2060 IC MARGA

Application Manual
Metrohm Applikon B.V.
Schiedam
The Netherlands
Phone +31 (0)10-2983555
Fax +31 (0)10-4379648
041-info@metrohm.com
www.metrohm.com/en/products/process-analyzers/

2060 IC MARGA

Application Manual

/
November 2020
Rob Proost
Metrohm Applikon B.V.
Schiedam

© 2020, Metrohm Applikon B.V.

All rights reserved. This manual is protected by copyright law. Without the prior written approval of
Metrohm Applikon B.V., this manual and any contents thereof may not be reproduced, stored or
made public in any form by any means.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents

Table of contents
1 General description 1
1.1 Safety Instructions ................................................................ 1
1.1.1 General notes on safety ........................................................... 1
1.1.2 Electrical safety ........................................................................ 1
1.1.3 Working with glass analyzer parts ............................................ 2
1.1.4 Tubing and capillary connections ............................................. 3
1.1.5 Potentially hazardous solvents and chemicals ........................... 3
1.1.6 Recycling and disposal ............................................................. 4

2 Analysis 5
2.1 Operating Principle ............................................................... 5
2.2 Eluents and Reagents ........................................................... 8
2.2.1 Chemicals and Apparatus ........................................................ 9
2.2.2 Cleaning procedure containers ............................................... 10
2.2.3 Eluents .................................................................................. 11
2.2.4 Reagents ............................................................................... 12
2.2.5 Internal Standard ................................................................... 13

3 Hardware 15
3.1 Analyzer Cabinets ............................................................... 15

4 Program 19
4.1 Program ............................................................................... 19

5 Typical results 20
5.1 Retention times (t R ) ......................................................... 20
5.2 Typical Chromatograms ..................................................... 21

6 Maintenance schedule 23
6.1 Maintenance schedule ....................................................... 23
6.2 Eluent replacement ............................................................. 24
6.3 Reagent and Standard replacement ................................. 26

7 Troubleshooting 28
7.1 Bacterial growth ................................................................. 28
7.2 Missing or no peaks in chromatograms ........................... 29
7.3 Anion IC - Anion Chromatograms ..................................... 31
7.4 Cation IC - Cation Chromatograms ................................... 32

￭￭￭￭￭￭￭￭ III

2060 IC
 Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

8 Appendix 33
8.1 Extension 2060 MARGA standard application with Flu-
oride ..................................................................................... 33
8.2 Wet rotating denuder module (V2LH000343) ................. 39
8.3 Steam jet aerosol collector module (V2LH000022) ......... 43
8.4 Ion chromatography ........................................................... 48

IV ￭￭￭￭￭￭￭￭

2060 IC
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ General description

1 General description

1.1 Safety Instructions

1.1.1 General notes on safety

WARNING

This analyzer may only be operated in accordance with the

specifications in this documentation.

WARNING

The end user is responsible for identification and, if possible,

mitigation of specific hazards that are outside the responsibil-
ity of Metrohm Applikon.

This analyzer has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
analyzer, the following instructions must be observed carefully.

1.1.2 Electrical safety

All relevant safety measures are to be observed when working with equip-
ment.

WARNING

Only personnel qualified by Metrohm Applikon are authorized

to carry out service work on the analyzer.

WARNING

Only connect the analyzer to other equipment that is in com-

pliance with the appropriate directives (i.e.: LVD, EMC etc.).

￭￭￭￭￭￭￭￭ 1
 Safety Instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

WARNING

If the analyzer is connected to ICT equipment, this equipment

should be in compliance with the EN 60950-1 incl. all (recent)
amendments.

Mains voltage

WARNING

Only operate the analyzer with a mains voltage specified for it

(see the analyzer identification plate).

Protection against electrostatic discharge

CAUTION

Always take ESD precautions.

The electronic components are sensitive to electrostatic charges and
can be destroyed by discharges.

1.1.3 Working with glass analyzer parts

All relevant safety measures are to be observed when working with equip-
ment.

WARNING

Broken glass and other sharps are physical hazards.

WARNING

Broken glass also has the potential to be a health hazard if it is

contaminated with toxic chemicals substances which may
enter the body through a cut or puncture.

2 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ General description

1.1.4 Tubing and capillary connections

CAUTION

Leaks in tubing and tubing connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing
connections. Damaged tubing ends lead to leakage. Appropriate
tools can be used to tighten or loosen connections.
Check the connections regularly for leakage. If the analyzer is used
mainly in unattended operation, then weekly inspections are manda-
tory.

1.1.5 Potentially hazardous solvents and chemicals

WARNING

This analyzer uses chemical reagents, the type of chemical

reagents depends on the analysis procedure (reagent specifica-
tions can be found in the dedicated application manual). You
should observe all relevant safety measures according to local
regulations when working with these chemicals. Before using
the chemical reagents, take the available Material Safety Data
Sheet (MSDS) and other relevant safety information into
account. Also, make use of the appropriate (personal) protec-
tive equipment.

WARNING

Depending on the analysis procedure and/or local regulations,

it can be possibe that the analyzer should be placed in a venti-
lated environment (e.g. (walk in) fume hood).

WARNING

Do not use flammable liquids inside the wet part of the ana-
lyzer and avoid the generation of flammable gasses due to
chemical reactions.

￭￭￭￭￭￭￭￭ 3
 Safety Instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

1.1.6 Recycling and disposal

This product is covered by European Directive 2012/19/EU, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

4 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Analysis

2 Analysis

2.1 Operating Principle

The 2060IC MARGA is a fully autonomous sampling and measurement
system that continuously measures the water-soluble gas and aerosol
components that have a direct effect on air quality. These results can then
be used to study the formation of aerosols from their precursor gases and
how their concentration and composition vary with diurnal and seasonal
cycles.
Table 1 Monitored Gases and Aerosols
Gases Aerosols
HCl Cl-
HNO2 (HONO) NO3-
HNO3 SO42-
NH3 K+
SO2 Na+
NH4+
Ca2+
Mg2+

The following scheme shows the air flow and liquid flow path of the
2060IC MARGA. The green lines represent the air flow, the blue lines the
liquid flow.

￭￭￭￭￭￭￭￭ 5
 Operating Principle ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Figure 1 Schematic overview 2060IC MARGA

An air pump in combination with a critical orifice draws ambient air with
an airflow of 1 m3per hour (optional 0.5 m3/h) into the wet part cabinet.
The maximum size of particulate matter (PM) can be selected by placing a
size selective inlet (e.g. PM10, PM2.5 or PM1.0) in front of the Wet Rotat-
ing Denuder (WRD) inlet.
The air enters the Wet Rotating Denuder (WRD) where acidic gases and
ammonia are collected by diffusion into a liquid film. Aerosols will not be
absorbed because of their higher mass and will travel through the
denuder. The level of liquid film within the WRD is kept constant using a
level sensor and a tubing pump fed by an absorbance solution. The liquid
level is kept constant to ensure equilibrium between the gas and liquid
phase. From the WRD the air flows into the Steam Jet Aerosol Collector
(SJAC) which is directly connected to the WRD.

