Metrohm Inline-Ultrafiltration User Manual

IC equipment
IC equipment: Inline-Ultrafiltration (6.5330.110)
Manual
8.110.8037EN / 2014-02-20
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: Inline-Ultrafiltration
(6.5330.110)
8.110.8037EN / 2014-02-20
Manual
zst
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.
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Table of contents

1 Introduction 1
1.1 Description of the IC equipment: Inline-Ultrafiltration ..... 1
1.2 About the documentation ................................................... 1
1.3 Symbols and conventions .................................................... 2
2 Overview 3
2.1 Parts of the IC equipment: Inline-Ultrafiltration ................ 3
2.2 Components of the ultrafiltration cell ................................ 3
2.3 Connectors of the ultrafiltration cell .................................. 4
2.4 Mode of operation for ultrafiltration .................................. 5
3 Installation 6
Table of contents
3.1 Preparing the ultrafiltration cell .......................................... 6
3.2 Connecting the ultrafiltration cell ..................................... 11
3.3 Inserting the ultrafiltration cell ......................................... 14
3.4 Deaerating the ultrafiltration cell ..................................... 16
4 Operation and maintenance 18
4.1 Operation ............................................................................ 18
4.1.1 Service life of the filtration membrane .................................... 18
4.1.2 Selecting the filtration membrane .......................................... 19
4.2 Maintenance ....................................................................... 20
5 Technical specifications 22
5.1 Ultrafiltration cell (6.2729.110) ......................................... 22
5.2 Filtration membrane (6.2714.020) .................................... 22
5.3 Dialysis membrane (6.2714.030) ....................................... 22
6 Accessories 23
Index 25
IC equipment: Inline-Ultrafiltration
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III

Table of figures

Table of figures
Figure 1 IC equipment: Inline-Ultrafiltration – Parts ......................................... 3
Figure 2 Ultrafiltration cell – Parts ................................................................... 3
Figure 3 Ultrafiltration cell – Connectors ......................................................... 4
Figure 4 Connecting the ultrafiltration cell ..................................................... 11
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IC equipment: Inline-Ultrafiltration
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1 Introduction

1 Introduction
1.1 Description of the IC equipment: Inline-Ultrafiltra­tion
The IC equipment: Inline-Ultrafiltration (6.5330.110) contains all accesso­ries required for Inline Ultrafiltration of difficult samples directly before injection.
The main component of the IC equipment: Inline-Ultrafiltration is the high-performance ultrafiltration cell. This cell is suitable for the filtration of samples that pose particular requirements with regard to filtration effec­tiveness and sample throughput.
The two channels of a peristaltic pump are required for pumping the sam­ple and the filtrate.

1.2 About the documentation

This manual describes the correct assembly and maintenance of the IC equipment: Inline-Ultrafiltration, the installation of the capillary connec­tions to and from the ultrafiltration cell and how to mount the holder on both the Sample Processor and the IC instrument.
The installation of the peristaltic pump is not described in this manual. This description can be found in the respective manuals for the ion chromato­graph or the Sample Processor.
CAUTION
Please read through this documentation carefully before putting the IC equipment: Inline-Ultrafiltration into operation. The documentation contains information and warnings which the user must follow in order to ensure safe operation of the IC equipment: Inline-Ultrafiltration.
IC equipment: Inline-Ultrafiltration
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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.
Method Dialog text, parameter in the software
File New Menu or menu item
[Next] Button or key
WARNING
This symbol draws attention to a possible life-threat­ening hazard or risk of injury.
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WARNING
This symbol draws attention to a possible hazard due to electrical current.
WARNING
This symbol draws attention to a possible hazard due to heat or hot instrument parts.
WARNING
This symbol draws attention to a possible biological hazard.
CAUTION
This symbol draws attention to possible damage to instruments or instrument parts.
NOTE
This symbol highlights additional information and tips.
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IC equipment: Inline-Ultrafiltration
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2 Overview

