Connections
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I see additional peak broadening, but the column is new. What could be the reason?
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All connections between injector, column and detector must be as short as possible, have a low dead volume and be absolutely tight. The PEEK capillary after the detector block must be free from constriction (the measuring cell is tested to 5 MPa = 50 bar back pressure).
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Eluents and standards
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What do I need to prepare eluents?
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For the preparation of the eluents only chemicals of a purity degree of at least "p.a." should be used. For diluting please use only high purity water.
Fresh eluents should always be microfiltered (0.45 µm filter) and degassed (with N2, He or vacuum). For alkaline eluents and eluents with low buffering capacity one should preferably use a CO2 absorber.
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My retention times are shifting with every new eluent. What can I do?
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Use degassed and CO2-free ultrapure water for eluent preparation. Dissolved CO2 will shift the pH and therefore the retention times. |
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My retention times are shifting during the usage of an eluent. What is the reason for this?
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In case of alkaline eluents, CO2 from the ambient will be dissolved in the eluent and change the eluent pH. To prevent the eluent from CO2 absorption you should use a CO2 absorber. |
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My baseline is slightly shifting and from time to time I recognize a small step in the baseline.
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There might be evaporation in the eluent container. The supply vessel containing the eluent must be closed as tightly as possible to avoid excessive evaporation. This is primarily important with eluents containing organic solvents (e.g. acetone), the evaporation of which can lead to drifts in the long term. If work is performed in a very sensitive range, even if one drop of condensate falls back in the eluent this can cause a noticeable change in the background conductivity. |
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Which kind of standards can be used for ion chromatography?
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You can prepare your own standard solutions from salts or you buy standards by chemical suppliers.
Please check if the pH of the solutions fits with the specifications of your separation column.
Standards and reagents especially for ion chromatography are available here.

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Peristaltic pumps
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What precautions do I need to take when using peristaltic pumps?
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- The pump tubings used by the peristaltic pump are consumable material with a limited lifetime and should be exchanged at regular intervals (approx. every 4 weeks under continuous use).
- Different positions can be used, the position should be changed monthly.
- The pressure of the pump tubing cartridge should not be too high: increase the pressure step by step until you observe a flow; add then 2 more steps.
- Use 3-stopper long-life tubings: 6.1826.3X0
- Inline filters have to be used and exchanged quarterly or if the backpressure is too high.
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Theory
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Abbreviations used in Ion Chromatography
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| CIC |
Combustion IC: The combination of a combustion and Ion Chromatography. In a fully automated process the samples are thermally digested under argon in the furnace unit and then combusted with oxygen. The resulting gaseous compounds are passed into an absorption solution, which is then transferred inline to a Metrohm ion chromatography system. Halogens and sulfur are analyzed typically. |
| DAD |
Diode Array Detector: Each wavelength of the UV and visible range of the light is measured with an individual diode. The optical resolution of the detector is defined by the number of diodes used (e.g. 844 UV/VIS Compact IC: optical resolution = 5 nm). |
| DSP |
Digital Signal Processing: Advanced digital measuring of the conductivity with a high resolution detector. Allowing the direct measurement of all conductivities in one single measuring range from 0 µS/cm up to 15'000 µS/cm without "Range/Full Scale" changes nor "Autoranging". The electronic resolution is 0.0047 nS/cm. All intelligent IC instruments are equipped with DSP. |
| EPOD |
Eluent Preparation on demand: Automatic preparation of eluents for uninterrupted IC analyses for several weeks. Dosino and Level Sensor are used to prepare the eluent as soon as required «on demand». |
| ESI |
Electro spray ionization: Sample introduction mode for MS detectors. At atmospheric pressure the effluent of the capillary is sprayed into a strong electric field. Ions of the respective charge are therefore fed into the mass spectrometer. |
| HETP |
Height Equivalent to a Theoretical Plate: Measures the efficiency of a stationary phase. It is the length of the respective column divided by the Number of Theoretical Plates. The smaller value for HETP the better is the efficiency. |
| IC-ICP/MS |
Hyphenation of Ion Chromatography with Inductively Coupled Plasma – Mass Spectrometric detection (IC-ICP/MS). Typical Analysis: Speciation of e.g. selenium, arsenic… |
| IC-MS |
Hyphenation of Ion Chromatography with Mass Spectrometric detection (IC-MS). Allows often the direct identification of unknown components. Typical Application: Very low level analysis, improved selectivity. |
| IEC |
Ion Exclusion Chromatography: Separation of ions (mainly weak acids) and neutral components (e.g. alcohols) on an ion exchanger material. In IEC a completely sulfonated cation exchanger whose sulfonic acids groups are electrically neutral with protons as counter-ions is frequently used as packing material. In aqueous eluents the functional groups are hydrated. The hydrate shell is limited by a partially negative charged membrane (Donnan membrane). It is only passable by uncharged, non-dissociated molecules such as water. Organic carboxylic acids can be separated if strong mineral acids such as sulfuric acid are used as the mobile phase. Due to their low acid constants (pKa values) the carboxylic acids are almost completely present in a non-dissociated form in strongly acidic eluents. They can pass through the Donnan membrane and be adsorbed at the stationary phase, whereas the sulfate ions of the completely dissociated sulfuric acid are excluded. May be used non-suppressed and with inverse suppression. Columns: Metrosep Organic Acids |