6 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Analysis

Within the SJAC, a supersaturated steam environment is created using a

steamer. The super saturated environment causes particles to grow by a
process known as deliquescence, the particles are collected by inertial sep-
aration. The particles, independent of size, grow by the condensated
steam till 2-3 micron. These droplets are transferred from air to liquid by
the cyclone behind the steamer chamber.
The liquid from both the denuder/WRD and SJAC is collected in two sepa-
rate 20 ml burette modules (called Denuder and SJAC), which are located
directly below the WRD and SJAC. These burettes collect 15 ml of liquid
sample, add 1.5 ml internal standard and transport the liquid at the end of
the cycle (default 1 hour) to the WRD and SJAC Sampling Mixing Vessel
Module, where the sample and internal standard are mixed and homo-
genized by 10 ml air.
97% of the cycle time the burettes collect sample and the remaining 3%
the burettes transfer the sample with internal standard to the pipettes.
During the 3% of the time the airpump WRD and SJAC are still active, so
100% of the cycle time liquid sample is collected from the air.
In the next cycle the IC burette transports the WRD and SJAC samples to
the cation and anion Ion chromatographs (IC’s) for analysis. During this
time, the WRD and SJAC burettes collect the next sample of this hour.
The anion and cation IC measures the following anions and cations,
expressed here as gases or aerosols:
Table 2 Anions and cations expressed as gases (WRD)
Measured cation and anion by IC Expressed gas
Cl- HCl
NO2- HNO2 (HONO)
NO3- HNO3
SO4-(*) SO2
NH4+ NH3
(*)Theabsorbance solution contains hydrogen peroxide. When sulfur diox-
ide gas diffuses into the absorbance liquid the following two reactions
occur:
￭ Reaction 1: SO2 + H2O →H2SO3
￭ Reaction 2: H2SO3 + H2O2→H2SO4 + H2O
￭ Hydrogen peroxide must be present in the absorbance solution; other-
wise the second reaction will not occur completely.
Table 3 Anions and cations expressed as aerosols (SJAC)

￭￭￭￭￭￭￭￭ 7
 Eluents and Reagents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Measured cation and anion by IC Expressed aerosol

Cl- Cl-
NO3- NO3-
SO42- SO42-
Na+ Na+
NH4+ NH4+
K+ K+
Mg2+ Mg2+
Ca2+ Ca2+

The addition of internal standard to the WRD and SJAC samples makes
accurate anion and cation IC data validation possible.
The air flow is regulated by a critical orifice which is integrated in the air
outlet connector.
The anion IC, cation IC, gas and aerosol results as well as all other hard-
ware parameters can be monitored using the 2060 and MagIC software.

2.2 Eluents and Reagents

The MARGA uses several eluents and reagents. The quality of the eluents
and reagents has a direct influence on the stability of the entire system
AND the reliability of the analysis results. All eluents and reagents must be
prepared with great care and accuracy.

NOTICE

Wear single use powder free gloves when handling liquids.

NOTICE

All glassware is cleaned at least three times with UltraPure water

(resistance of >18.2 MΩ) before the reagents or standard solutions
are prepared.

8 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Analysis

NOTICE

Before refilling the containers with fresh eluents and reagents, con-
tainers should be cleaned and disinfected to prevent contamination.
See procedure Cleaning procedure containers (see chapter 2.2.2,
page 10)

2.2.1 Chemicals and Apparatus

NOTICE

For preparation of the described eluents and reagents use of Pro Ana-
lyse grade chemicals and UltraPure water (resistance of >18.2 MΩ) is
required.

Chemicals
￭ Phosphoric acid (H3PO4) 85% (1.685 g/ml ~ 14.6 mol/l).
￭ Nitric acid (HNO3), 2 mol/l (ready to use from Merck or Sigma).
￭ Sodium carbonate (Na2CO3), 0.5 mol/l (ready to use from Merck or
Sigma).
OR
Sodium carbonate monohydrate (Na2CO3.H2O) in case you need/want
to prepare the stock solution for the anion eluent yourself.
￭ Hydrogen peroxide (H2O2) 30% or 35%.
￭ Potassium iodate (KIO3).
￭ Lithium Bromide (LiBr)
￭ Acetone (Propanon)
￭ UltraPure water (resistance of >18.2 MΩ)
￭ Hellmanex™ III, alkaline glass cleaning solution (dilute 100x before use,
1.5 ml in 150 ml Ultra Pure Water).

Apparatus
￭ Volumetric flask of 250 ml with stopper.
￭ Adjustable (recently calibrated) pipettes (range 0.00 -10.00 ml).
￭ Analytical balance with an accuracy of 1 mg.
￭ Balance with a maximum of at least 12 kg and accuray of 10 gram.
￭ Plastic funnel to fit in volumetric flasks.
￭ Plastic sample containers of 100 ml, 2 l, 5 l and 10 l.

￭￭￭￭￭￭￭￭ 9
 Eluents and Reagents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

2.2.2 Cleaning procedure containers

Before refilling the containers with fresh eluents and reagents, containers
should be cleaned and disinfected to prevent bacterial growth and con-
tamination.

Cleaning containers

1 Fill the container with 100 ml Ultrapure water.

2 Close container and shake vigorously.

3 Empty container.

4 Fill the container with 20 ml of acetone.

5 Close container and shake vigorously.

6 Empty container.

NOTICE

Dispose the acetone according to local regulations.

7 Fill the container with 100 ml Ultrapure water.

8 Close container and shake vigorously.

9 Empty container.

10 Repeat steps 7 to 9 a total of 3 times.

11 The container is now ready to be refilled.

NOTICE

Clean containers can be stored for future use with 20 ml acetone

inside.
In case clean and stored containers need to be used start at step 6.

10 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Analysis

2.2.3 Eluents
Carefully read this complete section before you continue with the prepara-
tion of reagents.

Anion eluent supplement stock solution

Concentration: 100 mmol/l KIO3

Storage: This solution is stable for 24 months if closed and stored in a
dark place at room temperature.

1 Accurately dissolve 0.535 g potassium iodate (KIO3) in a 250 ml volu-

metric flask.

2 Fill up to the 250 ml mark with ultrapure water and mix gently.

Anion IC eluent

NOTICE

Only use clean anion eluent containers for the preparation of anion
eluent. Cleaning procedure containers (see chapter 2.2.2, page 10)

Concentration: 3.6 mmol/l Na2CO3+ 10µmol/l KIO3

Anion eluent conductivity: 4 µS/cm (±1 µS/cm)

1 Pipette 72.0 ml sodium carbonate solution (Na2CO3 0.5 mol/l) + 1ml

potassium iodate (KIO3), supplement stock solution, into the 10 l
anion eluent container.

2 Fill up to 10.0 kg with ultrapure water.

3 Close container and mix gently.

OR

1 Accurately dissolve 4,46 gram (±0.05 g) sodium carbonate monohy-

drate (Na2CO3.H2O) in a 250 ml volumetric flask.

2 Add approx. 200 ml with ultrapure water, close with a cap and mix
gently till all salts are dissolved.

￭￭￭￭￭￭￭￭ 11
 Eluents and Reagents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3 Bring all liquid to the 10 l anion eluent container and rinse the flask 3
times with ultra pure water, add all rinses to the anion eluent con-
tainer.