2.1 Parts of the IC equipment: Inline-Ultrafiltration

2 Overview

Figure 1 IC equipment: Inline-Ultrafiltration – Parts

2.2 Components of the ultrafiltration cell

Stoppers
1
IC equipment: Inline-Ultrafiltration
Figure 2
Ultrafiltration cell – Parts
Upper chamber
2
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3

2.3 Connectors of the ultrafiltration cell

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Sealing ring
3
Washers
5
Lower chamber
4
Screws
6
For joining the upper and the lower part of the cell.
2.3 Connectors of the ultrafiltration cell
Figure 3 Ultrafiltration cell – Connectors
Upper chamber
1
Lower chamber
2
Filtrate outlet
3
Labeled OUT.
Sample outlet
5
Labeled OUT.
Sample inlet
4
Labeled IN.
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IC equipment: Inline-Ultrafiltration
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2.4 Mode of operation for ultrafiltration

2 Overview
The peristaltic pump delivers a continuous flow of sample solution at a high rate through the lower chamber of the ultrafiltration cell. The sample flows along the filtration membrane and then to the waste container.
At the same time, the peristaltic pump's second channel generates a vac­uum in the upper chamber of the ultrafiltration cell, thus pulling the sam­ple solution through the filtration membrane. The filtrate reaches the sam­ple loop and is then injected.
Less than 20% of the original sample solution volume is analyzed as fil­trate. The remainder flows directly into the waste container.
IC equipment: Inline-Ultrafiltration
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3.1 Preparing the ultrafiltration cell

3 Installation

This chapter describes how to assemble the ultrafiltration cell, how to fas­ten the ultrafiltration cell to the Sample Processor or in the ion chromato­graph and how to connect the ultrafiltration cell to the peristaltic pump and the injection valve.
Depending on the device combination, the ultrafiltration cell may be placed at different locations. Please observe the following recommenda­tions:
Devices Peristaltic pump Ultrafiltration cell
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Sample Processor with peristaltic pump and ion chromatograph
Only ion chromatograph, type Prep 1
Only ion chromatograph with peristaltic pump
on the Sample Processor on the Sample Processor
on the ion chromatograph on the ion chromatograph
on the ion chromatograph in the detector chamber of
3.1 Preparing the ultrafiltration cell
You have to insert a filtration membrane (6.2714.020) before you can insert the ultrafiltration cell.
the ion chromatograph with cell holder (6.2057.120)
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IC equipment: Inline-Ultrafiltration
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Inserting the filtration membrane
Required tools Ultrafiltration cell (6.2729.110)
Filtration membrane (6.2714.020) Hex key (6.2621.070) Tweezers (6.2831.010)
1
Removing the stoppers
3 Installation
Remove the three green stoppers. Turn the ultrafiltration cell around and place it on a table. The
screws face upwards.
2
Removing the screws
Loosen the screws with the hex key. Remove the screws with the washers and put them aside.
IC equipment: Inline-Ultrafiltration
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3.1 Preparing the ultrafiltration cell
3
Disassembling the ultrafiltration cell
Remove the upper part of the ultrafiltration cell. Remove the sealing ring.
4
Cleaning the ultrafiltration cell
CAUTION
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Damage to the ultrafiltration cell
Organic solvents (e.g. acetone) corrode and damage the ultrafiltra­tion cell material (PMMA).
Use only ultrapure water or a water-ethanol mixture (70:30) for
cleaning the ultrafiltration cell.
Thoroughly rinse off the sealing ring (2-3), the upper chamber
(2-2) and the lower chamber (2-4) of the ultrafiltration cell with
ultrapure water.
Dry all parts with a lint-free cloth.
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IC equipment: Inline-Ultrafiltration
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Wetting the filtration membrane
NOTE
In the package containing the filtration membranes, you will find sheets of different thicknesses and colors:
The firm white cardboard is a cover protecting the filtration
membranes. Do not place it in the ultrafiltration cell.
The thin light-blue sheets are separation sheets placed between
two filtration membranes. Do not place them in the ultrafiltra­tion cell.
The thin white sheets are the filtration membranes. Use only
these for ultrafiltration.
3 Installation
Using the tweezers, take a new filtration membrane out of the
package.
Place the filtration membrane in a petri dish filled with ultrapure
water and allow to hydrate for approx. two minutes.
6
Inserting the filtration membrane
NOTE
Make sure that the water-soaked filtration membrane does not dry out before it is inserted, as it can otherwise no longer be used!
Place the sealing ring back in the recess.
■ ■ Using the tweezers, place the wet filtration membrane centrally
inside the sealing ring onto the cell.
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3.1 Preparing the ultrafiltration cell
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Assembling the ultrafiltration cell
Place the upper part of the ultrafiltration cell on the lower part in
such a way that the two guide bolts fit exactly into the two bore holes.
8
Screwing the ultrafiltration cell together
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10
Screw the five screws with the washers in the ultrafiltration cell by
hand first.
Then firmly tighten them with the hex key in crosswise sequence.
IC equipment: Inline-Ultrafiltration
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3.2 Connecting the ultrafiltration cell

