 Rack R-967 Rack R-24 PSE, ASE8 Rack R-48

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Voltage1 100 V 50/60 Hz2 120 V 50/60 Hz3 230 V 50/60 Hz

Condenser0 NoneS Type S, Standard for chiller or tap water, P+G coatedC Type C, Cold trap for dry ice cooling, P+G coated

Round receiving flask, KS 24/20, P+G coated0 None2 2 l volume

Rack type (incl. Vacuum Cover)1 Crystal Rack R-4 Analyst2 Crystal Rack R-6 Analyst3 Rack R-12 Analyst

Residual volume1 1.0 ml2 0.3 ml3 3.0 ml

Graduated level indication of appendixY Yes N No

Polyvap order matrix

Order information for complete Syncore® instruments

Analyst order matrix

SiliCycle request procedure

How to buy SiliaPrep SPE Cartridges Need help for your SPE application

Choose your SPE Cartridges and Phases at:www.silicycle.com/spe-cartridges-listing

Order online www.silicycle.com/order-silicycle-products

By emailOrders can be emailed to the following address:info@silicycle.com

By phoneOrder with our Customer Service Staff:North America: +1 877 745 4292Worldwide: +1 418 874 0054

Answer all 5 questions and send to:support@silicycle.com for any applicationinformation.

1. What is your analyte (structure)?

2. What is your matrix (water, food, juice)?

3. What is the solvent solubility of your analyte?

4. What is the pH stability of your analyte?

5. What is your matrix volume?

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BUCHI SarlFR – 94656 Rungis CedexT +33 1 56 70 62 50F +33 1 46 86 00 31france@buchi.comwww.buchi.fr

BUCHI UK Ltd.GB – Oldham OL9 9QLT +44 161 633 1000F +44 161 633 1007uk@buchi.comwww.buchi.co.uk

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BUCHI Italia s.r.l.IT – 20090 Assago (MI)T +39 02 824 50 11F +39 02 57 51 28 55italia@buchi.comwww.buchi.it

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BUCHI ShanghaiCN – 200052 ShanghaiT +86 21 6280 3366F +86 21 5230 8821china@buchi.comwww.buchi.com.cn

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BUCHI CorporationUS – New Castle, Delaware 19720Toll Free: +1 877 692 8244T +1 302 652 3000F +1 302 652 8777us-sales@buchi.comwww.mybuchi.com We are represented by more than 100 distribution

partners worldwide. Find your local representative at

www.buchi.com

The scope of applications in parallel sample preparation, evaporation and concentration is shown in many application notes.

A comprehensive list of optimized evaporation settings for Syncore is online available at:

www.buchi.com Applications Parallel Evaporation

Dimensions (W x H x D) 480 x 354 x 487 mmWeight 30 kgPower rating 1500 WTemperature range heating plate up to 150 ºCRotation speed 0 to 600 rpmEccentricity 0 to 10 mmProgrammable temperature 9 steps up to 9 h 59 min programs –20 ºC to +150 ºC24 V DC vacuum cover 120 W, max. 70 °C

Technical Data Syncore® Platform

ConnectionTTL for external on/off signal 24 V DC temperature-controlled valve 24 V DC cooling water valve (0.5 ºC hysteresis)

Applications for Syncore®

Syncore® improves workflow in multiple sample processing, such as evaporation of chromatography, extractions samples

(BUCHI B-811, SpeedExtraction, ASE, soxhlet), sample concentration for GC/MS, HPLC analyses and parallel SPE.

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