4 Add 1ml potassium iodate (KIO3), supplement stock solution, into the
10 l anion eluent container.

5 Fill up the container till 10 l (10,00 Kg)

6 Close container and mix gently.

Cation IC eluent

NOTICE

Only use clean cation eluent containers for the preparation of cation
eluent. Cleaning procedure containers (see chapter 2.2.2, page 10)

Concentration: 4.0 mmol/l HNO3

Cation eluent conductivity: 1250 µS/cm (±50 µS/cm)

1 Pipette 20.0 ml nitric acid solution (HNO3 2 mol/l) into the 10 l cation
eluent container.

2 Fill up to 10.0 kg with ultrapure water.

3 Close container and mix gently.

2.2.4 Reagents
Carefully read this complete section before you continue with the prepara-
tion of reagents.

Absorbance solution (Wet Rotating Denuder)

NOTICE

Only use clean absorbance solution containers for the preparation of

absorbance solution. Cleaning procedure containers (see chapter
2.2.2, page 10)

12 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Analysis

Concentration: 10 mg/l H2O2

1 Fill the 10 l absorbance container up to 10.0 kg with ultrapure water.

2 Add 0.35 ml 30% or 0.3 ml 35% H2O2 to the container.

3 Close container and mix gently.

4 Repeat step 1-3 for the second container.

Suppressor regenerant solution

NOTICE

Only use clean suppressor solution containers for the preparation of

suppressor solution. Cleaning procedure containers (see chapter
2.2.2, page 10)

Concentration: 350 mmol/l H3PO4

1 Fill the 5 l regenerant container up to 4.5 kg with ultrapure water.

2 Add 115 ml (= 194 gram) H3PO4 to the container.

3 Close container and mix gently.

System cleaning solution

Concentration: 1% H2O2

1 Fill a 2 l container up to 1.9 kg with ultrapure water.

2 Add 65 ml 30% or 56 ml 35% H2O2 to the container.

3 Close container and mix gently.

2.2.5 Internal Standard

Carefully read this complete section before you continue with the prepara-
tion of the internal standard.

￭￭￭￭￭￭￭￭ 13
 Eluents and Reagents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Internal standard stock solution

Concentration: 4000.0 mg/L LiBr contains 320.0 mg/L Li+ and 3680.0
mg/L Br-
Storage: This solution is stable for 24 months if closed and stored in a
dark place at room temperature.

1 Accurately dissolve 1000 mg (±2 mg) lithium bromide (LiBr) in a 250

mL volumetric flask.

2 Fill up to the 250 mL mark with ultrapure water

3 Close the volumetric flask with the stopper and mix gently.

Internal standard working solution

NOTICE

Only use clean internal standard solution containers for the prepara-
tion of internal standard solution. Cleaning procedure containers (see
chapter 2.2.2, page 10)

Concentration: 4000.0 µg/L LiBr contains 320.0 µg/L Li+ and 3680.0 µ/L
Br-

1 Pipette 4.70 mL of the internal standard stock solution into the 5 L

internal standard container.

2 Fill up to 4700 gram with ultrapure water.

3 Close container and mix gently.

14 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Hardware

3 Hardware

3.1 Analyzer Cabinets

Basic Cabinet
This paragraph describes the standard wet part configuration. Depending
on your specific needs the analyzer may have been configured differently.

Figure 2 Lay-out of a standard Wet Part Cabinet

￭￭￭￭￭￭￭￭ 15
 Analyzer Cabinets ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

IMPORTANT: The tubing used to feed the steamer (black color), connect-
ing the tubing pump (2A) and the steamer (1B) is called the Steamer Feed
Tubing (part nr: V0M5217130).
The basic cabinet contains 12 wet part module positions, here called 1A
(left top) till 3D (right bottom).
1A: SJAC Module with vacuum sensor.
This module is used for the electronics of the SJAC sensor, the electronics
for the SJAC heater and the vacuum sensor of the vacuum/air pump.
1B: Blind plate.
Here the Steam Jet Aerosol Collector with heater, level sensor and filter are
positioned.
1C: WRD module.
This is the Wet Rotating Denuder module with rotation mechanism, level
sensor and sample filter
1D: Blind plate.
2A: Multi speed tubing pump module.
This module is the SJAC steamer feed tubing pump that feeds the absorb-
ance liquid for the Steam Jet Aerosol Collector. The tubing pump flow is
0.85 ml/min for default critical orifice of 1 m3/h. (Or 0.42 ml/min for
optional critical orifice of 0.5 m3/h).
2B: Double pipette module.
This module contains two glass Sample mixing vessel modules, one to mix
and store the aerosol liquid sample (at the left) and one to mix and store
the gas liquid sample (at the right) both collected in the previous hour.
2C: Burette Module with 20 ml dosing unit.
This module is the Wet Rotating Denuder (WRD) burette for collecting gas
sample (connection port-3), adding internal standard LiBr (connection
port-4), air for mixing in sample mixing vessel module (connection port-2)
and WRD pipette (connection port-1).
2D: Multi speed tubing pump module.
This module is the Wet Rotating Denuder (WRD) fill tubing pump that
feeds the absorbance liquid, controlled by the WRD level sensor, to main-
tain stable water level in the WRD. The flow (when continues running) is
6.9ml/min.
3A: Multi speed tubing pump module.
This module is the Steam Jet Aerosol Collector (SJAC) fill tubing pump that
feeds the absorbance liquid, controlled by the SJAC level sensor, to main-

16 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Hardware

tain stable water level in the SJAC. The flow (when continues running) is
6.9ml/min.
3B: Burette Module with 20ml dosing unit.
This module is the Steam Jet Aerosol Collector (SJAC) burette for collecting
aerosol sample (connection port-3), adding internal standard LiBr (connec-
tion port-4), air for mixing in sample mixing vessel module (connection
port-2) and SJAC pipette (connection port-1).
3C: Burette Module with 10ml dosing unit.
This module is the Ion Chromatograph (IC) burette for transfer of gas liq-
uid sample (connection port-1), or aerosol liquid sample (connection
port-2), or external standard (connection port-4) to the cation and anion
IC (connection port-3).
3D: Blind plate.

Ion Chromatography Cabinet

This paragraph describes the standard configuration of the IC cabinet.
Depending on your specific needs the analyzer may have been configured
differently.

Figure 3 Lay out of a standard IC Cabinet

1: Waste vessel with drain connected to the waste connections. The
waste tube is on the top side connected to the drain of the vessel and on
the bottom side connected to the waste hole of the bottom plate.