This chapter describes how to establish the capillary connections of the fil­tration system (regardless of whether the filtration cell is installed on the Sample Processor or in the ion chromatograph). 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 Sam- ple Processor or the ion chromatograph for this information.
The following figure shows a schematic overview of all capillary connec­tions of the filtration system.
3 Installation
Required accessories
Figure 4
Connecting the ultrafiltration cell
NOTE
In order to keep dead volume to a minimum, make sure that the
capillaries are as short as possible.
The capillaries that are used for transferring the filtrate are thinner
than the capillaries used for transferring the sample.
To prevent the capillaries leading into the ion chromatograph from
being pinched, always guide them through the capillary feed­throughs provided for this purpose (see the manual for the ion chro- matograph).
Connecting the ultrafiltration cell
Ultrafiltration cell (6.2729.110) PTFE capillary, 0.5 mm ID / 20 cm (6.1803.050) PTFE capillary, 0.97 mm ID / 20 cm (6.1803.060) PTFE capillary, 0.97 mm ID / 1 m (6.1803.080)
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3.2 Connecting the ultrafiltration cell
Pump tubing LFL (orange/yellow), 3 stoppers (6.1826.320) Pump tubing LFL (yellow/yellow), 3 stoppers (6.1826.390) PEEK capillary, 0.5 mm ID / 1 m (6.1831.060) PEEK capillary, 0.5 mm ID / 70 cm (6.1831.160) Pressure screw PVDF (6.2744.000) Coupling olive/UNF 10/32 (6.2744.030) Pressure screw, short (6.2744.070) Pump tubing connection with locking nut (6.2744.160)
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1
Preparing the pump tubing for the sample
Use the pump tubing with yellow stoppers (6.1826.390) for convey­ing the sample.
Attach the coupling olive/UNF 10/32 (6.2744.030) to the inlet. Attach the pump tubing connection with locking nut
(6.2744.160) to the outlet (see chapter "Installing the peristaltic pump" in the manual for the ion chromatograph or in the man­ual for the Sample Processor).
2
Preparing the pump tubing for the filtrate
Use the pump tubing with orange/yellow stoppers (6.1826.320) for conveying the filtrate.
Attach the coupling olive/UNF 10/32 (6.2744.030) to the inlet. Attach the pump tubing connection with locking nut
(6.2744.160) to the outlet (see chapter "Installing the peristaltic pump" in the manual for the ion chromatograph or in the man­ual for the Sample Processor).
3
Connecting the capillaries to the pump tubing for the sample
Tighten the PEEK capillary (6.1831.160) to the inlet of the pump
tubing with yellow stoppers (6.1826.390) using a pressure screw (6.2744.070).
Tighten the PTFE capillary (6.1803.060) to the outlet of the pump
tubing with yellow stoppers (6.1826.390) using a pressure screw (6.2744.070).
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3 Installation
4
Connecting the capillaries to the pump tubing for the filtrate
Tighten the PTFE capillary (6.1803.050) to the inlet of the pump
tubing with orange/yellow stoppers (6.1826.320) using a pressure screw (6.2744.070).
Tighten the PEEK capillary (6.1831.060) to the outlet of the pump
tubing with orange/yellow stoppers (6.1826.320) using a pressure screw (6.2744.070).
5
Connecting capillaries to the ultrafiltration cell
CAUTION
Use only PVDF pressure screws (6.2744.000) to tighten capillaries to the ultrafiltration cell.
PEEK pressure screws are too hard and could damage the ultrafil­tration cell material.
Tighten the PTFE capillary (6.1803.060) to the inlet labeled IN of
the ultrafiltration cell's lower chamber using a PVDF pressure screw (6.2744.000).
Tighten the PTFE capillary (6.1803.080) to the outlet labeled OUT
of the ultrafiltration cell's lower chamber using a PVDF pressure screw (6.2744.000).
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3.3 Inserting the ultrafiltration cell

