IC equipment IC equipment: Dialysis (6.5330.100) Manual 8.110.
Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com IC equipment IC equipment: Dialysis (6.5330.100) Manual 8.110.
Teachware Metrohm AG CH-9100 Herisau teachware@metrohm.com This documentation is protected by copyright. All rights reserved. Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above. Documentation in additional languages can be found on http://documents.metrohm.com.
■■■■■■■■■■■■■■■■■■■■■■ Table of contents Table of contents 1 Introduction 1 1.1 Description of the IC equipment: Dialysis .......................... 1 1.2 About the documentation ................................................... 1 1.3 Symbols and conventions .................................................... 2 2 Overview 3 2.1 Parts of the IC equipment: Dialysis ..................................... 3 2.2 Parts of the dialysis cell .......................................................
■■■■■■■■■■■■■■■■■■■■■■ Table of figures Table of figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 IV ■■■■■■■■ IC equipment: Dialysis – Parts ............................................................ 3 Dialysis cell – Parts ............................................................................. 4 Dialysis cell – Connectors ................................................................... 4 Stopped-flow dialysis .........................................................................
■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction 1 Introduction 1.1 Description of the IC equipment: Dialysis The IC equipment: Dialysis (6.5330.100) contains all accessories required for inline dialysis of matrix-contaminated samples (e.g. emulsions, samples containing fat and protein, body fluids or waste waters with high pollution loads) directly before injection. The main component of the IC equipment: Dialysis is the high-performance dialysis cell.
■■■■■■■■■■■■■■■■■■■■■■ 1.3 Symbols and conventions 1.3 Symbols and conventions The following symbols and formatting may appear in this documentation: Cross-reference to figure legend The first number refers to the figure number, the second to the instrument part in the figure. Instruction step Carry out these steps in the sequence shown.
■■■■■■■■■■■■■■■■■■■■■■ 2 Overview 2 Overview 2.
■■■■■■■■■■■■■■■■■■■■■■ 2.2 Parts of the dialysis cell 2.2 Parts of the dialysis cell Figure 2 Dialysis cell – Parts 1 Stoppers 2 Left chamber 3 Sealing ring 4 Right chamber 5 Washers 6 Screws For joining the right and the left chamber. 2.
■■■■■■■■■■■■■■■■■■■■■■ 2.4 2 Overview Mode of operation for dialysis Figure 4 Stopped-flow dialysis Sample is delivered continuously on the sample side of the dialysis cell. After a rinsing phase, the acceptor flow is stopped. Because of the concentration gradient, the ions pass through the membrane. The acceptor flow remains stationary until a concentration equilibrium is achieved between the two cell halves.
■■■■■■■■■■■■■■■■■■■■■■ 3.1 Preparing the dialysis cell 3 Installation This chapter describes the assembly and connection of the dialysis cell and the conditioning of the dialysis system. Depending on the ion chromatograph, the dialysis cell may be placed at different locations. Please observe the following recommendations: ■ ■ 3.1 If you are working with an ion chromatograph that has a peristaltic pump and a cell holder, then place the dialysis cell in the cell holder.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Loosen the screws with the hex key. Remove the screws with the washers and put them aside. ■ ■ 3 Disassembling the dialysis cell Remove the upper part of the dialysis cell. Remove the sealing ring. ■ ■ 4 Cleaning the dialysis cell CAUTION Damage to the dialysis cell Organic solvents (e.g.: acetone) corrode and damage the dialysis cell material (PMMA).
■■■■■■■■■■■■■■■■■■■■■■ 3.1 Preparing the dialysis cell 5 Wetting the dialysis membrane NOTE In the package containing the dialysis membranes, you will find sheets of different thicknesses and colors: ■ ■ ■ ■ ■ The firm white cardboard is a cover protecting the filtration membranes. Don not place it in the dialysis cell. The thin light-blue sheets are separation sheets placed between two filtration membranes. Do not place them in the dialysis cell. The thin white sheets are the dialysis membranes.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation ■ Using the tweezers, place the wet dialysis membrane centrally inside the sealing ring onto the cell. 7 Assembling the dialysis cell ■ Place the upper part of the dialysis cell on the bottom part in such a way that the two guide bolts fit exactly into the two bore holes. 8 Screwing the dialysis cell together ■ ■ IC equipment: Dialysis Screw the five screws with the washers in the dialysis cell by hand first.
■■■■■■■■■■■■■■■■■■■■■■ 3.2 Connecting the dialysis cell 3.2 Connecting the dialysis cell This chapter describes how to establish the capillary connections of the dialysis system. It does not, however, describe the tubing configuration for the peristaltic pump. Please refer to the chapter "Installing the peristaltic pump" in the manual for the Sample Processor or the ion chromatograph for this information. Connections for acceptor solution Required accessories ■ ■ ■ ■ ■ ■ ■ ■ ■ ■ Dialysis cell (6.2729.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation The acceptor solution is pumped with two pump tubings with yellow/ orange stoppers (6.1826.320). Additional information on the tubing configuration of the peristaltic pump can be found in the chapter "Installing the peristaltic pump" in the manual for your ion chromatograph. 1 Preparing two pump tubings for the sample Use the two pump tubings with black stoppers (6.1826.340) for conveying the sample.