￭￭￭￭￭￭￭￭ 17
 Analyzer Cabinets ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

2: On the bottom, left half of the IC cabinet is the cation Ion Chromato-
graph (IC) located, with high-pressure pump, purge valve, injector with
200 µl sample loop and pulsation dampener.
3: On the bottom right half of the IC cabinet is the anion IC located, with
high pressure pump, purge valve and injector with 100 µl sample loop,
pulsation dampener, chemical suppressor with peristaltic pump for regen-
eration and eluent CO2 remover.
4: This is the chemical suppressor regeneration (peristaltic) pump. During
analysis this pump is active/on, the speed is set to 1 in MagIC (corresponds
with 0.1 ml/min).
5: This chemical suppressor is a cation exchanger: All cations are
exchanged for hydrogen ions (H+), suppressing the eluent conductivity
(carbonate eluent becomes water and CO2) and strengthen the anion ions
to be determined.
6: The CO2 suppressor consists of a special membrane, which removes
CO2 eluent from the liquid before detection, reducing the eluent conduc-
tivity and improving the linearity of the calibration lines of the components
to be analyzed.
7: At the right side of the anion IC the column oven is located. Inside the
column oven there is room for two analytical column with pre-columns,
one for anion and one for cation analysis. The column oven houses two
preheating coils to preheat both eluents to the application temperature
(default 45 °C).
8: The cation conductivity detector (used with direct conductivity detec-
tion) is located behind the white thermic isolation cover. The cation detec-
tor is located at the top.
9: The anion conductivity detector (used with sequential suppressed con-
ductivity detection) is located behind the white thermic isolation cover.
The anion detector is located at the bottom.

18 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Program

4 Program

4.1 Program

NOTICE

For reference use only, do not change the program!

The original programs (2060 and MagIC Net) are stored on the USB-drive
that came with the analyser.

￭￭￭￭￭￭￭￭ 19
 Retention times (tR) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

5 Typical results
This chapter shows and explains the results you might expect from your
2060IC MARGA analyzer.

NOTICE

The results of your analyzer and the expected results may differ and
can be caused by:
￭ Use of different separation columns.
￭ Quality of eluents, reagents and standards.
Status of the complete analyzer as a result of regular maintenance
or lack of regular maintenance.

5.1 Retention times (tR)

The retention times for both anion and cation are quite stable over time.
Aging of the column over time results in lower retention times.

Column lifetime
The column lifetime depends on the eluent quality and the general main-
tenance of the entire 2060IC MARGA including the sampling device. The
level of air polution influences (decreases) the column life time.
The typical lifetime of a column is two to four months. It is recommended
to replace the column every three months.

Retention times (tR) anions

Column used: Metrosep A Supp 7 150/2.0 (6.1006.640)
Guard column: Metrosep RP2 Guard/3.5 (V0W8006069 or 6.1011.030)
Table 4 Typical retention time anions
Component New column Used column
[minutes, ±5%] [minutes, ±5%]
Cl- 8.1 7.9
NO2- 9.8 9.6
Br- (internal standard) 11.6 11.3
NO3- 13.4 12.9
SO4-(*) 17.3 16.6

20 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Typical results

Retention times (tR) cations

Column used: Metrosep C 6 - 150/2.0 (6.0151.220)
Guard column: Metrosep RP2 Guard/3.5 (V0W8006069 or 6.1011.030)
Table 5 Typical retention time cations
Component New column Used column
[minutes, ±5%] [minutes, ±5%]
Li+ (internal standard) 4.8 4.7
Na+ 5.7 5.6
NH4+ 6.3 6.1
K+ 7.8 7.6
Mg2+ 17.5 16.9
Ca2+ 21.5 20.8

5.2 Typical Chromatograms

Gas phase

Figure 4 Typical anion chromatogram; gas phase

￭￭￭￭￭￭￭￭ 21
 Typical Chromatograms ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Figure 5 Typical cation chromatogram; gas phase

Aerosol phase

Figure 6 Typical anion chromatogram; aerosol phase

Figure 7 Typical cation chromatogram; aerosol phase

22 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Maintenance schedule

6 Maintenance schedule
This chapter describes all the maintenance steps for the 2060IC MARGA
analyzer. The maintenance of a Metrohm Process Analytics analyzer
depends on many variables:
￭ Kind of sample and used application
￭ Number of cycles per hour (or day)
￭ Importance to the customer (e.g. following a trend or the need for
absolute/exact values)

6.1 Maintenance schedule

CAUTION

The user should only perform maintenance as listed below or in the

user manual. All other maintenance and/or service jobs should only
be performed by a certified Metrohm Process Analytics service engi-
neer.

The 2060IC MARGA system requires frequent maintenance to ensure

good performance during daily operation. The maintenance topics and
the frequency are listed in the following tables:

Eluents, reagents and standards

Table 6 Eluent, reagents and standards
Chemical 2 weeks 1 month 2 months

Replace absorbance liquid (2x 10 L containers) X

Empty waste container X

Replace anion and cation eluents X

Replace internal standard solution X

Replace suppressor solution X

Basic Cabinet
Table 7 Wet Part Cabinet
Description 2 weeks 1 month 6 months 12 months

Internal plate of the air inlet X

Replace sample filter WRD X

￭￭￭￭￭￭￭￭ 23
 Eluent replacement ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Description 2 weeks 1 month 6 months 12 months

Check WRD and clean if necessary X

Replace sample filter SJAC X

Check SJAC and clean if necessary X

Check Sampling Mixing vessel and clean if X

necessary

Replace Pump Tubing X

Replace Cylinder and piston (Dosing unit) X

Ion Chromatography Cabinet

Table 8 Ion Chromatography Cabinet
Description 1 month 2 months 3 months 6 months

Replace anion and cation guard columns X

Flush system with cleaning solution X

Replace anion column Depends on the sample and eluent.

Replace cation column Depends on the sample and eluent.

Replace filters in storage containers (eluents, X

internal standard and H3PO4)

Replace inline filters before pulsation dem- X

pers

Replace inline filters behind suppressor pump X

6.2 Eluent replacement

CAUTION

Wear single use powder free gloves when replacing eluents.

NOTICE

Step 4, 5, 6 and 7 below of the anion and cation replacement proce-

dure must be done within 20 seconds. This is to prevent air from
entering the eluent tubing, which results in a failure, the system will
stop in between 3-10 minutes.

24 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Maintenance schedule

Replacement Anion IC eluent

1 Clean the spare 10 L anion eluent container Cleaning procedure con-

tainers (see chapter 2.2.2, page 10).

2 Prepare fresh anion eluent (see "Anion IC eluent", page 11).

3 Unscrew the cap of the fresh anion eluent container.

4 Slide gently the container out of the chemical cabinet.

5 Unscrew the currently used anion eluent container cap.

6 Hold the cap with the tubing and filter in the air.

7 Insert tubing into the fresh eluent container and tighten cap.

8 Slide fresh eluent container in the chemical cabinet position.

Replacement Cation IC eluent

1 Clean the spare 10 L cation eluent container Cleaning procedure

containers (see chapter 2.2.2, page 10).

2 Prepare fresh cation eluent (see "Cation IC eluent", page 12).

3 Unscrew the cap of the fresh cation eluent container.

4 Slide gently the container out of the chemical cabinet.

5 Unscrew the currently used cation eluent container cap.

6 Hold the cap with the tubing and filter in the air.

7 Insert tubing into the fresh eluent container and tighten cap.

8 Slide fresh eluent container in the chemical cabinet position.

￭￭￭￭￭￭￭￭ 25
 Reagent and Standard replacement ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6.3 Reagent and Standard replacement

CAUTION

Wear single use powder free gloves when replacing reagents and
standards.

Replacement of the absorbance solution

1 Clean the spare 10 L absorbance solution container Cleaning proce-

dure containers (see chapter 2.2.2, page 10).