Tighten the PTFE capillary (6.1803.050) to the outlet labeled OUT
of the ultrafiltration cell's upper chamber using a PVDF pressure screw (6.2744.000).
6
Connecting the remaining capillaries
Tighten the free end of the PEEK capillary (6.1831.160) to the
needle of the Sample Processor (see manual for the Sample Pro­cessor).
Tighten the free end of the PEEK capillary (6.1831.060) to Port 1
of the injection valve in the ion chromatograph (see manual for the ion chromatograph).
Either tighten the free end of the PTFE capillary (6.1803.080) to
the waste collector or guide it directly to the waste container and tighten it there.
3.3 Inserting the ultrafiltration cell
The ultrafiltration cell can be fastened either to the Sample Processor or in the ion chromatograph.
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Required accessories
Fastening the ultrafiltration cell to the Sample Processor
Filtration cell holder (6.2057.030) Ultrafiltration cell (6.2729.110)
1
Attaching the holder
Tighten the filtration cell holder (6.2057.030) to the IC Sample Pro­cessor (see manual for the IC Sample Processor).
2
Inserting the ultrafiltration cell
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IC equipment: Inline-Ultrafiltration
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Insert the ultrafiltration cell in such way that the screw heads are
located in the holes in the filtration cell holder provided for this purpose.
Inserting the ultrafiltration cell in the ion chromatograph
Required accessories Filtration cell holder (6.2057.140)
Ultrafiltration cell (6.2729.110)
1
Hanging in the holder
3 Installation
Hang the filtration cell holder (6.2057.140) in the holding device
in the ion chromatograph provided for this purpose.
2
Inserting the ultrafiltration cell
Insert the ultrafiltration cell in such way that the screw heads are
located in the holes in the filtration cell holder provided for this purpose.
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3.4 Deaerating the ultrafiltration cell

3.4 Deaerating the ultrafiltration cell
Every time a new filtration membrane is inserted, the air which may still be present in the filtration cell and in the capillaries must be removed. To accomplish this, rinse out all capillaries with e.g. ultrapure water.
NOTE
The entire filtration system must be completely connected prior to the rinsing procedure.
Rinsing the ultrafiltration cell
1
Settings in the software
Immerse the needle of the Sample Processor into the rinsing solu-
tion.
Switch on the peristaltic pump. Rinse the filtration system with ultrapure water for approx. 5 min.
2
Monitoring the rinsing process
Check whether equal amounts of solution are emerging from
both feed lines to the waste container.
Check whether all the capillary connections from the rinsing solu-
tion through the peristaltic pump and the ultrafiltration cell are leak-tight all the way to the waste container. If liquid is escaping somewhere, then tighten the corresponding connection or redo the connection.
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IC equipment: Inline-Ultrafiltration
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3 Installation
Check whether any air bubbles remain trapped in the ultrafiltra-
tion cell. If air bubbles are trapped in the cell, then unscrew the PTFE capil­laries from the filtrate outlet (3-3) and from the sample outlet (3-5) and wait until the air bubbles have escaped. Afterwards, tighten the capillaries to the ultrafiltration cell again.
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4.1 Operation