■■■■■■■■■■■■■■■■■■■■■■ 3.2 Connecting the dialysis cell ■ Tighten a PTFE capillary, 0.5 mm ID / 1 m (6.1803.040), to the outlet of the pump tubing with black stoppers (6.1826.340) using a pressure screw (6.2744.070). Tighten the other end of the PTFE capillary to the sample inlet of the dialysis cell (3-4) using a pressure screw (6.2744.000). 4 Connecting the sample outlet ■ ■ Tighten a PTFE capillary, 0.5 mm ID / 1 m (6.1803.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation ■ ■ Tighten a PTFE capillary (6.1803.040) to the inlet of the pump tubing with orange/yellow stoppers (6.1826.320) using a pressure screw (6.2744.070). Immerse the other end of the PTFE capillary in the vessel containing the acceptor solution (6.1808.070 with 6.1602.150) and fasten with a PVDF pressure screw (6.2744.000). Tighten another PTFE capillary (6.1803.040) to the outlet of the pump tubing with orange/yellow stoppers using a pressure screw (6.2744.070).
■■■■■■■■■■■■■■■■■■■■■■ 3.3 Inserting the dialysis cell 3.3 Inserting the dialysis cell Inserting the dialysis cell into the ion chromatograph 1 ■ Insert the dialysis cell into the cell holder provided for this purpose. Inserting the dialysis cell into the cell holder If the ion chromatograph is not equipped with a cell holder, then the dialysis cell with the dialysis cell holder (6.2057.130) has to be used. 1 ■ ■ 14 ■■■■■■■■ Insert the dialysis cell into the dialysis cell holder (6.2057.130).
■■■■■■■■■■■■■■■■■■■■■■ 3.4 3 Installation Conditioning the dialysis system Prior to the first analysis, the dialysis cell with dialysis membrane in place and all capillaries must be rinsed with ultrapure water. 1 Setting the injection valve Set the injection valve to the FILL position in the software. 2 Putting both peristaltic pumps into operation ■ ■ ■ Immerse the aspiration capillary in the acceptor solution (degassed ultrapure water). Use the software to switch on both peristaltic pumps.
■■■■■■■■■■■■■■■■■■■■■■ 4.1 Operation 4 Operation and maintenance 4.1 Operation 4.1.1 Optimizing the dialysis Determining the rinsing time A rinsing time of two minutes is usually sufficient for completely rinsing the sample and the acceptor channel. If necessary, this time can be extended.
■■■■■■■■■■■■■■■■■■■■■■ 4 Operation and maintenance 12.0 Fluoride Fluoride Chloride Chloride 10.0 Nitrite Nitrite Area [µS/cm*min] 8.0 Bromide Bromide Nitrate Nitrate 6.0 Phosphate Phosphate 4.0 Sulfate Sulfate 2.0 0.0 10 15 20 25 30 35 40 45 Transfer time [sec] Figure 5 Area / transfer time diagram According to this curve, the optimum transfer time is between 27 and 32 seconds.
■■■■■■■■■■■■■■■■■■■■■■ 4.1 Operation 2 Measuring the standard solution with dialysis ■ ■ ■ Set the dialysis time in the software to 5 minutes. Immerse the sample aspiration capillary in the standard solution used in step 1. Start a determination in the software and wait until the chromatogram has been evaluated. 3 Additional measurements ■ ■ Increase the dialysis time in the software by 1 minute each time and start the determination. Repeat the measurements until the measured values are stable.
■■■■■■■■■■■■■■■■■■■■■■ 4 Operation and maintenance 4 Putting the dialysis system into operation ■ ■ ■ ■ Immerse the aspiration capillary for the acceptor solution in the acceptor solution. Immerse the sample aspiration capillary in a rinsing solution (e.g. ultrapure water). Start both peristaltic pumps in the software. Rinse the dialysis system with the acceptor solution and the rinsing solution for approx. 10 minutes and then switch off the peristaltic pumps again.
■■■■■■■■■■■■■■■■■■■■■■ 4.2 Maintenance 4.2 Maintenance The dialysis membrane may need to be replaced: ■ ■ ■ ■ if the signal intensity during dialysis decreases. if the dialysis membrane dries out. if the dialysis membrane becomes damaged as a result of depositions or bacterial growth. if the sample channel is blocked (i.e., the sample can no longer be pumped through the dialysis cell).
■■■■■■■■■■■■■■■■■■■■■■ 5 Technical specifications 5 Technical specifications 5.1 Dialysis cell (6.2729.100) Material PMMA (poly(methyl methacrylate)) Solvent compatibility Water or water-ethanol mixture (70:30) (no other organic solvents) Cell volume 240 µL (each from inlet to outlet opening) 5.2 Dialysis membrane (6.2714.010) Pore diameter 0.20 µm Membrane diameter 47 mm Material Cellulose acetate 5.3 Dialysis membrane (6.2714.030) Pore diameter 0.
■■■■■■■■■■■■■■■■■■■■■■ 6 Accessories Up-to-date information on the scope of delivery and optional accessories for your instrument can be found on the Internet. NOTE When you receive your new instrument, we recommend downloading the accessories list from the Internet, printing it out and keeping it together with the manual for reference purposes.
■■■■■■■■■■■■■■■■■■■■■■ 6 Accessories The Partslists webpage will be displayed. 7 Select the desired output language. 8 With the article number entered, click on the command Generate PDF. The PDF file with the accessories data will be created in the language selected. Direct access for all instruments If you are unable to find your instrument using the search as described above, this may be due to the instrument not being sold anymore.
■■■■■■■■■■■■■■■■■■■■■■ Index Index C Capillary connections ................ 10 Connections ............................. 10 D Dialysis Carry out ............................ 18 Mode of operation ............... 5 Optimize ............................ 16 Dialysis cell Connectors ........................... 4 Parts ..................................... 4 Prepare ................................. 6 24 ■■■■■■■■ Dialysis system Condition ........................... 15 Connect .............................