2 Prepare fresh absorbance solution (see "Absorbance solution (Wet

Rotating Denuder)", page 12).

3 Unscrew the cap of the fresh absorbance solution containers.

4 Slide gently the container out of the chemical cabinet.

5 Unscrew the currently used absorbance solution container cap.

6 Hold the cap with the tubing and filter in the air.

7 Insert tubing into the fresh absorbance solution container and

tighten cap.

8 Slide fresh absorbance containers in the chemical cabinet position.

Replacement suppressor regenerant solution

1 Clean the spare 5 L suppressor regenerant container Cleaning proce-

dure containers (see chapter 2.2.2, page 10).

2 Prepare fresh suppressor regenerant (see "Suppressor regenerant sol-

ution", page 13).

3 Unscrew the cap of the fresh suppressor regenerant container.

4 Slide gently the container out of the chemical cabinet.

26 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Maintenance schedule

5 Unscrew the currently used suppressor regenerant container cap.

6 Hold the cap with the tubing and filter in the air.

7 Insert tubing into the fresh suppressor regenerant container and

tighten cap.

8 Slide fresh suppressor regenerant container in the chemical cabinet

position.

Replacement of the internal standard solution

1 Clean the spare 5 L internal standard container Cleaning procedure

containers (see chapter 2.2.2, page 10).

2 Prepare fresh internal standard (see "Internal standard working solu-

tion", page 14).

3 Unscrew the cap of the fresh internal standard container.

4 Slide gently the container out of the chemical cabinet.

5 Unscrew the currently used internal standard container cap.

6 Hold the cap with the tubing and filter in the air.

7 Insert tubing into the fresh internal standard container and tighten
cap.

8 Slide fresh internal standard container in the chemical cabinet posi-

tion.

￭￭￭￭￭￭￭￭ 27
 Bacterial growth ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

7 Troubleshooting
This chapter describes troubleshooting for the standard 2060IC MARGA
application.

7.1 Bacterial growth

The MARGA uses different reagents and eluents for the Ion Chromatogra-
phy systems. The quality of the reagents and eluents has a direct influence
on the stability of the 2060IC MARGA system and the analysis results. All
eluents must be prepared with great care to prevent BACTERIAL
GROWTH and accuracy to ensure reliable and reproducible results.

NOTICE

Most bacterial problems are caused by dirt/grease on the hands of

the operator.

NOTICE

Wear single use powder free gloves when handling liquids or per-
forming maintenance or repairing the system.

Bacterial growth in the system

The first indication is that the NH4+ peak in the cation gas chromatogram
is far too low or has disappeared completely.
After disappearance of NH4+, the NO2- peak in the anion gas chromato-
gram will start to disappear.
After that the NO3- peak will be disappearing.
The nitrogen present in NH3, HNO2 and HNO3 is consumed (eaten) by the
bacteria and NH3 is the first one to be consumed by the bacteria.

Peroxide is used to prevent bacterial grow, but when the bacterial grow is
there a higher percentage (0.1%) peroxide is only working at the very
beginning of the bacterial presence. 0.1% per-acetic acid is needed to kill
the bacteria.

28 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Troubleshooting

CAUTION

Do not keep the system in analysis when you use higher concentra-
tions of peroxide or per-acetic acid. It will destroy your columns!!!

Clean the complete system and do not forget the denuder caps: quite
often you will find somekind of bacteria based slurry. When present, take
out the denuder seals and clean the caps and seals manually with a tissue,
before you start the cleaning procedure rinse without analyses (no injec-
tions). All components including inlet, tubings, WRD, SJAC, dosino’s and
injection loops (fill position) must be cleaned and rinsed. After cleaning
the system against bacteria, first rinse the system thoroughly with normal
absorbance liquid before you restart the measurement to save your col-
umns.

Bacterial growth in the eluent and reagent containers

Bacterial growth in the eluent container and reagent containers will result
in reduced performance of the 2060IC MARGA analyzer.
Bacterial growth in the eluent containers results in high back pressure of
the IC-system. The typical back pressure of a system depends on the com-
bination of pre-column and analytical column. The best way to under-
stand your system is to keep track of the back pressure on a weekly basis
in a logbook.
Bacterial growth in reagents results in accelerated fouling of the WRD,
SJAC, Burettes and Sampling Mixing Vessels.

7.2 Missing or no peaks in chromatograms

Missing or no peaks in chromatograms (gas phase)
Problem Cause Remedy
Air in Wet Rotating Sample filter is loose. Connect filter properly to the denuder cap.
Denuder (WRD)
Sample filter is blocked. Replace filter with a new filter.
Burette
WRD level completely ￭ Absorbance liquid containers (almost)
down. empty. Replace with a full fresh prepared
container.
￭ Tubing in WRD fill pump is broken.
Replace/repair tubing.
￭ Make sure all tubings are connected leak
free, NO liquid or air leakages.

￭￭￭￭￭￭￭￭ 29
 Missing or no peaks in chromatograms
Problem Cause
Missing Lithium/ Internal standard container
Bromide peak in is (almost) empty.
chromatogram
Possible leakage (air or liq-
uid).
Missing or no peaks in chromatograms (aerosol phase)
Problem Cause
Air in Steam Jet Aer- Sample filter is loose.
osol Collector (SJAC)
Burette
Sample filter is blocked.
SJAC level completely
down.
SJAC liquid level too low.
no liquid in outlet tubing
SJAC.
Missing Lithium/ Internal standard container
Bromide peak in is (almost) empty.
chromatogram
Possible leakage (air or liq-
uid).
No steam gener- Absorbance liquid contain-
ated. ers (almost) empty.
Tubing in SJAC fill pump is
broken.
Steamer is broken.
30 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Remedy
Prepare fresh internal standard and replace
container.
Check all connections for possible leakages (air
or liquid).
Remedy
Connect filter properly to the SJAC filter con-
nection.
Replace filter with a new filter.
￭ Absorbance liquid containers (almost)
empty. Replace with a full fresh prepared
container.
￭ Tubing in SJAC fill pump is broken. Replace/
repair tubing.
￭ Make sure all tubings are connected leak
free, NO liquid or air leakages.
Clean SJAC level sensor with a tissue.
￭ Clean SJAC level sensor with a tissue.
￭ Recalibrate level sensor.
Prepare fresh internal standard and replace
container.
Check all connections for possible leakages (air
or liquid).
Replace with a full fresh prepared container.
Replace/ repair tubing.
Check temperature and replace steamer if nec-
essary.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Troubleshooting

7.3 Anion IC - Anion Chromatograms

Anion
Problem Cause Remedy
(Very) High baseline Suppressor pump has no ￭ Suppressor liquid container is empty -
liquid flow replace with a full fresh prepared container.
￭ Suppressor filter blocked - replace suppres-
sor filter.
￭ Suppressor pump tubing broken - replace
pump tubing suppressor pump.
￭ Suppressor pump is not on - switch on sup-
pressor pump.

Baseline conductiv- IN/OUT suppressor not con- Correct connections - label IN is for column,
ity changes in every nected correctly. label OUT for CO2 remover (MCS)
chromatogram

No baseline separa- wrong eluent: anion eluent Refresh eluent

tion (overlapping conductivity must be 3-4
peaks) µS/cm

Aging column. Replace column.