4 Operation and maintenance

4.1 Operation

4.1.1 Service life of the filtration membrane

One of the most commonly encountered problems in filtration is that solid substances in the sample are deposited on the filtration membrane, caus­ing it to become blocked over time. The ultrafiltration cell has been designed so as to prevent this effect to the extent possible. It has a sym­metrical design and is placed horizontally in the Sample Processor or in the ion chromatograph. The sample flows through the lower chamber of the ultrafiltration cell and the filtrate is aspirated from the top. In this way, solid substances adhere less to the membrane.
Nevertheless, depending on the level and type of contamination in the sample, the filtration process must be monitored and the filtration mem­brane replaced if necessary.
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A declining recovery rate in standard solution analyses is an indicator for an imminent blockage of a filtration membrane. These standard solutions should ideally be prepared with the sample matrix to be analyzed.
If a large number of samples is analyzed, we recommend measuring check standards regularly (in the case of samples with high particle loads, after every 5th to 10th sample). No general prediction regarding the number of filtration cycles can be made. Also, the change in the recovery rate may be different with more samples being analyzed. Whereas the recovery rate with one sample matrix may remain constant over many samples and then suddenly drop off severely, its decline may be slow and continuous with a different sample composition.
At which time a filtration membrane needs to be replaced depends on the sample matrix and the specifications of the analysis method applied. Expe­rience has shown that minuscule particles and suspended substances in the sample matrix will lead to blockage of the filtration membrane faster than coarser particles will, because the latter will be more readily propel­led past the membrane in the flow of sample material.
The following table lists some sample types that were filtered with the ultrafiltration cell (6.2729.110) and a filtration membrane (6.2714.020) with a pore size of 0.2 µm and subsequently analyzed on a Metrohm ion chromatograph. The concentration of the following seven anions was determined for each sample type: F–, Cl–, NO
, Br–, NO
2
, HPO
3
2–
4
, SO
2–
.
4
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4 Operation and maintenance
Table 1 Filtration of various samples
Sample designation Number of samples per filter
Orange juice with fruit pulp 40
Surface water 500
Drinking water 1,000
Ground water 500
Waste water 1 1,000
Waste water 2 130
Waste water 3 40
Waste water 4 80
NaCl solution (1%) 5,000
Schöniger absorption solution 100
Acidic earth extracts 1,000
Aqueous earth extracts 200

4.1.2 Selecting the filtration membrane

You can apply existing sample preparation procedures to the Metrohm ultrafiltration cell (6.2729.110). If you wish to use a different filtration membrane than the one supplied, please note that, even if the particle size is known, selecting a membrane with a suitable pore size does not automatically yield the desired results.
Our investigations have shown that the retention capacity of conventional filtration membranes does not always correspond to their specified pore size. The following table shows the qualitative filtration action of filtration membranes with different nominal pore sizes. Aqueous solutions contain­ing silica particles with particle sizes of 1.5 µm and 5 µm were used in the test.
Table 2
Test solutions: silica particles in water
0.5%, 5 µm 0.15 µm no permeation
0.5%, 5 µm 3 µm no permeation
0.5%, 5 µm 8 µm no permeation
0.5%, 5 µm 10 µm permeation
Selection of the filtration membrane
Pore size of the filtration membrane
Effect
1
2
IC equipment: Inline-Ultrafiltration
0.5%, 5 µm 12 µm no permeation
0.5%, 1.5 µm 0.15 µm no permeation
0.5%, 1.5 µm 3 µm permeation
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4.2 Maintenance

1
Nominal pore size according to manufacturer's statement.
2
Except for this membrane, all membranes were from the same manufac-
turer.
Please also note that because of the lower filter thickness the retention capacity of filtration membranes may be lower than that of filters with the same pore size but a higher filter thickness. You should take this into account when selecting an appropriate filtration membrane.
4.2 Maintenance
The filtration membranes used have to be in perfect condition in order to enable a consistent quality of the analysis results. Therefore, this mem­brane has to be replaced at regular intervals.
Additional information on estimating when a filtration membrane needs to be replaced can be found in Chapter 4.1.1.
Replacing the filtration membrane
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1
Taking the ultrafiltration cell out of the system
In the software, stop the system and wait until the pressure has
been released.
Remove all capillaries from the ultrafiltration cell. Take the ultrafiltration cell out of the holder.
2
Cleaning the ultrafiltration cell
Carry out steps 2 to 8 in the instructions Inserting the filtration
membrane on page 7.
3
Connecting capillaries to the ultrafiltration cell
CAUTION
Damage to the ultrafiltration cell caused by using the wrong pressure screws
PEEK pressure screws are too hard and could damage the ultrafil­tration cell material.
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Use only PVDF pressure screws (6.2744.000) to tighten capilla-
ries to the ultrafiltration cell.
IC equipment: Inline-Ultrafiltration
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4 Operation and maintenance
Tighten the PTFE capillary (6.1803.060) to the inlet labeled IN of the ultrafiltration cell's lower chamber using a PVDF pressure screw (6.2744.000).
Tighten the PTFE capillary (6.1803.080) to the outlet labeled OUT
of the ultrafiltration cell's lower chamber using a PVDF pressure screw (6.2744.000).
Tighten the PTFE capillary (6.1803.050) to the outlet labeled OUT
of the ultrafiltration cell's upper chamber using a PVDF pressure screw (6.2744.000).
4
Inserting the ultrafiltration cell into the holder
Place the ultrafiltration cell back in the holder (see Chapter 3.3,
page 14).
5
Deaerating the ultrafiltration cell
Carry out all steps contained in the instructions Rinsing the ultrafiltra­tion cell on page 16.
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5.1 Ultrafiltration cell (6.2729.110)

5 Technical specifications

5.1 Ultrafiltration cell (6.2729.110)
Material PMMA (poly(methyl methacrylate))
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Solvent compati­bility
Cell volume 240 µL (each from inlet to outlet opening)
Water or water-ethanol mixture (70:30) (no other organic solvents)

5.2 Filtration membrane (6.2714.020)

Pore diameter
Membrane diame­ter
Material Regenerated cellulose
0.2 µm
47 mm

5.3 Dialysis membrane (6.2714.030)

Pore diameter
Membrane diame­ter
Material Polyamide
0.2 µm
47 mm
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6 Accessories
Up-to-date information on the scope of delivery and optional accessories for your instrument can be found on the Internet.
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.
Instruments currently sold
If you do not know the article number of your instrument, proceed as fol­lows:
Downloading the accessories list

6 Accessories

NOTE
Go to the Metrohm website http://www.metrohm.com/com.
1
2
Click on .
The Search webpage will be displayed.
Enter a search term relating to the instrument into the search field
3
and click on Find.
The search results will be displayed.
In the search results, select the Devices tab (if it is not already
4
selected) and then click on the Metrohm article number of the required instrument (e.g. 2.852.0050).
The page with information pertaining to the searched article is dis­played.
Select the Parts tab.
5
The complete list of accessories with the scope of delivery and the optional accessories will be displayed.
6
Click on .
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The Partslists webpage will be displayed.
Select the desired output language.
7
With the article number entered, click on the command Generate
8
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. Using the article number, you can download accessories lists for all instruments as follows:
Downloading the accessories list
Type http://partslists.metrohm.com into your Internet browser.
1
The Partslists webpage will be displayed.
Select the desired output language.
2
Enter the article number and click on the Generate PDF command.
3
The PDF file with the accessories data will be created in the language selected.
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Index

Index
C
Capillary connections ................ 11
F
Filtration membrane
Assembly .............................. 6
Replace .............................. 20
Select ................................. 19
Service life .......................... 18
I
Installation ................................. 6
M
Maintenance ............................ 20
O
Operation ................................. 18
T
Technical specifications ............ 22
U
Ultrafiltration
Mode of operation ............... 5
Ultrafiltration cell
Components ........................ 3
Connect ............................. 11
Connectors ........................... 4
Deaerate ............................ 16
Insert .................................. 14
Rinse .................................. 16
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