Retention time (tR) Leakage on high pressure Replace both piston seals in anion pump
shifts in every chro- pump
matogram
No leakage Replace inlet and outlet valves in anion pump

Malfunctioning eluent Replace degasser. Contact your Metrohm serv-

degasser ice organisation.

Sudden increase of Suppressor is not com- ￭ Suppressor liquid container is empty -

baseline pletely regenerated replace with a full fresh prepared container.
￭ Suppressor filter blocked - replace suppres-
sor filter.
￭ Suppressor pump tubing broken - replace
pump tubing suppressor pump.
￭ Regeneration liquid (phosphoric acid) con-
centration is too low - replace with a full
fresh prepared container.

Suppressor is not OK. Suppressor capacity is too low - change it for

new one.

￭￭￭￭￭￭￭￭ 31
 Cation IC - Cation Chromatograms ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

7.4 Cation IC - Cation Chromatograms

Cation
Problem Cause Remedy
No baseline separa- wrong eluent: cation elu- Refresh eluent
tion (overlapping ent conductivity must be
peaks) 1200-1300 µS/cm

Aging column. Replace column.

Retention time (tR) Leakage on high pressure Replace both piston seals in cation pump
shifts in every chro- pump
matogram
No leakage Replace inlet and outlet valves in cation pump

Malfunctioning eluent Replace degasser. Contact your Metrohm serv-

degasser ice organisation.

32 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

8 Appendix

8.1 Extension 2060 MARGA standard application with

Fluoride
This add-on shows how fluoride can be added to the anion analyses of
the 2060 MARGA. Because fluoride elutes at the beginning of the chro-
matogram and low detection limits require a relatively large injection vol-
ume, a column with an inner diameter of 4 mm instead of 2 mm is used.
A 4 mm internal diameter column uses more eluent than a 2 mm. With a
Metrohm A Supp 7 – 150/4.0 column (6.1006.620) the eluent flow is 0,7
ml/min, instead of 0,2 ml/min for the standard 2060 MARGA column Met-
rohm A Supp 7 – 150/2.0 (6.1006.650).

NOTICE

Carefully read this complete section before you continue with the
preparation of reagents.

Column
￭ 6.1006.620 - Metrosep A Supp 7 - 150/4.0.
￭ 6.1011.030 - Metrosep RP 2 Guard/3.5.

NOTICE

For preparation of the described eluents and reagents use of Pro Ana-
lyse grade chemicals and UltraPure water (resistance of >18.2 MΩ) is
required.

Apparatus
￭ 6.2832.000 - MSM rotor A.
￭ 6.2842.020 - Adapter sleeve for Suppressor Vario.
￭ Volumetric flask of 250 ml with stopper.
￭ Adjustable (recently calibrated) pipettes (range 0.00 -10.00 ml).
￭ Analytical balance with an accuracy of 1 mg.
￭ Balance with a maximum of at least 12 kg and accuray of 10 gram.
￭ Plastic funnel to fit in volumetric flasks.
￭ Plastic sample containers of 250 ml.

￭￭￭￭￭￭￭￭ 33
 Extension 2060 MARGA standard application with Fluoride ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Chemicals
￭ Phosphoric acid (H3PO4) 85% (1.685 g/ml ~ 14.6 mol/l).
￭ Nitric acid (HNO3), 2 mol/l (ready to use from Merck or Sigma).
￭ Sodium carbonate (Na2CO3), 0.5 mol/l (ready to use from Merck or
Sigma).
OR
Sodium carbonate monohydrate (Na2CO3.H2O) in case you need/want
to prepare the stock solution for the anion eluent yourself.
￭ Hydrogen peroxide (H2O2) 30% or 35%.
￭ Oxalic acid dihydrate (C2H2O4.2H2O)
￭ UltraPure water (resistance of >18.2 MΩ)

Anion eluent supplement stock solution (Fluoride add-on)

Concentration: 30 mmol/l C2H2O4 (Oxalic Acid).

Storage: This solution is stable for 24 months if closed and stored in a
dark place at room temperature.

1 Accurately dissolve 0.945 g (±0.01 g) g Oxalic acid dihydrate

(C2H2O4.2H2O) in a 250 ml volumetric flask.

2 Fill up to the 250 ml mark with ultrapure water and mix gently.

Anion IC eluent (Fluoride add-on)

NOTICE

Only use clean anion eluent containers for the preparation of anion
eluent. Cleaning procedure containers (see chapter 2.2.2, page 10)

Concentration: 3.5 mmol/l disodium carbonate (Na2CO3) + 2.0 mmol/l

sodium hydrogen carbonate (NaHCO3)+ 3 µmol/l Oxalic acid (C2H2O4)
Anion eluent conductivity: 3.5 µS/cm (±1 µS/cm)

1 Accurately weigh 4.34 gram (±0.05 g) disodium carbonate mono

hydrate (Na2CO3.H2O) in a 250 ml plastic container.

2 Add approx. 200 ml with ultrapure water, close with a screw cap and
mix gently till all salts are dissolved.

3 Accurately weigh 1.68 gram (±0.02 g) sodium hydrogen carbonate

(NaHCO3) in a second 250 ml plastic container.

34 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

4 Add approx. 200 mL with ultrapure water, close with a screw cap
and mix gently till all salts are dissolved.

5 Bring all liquid into the 10 l anion eluent container and rinse both
250 ml plastic containers 3 times with ultra pure water, add all rinses
to the anion eluent container.

6 Add 1 ml Oxalic acid (C2H2O4) stock solution into the 10 l anion elu-
ent container.

7 Fill up the container till 10 l (10,00 Kg)

8 Close container and mix gently.

IC settings (Fluoride add-on)

Table 9
Flow 0.7 ml/min
Partial injection volume 60 µl
Injection loop 100 µl
Temperature column 45 °C
Detector type Conductivity
Analysis time 20 minutes
Speed peristaltic pump suppressor 2 (0.3 ml/min)

Additional MagIC Net calculation formulas for fluoride

HF gas concentration

￭￭￭￭￭￭￭￭ 35
 Extension 2060 MARGA standard application with Fluoride ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

F aerosol concentration

36 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

Example chromatograms (anion only)

2060 IC MARGA Standard mix including Fluoride
Table 10
Fluoride 200 µg/l
Chloride 700 µg/l
Nitrite 500 µg/l
Bromide 800 µg/l
Nitrate 1.200 µg/l
Sulfate 1.000 µg/l

￭￭￭￭￭￭￭￭ 37
 Extension 2060 MARGA standard application with Fluoride ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

2060 IC MARGA gas sample

2060 IC MARGA aerosol sample

38 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

8.2 Wet rotating denuder module (V2LH000343)

Description
The wet rotating denuder (WRD) is used for sampling of water soluble
gases in liquid. Air enters the WRD where acid gases and ammonia are
collected by diffusion into a liquid film. Aerosols will not be absorbed
because of their higher mass and will travel through the denuder. The level
of the liquid within the WRD is kept constant using a level sensor and a
tubing pump fed with an absorbance solution.

Figure 8 WRD module overview

1 Air outlet connection (OD = 12 mm) 2 Sample filter

3 Air inlet connection (OD = 12 mm) 4 Glass tubes

5 Level sensor

The WRD consists of two concentric glass tubes, forming an annulus pas-
sage. These tubes rotate at 8 revolutions per min, forming a continuous
liquid film on the inside of the outer cylinder and the outside of the inner
cylinder. Air is drawn in and, due to high diffusion coefficients, close to
100% of acid gases and ammonia are stripped from the air mass. The
resulting solution of gases is continuously sampled. Due to the geometry
and air velocity a laminar flow of the air within the annulus is realized.
Aerosols pass through to the WRD.
It is desired that the WRD module is positioned on the upper row of the
wet part. This improves both the accessibility of the modules as well as the
performance of the instrument; less dead volume due to shorter tubing.

Connections
￭ Wet connections
– The sample outlet can be connected to a sampling module (eg.
pump, burette module etc.) with an M6 flared tubing.
– The WRD feed can be connected to an absorbance tubing pump
which is controlled by the level sensor.

￭￭￭￭￭￭￭￭ 39
 Wet rotating denuder module (V2LH000343) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

￭ Air connections
– The air inlet can be connected to an air inlet device using a 1/2""
PE tubing. Make sure that the inlet tube ferrules are installed cor-
rect. The inlet tube must be pushed completely into the denuder
cap. This is to avoid dead volume and disturbance of the laminar
flow.

￭ Electrical connections
– The WRD motor is connected to a digital output on the wet part
I/O controller.
– The level sensor is connected to a digital input on the wet part
I/O controller.

Basic maintenance

CAUTION

Wear single use powder free gloves during the following procedures

Rinsing the WRD module

This procedure describes the rinsing procedure for the WRD.

1 Stop the analyzer.

2 Remove Denuder
Carefully remove the glass denuder from the wet part by removing
the right denuder cap.
Inspect the Denuder Bearing Caps for debris or particles. If required
demount the denuder caps from the wet part and rinse with ultra-
pure water from a rinse bottle.

3 Remove visible contamination between denuder tubes

Inspect the denuder for visible contamination (debris/particles).
Remove the contamination with ultrapure water from a rinse bottle.
For persistent contamination, use a cable tie to dislodge the contami-
nation from the surface and then rinse out with ultrapure water. Use

40 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

tissues to clean the ends of the denuder of any Teflon powder left
behind from wear of the seals.

Hellmanex™ III, alkaline glass cleaning solution

(Dilute 100x before use with SJAC or WRD).

Cleaning the WRD module

This procedure describes the cleaning procedure for the WRD.

1 Insert one end of the denuder into the first cleaning cap assembly.

2 Remove the PVC screw cap of the second cleaning cap assembly and
mount it on the other end of the denuder.

3 Stand the denuder vertically on a flat and stable surface and fill with
150 ml of sufficient cleaning reagent.
Hellmanex™ III, alkaline glass cleaning solution (dilute 100x before
use, 1.5 ml in 150 ml Ultra Pure Water).

4 Close the top cleaning cap assembly with its PVC screw cap.

5 Gently swing/rotate the filled denuder.

6 Leave the assembly on a horizontal surface for 5-10 minutes with a

sufficient cleaning reagent to soak the denuder surface

7 Repeat steps 5) and 6) three times

8 Remove one end cap and empty the denuder.

9 Fill with 150 ml ultrapure water and replace the end cap.

10 Gently swing/rotate the filled denuder.

11 Repeat steps 8) to 10) 3 times

12 Check effectiveness of cleaning by slowly rotating the denuder unit

on a level surface when filled with 100- 150 ml ultrapure water. If
the surfaces are well cleaned, the liquid front should remain a
straight unbroken line over the entire length. If this is not the case,
repeat steps 3) to 11)

￭￭￭￭￭￭￭￭ 41
 Wet rotating denuder module (V2LH000343) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

13 Empty denuder, remove cleaning cap assemblies and reinstall the

denuder into the Sample Box

Replacement sample filter

CAUTION

Step 3, 4, 5 and 6 must be done within 20 seconds. This is to prevent

air from entering the system.

The WRD sample filter is located at the left side of the denuder.

1 Activate the new sample filter by slowly passing 5 ml acetone

through the filter, using a 5 or 10 mL syringe.

2 Rinse the new filter twice with 5 ml ultrapure water using a syringe.

NOTICE

When rinsing the filter with water, be sure that no air bubbles
introduced into the filter.

3 Unscrew the female luer lock located on the right side of the current
WRD sample filter.

4 Disconnect the male luer located on the left side of the current WRD
sample filter.

5 Screw the female luer lock located on the right side onto the new
activated WRD sample filter.

6 Connect the male luer located on the left side onto the new activa-
ted WRD sample filter.

Specifications
Contact material Borosilicate glass, PET-P, PTFE (seal)

Absorbance liquid volume 10 - 15 ml

Rotating speed 8 RPM

42 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

Recommended spare parts

Qty. Order no. Description

V0W1030009 Sample filter

Sample filter used for WRD module and SJAC module.

8.3 Steam jet aerosol collector module (V2LH000022)

Aerosols are collected in the Steam Jet Aerosol Collector (SJAC) module.
Air stripped from water soluble gases is drawn through the SJAC module.
By steam injection a water super saturated condition is created, forcing a
water vapor condensation process. The aerosols grow into larger, heavier
droplets due to the process of deliquescence. Further on the air passes
through a glass spiral tube, which acts as a cyclone, transferring te aero-
sols into the liquid. The resulting solution of dissolved ionic aerosol species
is collected at the bottom of the SJAC which is then continuously sampled.
Controlled by a level sensor, water is added to the sample to fill up the
sample flow to the desired volume. In this way no air will enter the sam-
pling system.
The air flow is regulated by a critical orifice which is integrated in the air
outlet connector.

￭￭￭￭￭￭￭￭ 43
 Steam jet aerosol collector module (V2LH000022) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Figure 9 Steam Jet Aerosol Collector Module overview

1 Steamer Connector 2 Vacuum Sensor Connector

3 Level Sensor Fiber 4 T-connector

5 Air out + Critical orifice 6 SJAC level addition connection

7 Steamer Pump Tubing 8 SJAC Heater

9 Air in (from denuder) 10 Growing chanber

11 Cyclone 12 Sample filter

13 Level Sensor

44 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

Connections
￭ Wet connections
– The Sample Filter can be connected to a sampling module (WRD
and SJAC) with a luer -M6 adapter and M6 flared tubing.
– The SJAC level addition connection can be connected to an
absorbance tubing pump, which is controlled by the Level sen-
sor, with an M6 flared tubing.
– The SJAC steamer is connected to an absorber liquid pump with
a Norprene® tubing (V0M5217130; Norprene® tubing ID
1.6mm OD 4.8mm)
– The Air out is part of the Air flow regulation. The Air flow is
regulated by a Critical Orifice, which is integrated in the air out-
let connector.
￭ Electrical connections
– The SJAC steamer is connected to a PID control output on the
Wet part I/O controller.
– The Level sensor is connected to a digital input on the Wet part
I/O controller. This sensor can regulate a digital output.

Figure 10 SJAC Electrical Connections Assembly

1 Vacuum sensor connector I/O board 2 Heater

￭￭￭￭￭￭￭￭ 45
 Steam jet aerosol collector module (V2LH000022) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3 Analog output 4 Level sensor

5 6

Basic maintenance

CAUTION

Wear single use powder free gloves during the following procedures

Cleaning SJAC glass part in 1% H2O2

1 Stop the analyzer.

2
CAUTION

Be carefull: the steam generator can be really hot!

NOTICE

Before disconnecting the SJAC steamer has to be cooled for at

least 15 minutes to prevent damage.

Disconnect the tubings, filter, critical orifice, sample present detector

and steam generator of the glass part of the SJAC.

3 Rinse the SJAC with ultrapure water.

4 Place the SJAC in a beaker .

5 Add 1% H2O2 to the beaker till the SJAC is completely submerged.

6 Place the SJAC in an ultrasonic bath for 10 minutes.

7 Empty the SJAC.

8 Rinse the SJAC with ultrapure water three times.

9 Reconnect the tubings, filter, critical orifice, sample present detector

and steam generator to the glass part of the SJAC.

46 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

Replacement sample filter

CAUTION

Step 3, 4, 5 and 6 must be done within 20 seconds. This is to prevent

air from entering the system.

The SJAC sample filter is located at the left front side of the SJAC.

1 Activate the new sample filter by slowly passing 5 ml acetone

through the filter, using a 5 or 10 mL syringe.

2 Rinse the new filter twice with 5 ml ultrapure water using a syringe.

NOTICE

When rinsing the filter with water, be sure that no air bubbles
introduced into the filter.

3 Remove the sample filter from the SJAC.

4 Disconnect the male luer connector located on the outlet side of the
current SJAC sample filter.

5 Place the new activated SJAC sample filter.

6 Connect the male luer connector onto the new activated SJAC sam-
ple filter.

Specifications
Contact material Borosilicate glass, PET-P, SS, PTFE, Silicone

Absorber liquid volume 1 ml

Airflow 0.5 or 1.0 m3/hour

￭￭￭￭￭￭￭￭ 47
 Ion chromatography ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Recommended spare parts

Qty. Order no. Description

V0W1030009 Sample filter

Sample filter used for WRD module and SJAC module.

8.4 Ion chromatography

Anion IC

48 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

Cation IC

IC Cabinet

1 Eluent degasser 2 High pressure pump

3 Purge valve 4 Inline filter

￭￭￭￭￭￭￭￭ 49
 Ion chromatography ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

5 Pulse dampener 6 Injection valve

7 Column oven 8 Detector compartment

9 Suppressor regeneration pump 10 MSM suppressor

11 MCS suppressor 12 Absorber cartridge used with MCS sup-

pressor

Absorber tubes
Fill the anion absorbing tube on the eluent container with cotton wool
and soda lime. The soda lime will absorb the CO2 from the air which pre-
vents lowering of the pH of the eluent (Na2CO3). If the pH of the anion
eluent lowers because of CO2 the separation of the components on the
anion column will change (become worse/slower).
Fill the cation absorbing tube on the eluent container only with cotton
wool to prevent dust falling in.
Part number: 6.2837.100 - CO2 adsorption cartridge CW

Eluent aspirating filter (20µm)

This filter prevents problems / contaminations of particles, iron and/or
algae which may clog filters in the IC-system. Change the filter when it
changes of color or every 6 months.
Part number: 6.2821.090 - Aspiration filter, 5 pieces

Eluent degasser
Unstable baseline or shifting retention times indicates eluent flow disturb-
ance. This can be caused by a malfunctioning eluent degasser.
Contact your Metrohm organisation for a repair.

High pressure pump

The pump heads have cylinder/pistons working in series, on the bottom
and top of the first cylinder are the inlet (bottom) check valve and outlet
(top) check valve. When the first cylinder refills the top check valve blocks
the flow to prevent backflow of the eluent in the first cylinder. Now the
first cylinder is refilled with new eluent from the eluent container. The sec-
ond cylinder comes in action and takes care of the continues eluent flow.
When the first cylinder is refilled, the bottom check valve blocks, to pre-
vent eluent backflow to the container, and the top check valve opens to
continue the eluent flow through the IC system.
When the check valves are dirty or stuck, the eluent flow is not continues
anymore (non-stable flow). The check valves need to be changed for new
ones.
Part number: 6.2824.160 - Outlet valve PEEK

50 ￭￭￭￭￭￭￭￭
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Appendix

Part number: 6.2824.170 - Inlet valve PEEK

IC Inline filter
The inline filter protects the columns, both separation and guard, for con-
taminations/ particles by the eluent. Change the filters every 6 months, or
when those are dirty and the eluent system pressure goes up. When the
suppressor liquid flow stops dripping in the waste bucket or slows down,
the inline filter has to be changed.
Part number: 6.2821.130 - Spare filter for inline filter, 10 pieces

Injection Valve
The injection loops can become dirty from sample in the inside of the
tube, interfering the chromatogram. Replace the anion and cation sample
loop every year for a new one.
Part number: V2LH001061 - Sample Loop PEEK 100 µl (used in anion IC)
Part number: V2LH001071 - Sample Loop PEEK 200 µl (used in cation IC)

Pre-Column
The 2060IC MARGA uses RP2 pre-column as guard columns. Change
those guard columns (for anion and cation) every month, or when the elu-
ent pressure moves slowly up. The RP2 housing can be reused; there is a
replacing set of 10 RP2 discs with filters.
Part number: 6.1011.030 - Metrosep RP 2 Guard/3.5
Part number: 6.1011.130 - Spare filter for RP 2 Guard/3.5, 10 pieces

Column
The quality of the separation column of anion and cation is normally
slowly decreasing till the end of it’s lifetime. This can be seen on peak
shape (fronting or tailing), broadening peaks, loss of capacity (lower reten-
tion times) or increasing back pressure. As long as the peaks are baseline
separated and the pressure is inside the limits, the column can still be
used.
An average lifetime is 2-4 months of continues analyses. Dirt and bacteria
will shorten it‘s lifetime.
Part number: 6.1006.640 - Metrosep A Supp 7 - 150/2.0, anion column
Part number: 6.0105.1220 - Metrosep C 6 - 150/2.0, cation column

MSM suppressor
The 2060 IC MARGA uses 2 mm ID separation columns. For proper opera-
tion a MSM LC-A (low capacity for anion separations) suppressor is used.
It exchanges all cations in the eluent and sample in H+ resulting in lower
baseline and enhancing sensitivity of the components.

￭￭￭￭￭￭￭￭ 51
 Ion chromatography ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Using phosphoric acid, instead of sulphuric acid, the heavy metals present
in the airosols are also removed from the suppressor.
Part number: 6..2844.000 - MSM-LC Rotor A

MCS suppressor
The MCS (Metrohm CO2 Suppressor) is a special designed degasser to
remove the CO2 from the eluent and sample, effecting in strongly reduced
system-peak in anion chromatogram and improving linearity of the cali-
bration line.
The MCS uses a CO2 adsorption cartridge to adsorb the CO2. When the
CO2 adsorption cartridge becomes wet (moisture in the inside), it has to
be replaced.
Contact your Metrohm organisation for a repair.

52 ￭￭￭￭￭￭￭￭