| LOD |
Limit of Detection: The concentration of the analyte at which the resulting peak can be distinguished from baseline noise. Literature and norms describe different ways of determination of the LOD. |
| LOQ |
Limit of Quantification: The minimum concentration of the analyte at which the resulting peak can be quantified with a defined security level. Typically 3 to 5 times higher than LOD. |
| MARGA |
Monitor for AeRosols & GAses in Ambient Air: Dedicated instrument for the analysis of anions and cations in ambient air and aerosol. MARGA continuously samples aerosols as well as acidic and basic gases in air. Anions and cations are analyzed by two built-in Compact ICs. System for semi-continuous analysis for unattended work. For aerosol sampling only see PILS. |
| MCS |
Metrohm CO2 Suppressor: Removes dissolved CO2 after chemical suppression of carbonate / bicarbonate eluents. The dissolved carbonic acid partially dissociates to bicarbonate. This leads to a slightly higher background conductivity. With the MCS this background is minimized to very low levels comparable to those from hydroxide eluents. This minimizes the water dip as well a the system peak. Typical background conductivity after MCS is < 1 µS/cm. With hydroxide eluents the MCS removes the background from carbonate traces. It also removes excess CO2 ion exclusion applications before the MSM. |
| MIDT |
Metrohm Inline Dilution Technique: It allows to automatically dilute the sample according to a set dilution factor. Liquid handling is performed with a Dosino. Works with MagIC Net™. Applying ProfIC-4 system |
| MiPCT |
Metrohm intelligent PreConcentration Technique: Dosino based variable preconcentration technique for extremely flexible calibration out of one standard solution and high calibration range. Applying ProfIC-5 system |
| MiPCT-ME |
Same as MiPCT but with additional Matrix Elimination. Applying ProfIC-5 plus an additional Dosino. |
| MiPT |
Metrohm intelligent Partial Loop Technology: Partial loop injection technique making use of Dosino liquid handling. Multi-point-calibration out of one standard solution, sample volume adjustment. Sample concentration range 1:10'000 in ppb/ppm concentrations. Applying ProfIC-15 system |
| MiPuT |
Metrohm intelligent Pick-up technique: Allows to inject 1 to 60 µL of a small volume sample. Required sample volume: only the volume to be injected. Partial loop injection technique making use of Dosino liquid handling. Multi-point-calibration out of one standard solution, sample volume adjustment. |
| MISP |
Metrohm Inline Sample Preparation. Consists of all automated inline sample preparation techniques used with Metrohm IC systems. Examples: Inline Ultrafiltration, Inline Dialysis, Inline Dilution, Inline Neutralization etc. |
| MSM II |
Metrohm Suppressor Module: Packed bed suppressor with 3 identical suppressor compartments packed with a cation exchanger material. Allowing uninterrupted analysis with chemical suppression due to off-line regeneration and rinsing of the used compartments. Suppressor device with the lowest apparent baseline noise. And therefore the lowest detection limits. Pressure and solvent compatible. Due to its stability Metrohm offers a 10 year warranty on the MSM. |
| MSM-HC |
Metrohm Suppressor Module – High Capacity: Same as MSM but with four times higher exchange capacity. Allows the use of higher concentrated eluents and stronger gradients. |
| MSM-LC |
Metrohm Suppressor Module – Low Capacity: Same as MSM but with lower exchange capacity. Used for 2 mm columns. |
| PAD |
Pulsed Amperometric Detection: Electrochemical detection applying different potentials (pulses) to the working electrode. All components which are oxidized or reduced at the can be analyzed. Also those which react with the surface or cover it. To remove such disturbing reaction products, highly oxidative and reductive potentials are applied to the working electrode after the measuring potential. This removes the reaction products from the previous measuring cycle and renews the electrode surface. Typical applications: carbohydrates, amino acids. Instrument: 871 Advanced Bioscan |
| PCR |
Post-Column Reaction: After the analytical column a transparent ion is converted into a c component with better detectability (e.g. UV/VIS absorbance) by adding of a reagent. This product is the detected with UV/VIS detection. The reaction of the analyte and the reagent is usually very selective and yields often in a colored product (à VIS-Detection), e.g. chromate + diphenylcarbazide à complex (540 nm); bromate + iodide à triiodide (I3-, 352 nm).Parameters that will influence the sensitivity are the reaction time (flow rate / length of reaction coil), the reaction temperature, pH, concentration of catalysts. |
| PILS |
Particle Into Liquid Sampler: Aerosol sampler to be connected to IC or other analysis techniques. Allows the semi-continuous analysis of the chemical (ionic) composition or aerosols (particulate matter). Acidic and basic gases have to removed by denuders prior to the PILS. For the analysis of gases and aerosol see MARGA |
| UV/VIS |
UV/VIS Detection: The absorbance of light is the signal for measuring the chromatogram. There are four different ways of applying UV/VIS detection in IC: direct UV/VIS, indirect UV/VIS, UV/VIS after post-column reaction and UV/VIS after pre-column reaction |
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Metrohm Inline Sample Preparation (MISP) techniques
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| Inline Calibration |
Method used to calibrate ranges very low concentrations (ppt to ppb) with an easy to handle higher concentrated standard solution. Requires a second injector and a preconcentration column. |
| Inline Cation Removal |
MISP method to remove excess of counter ions from the sample. The sample is injected into a stream of transfer solution (typically ultra pure water). In the sample prep module (same reaction like in suppression) the cations of sample are removed. On the preconcentration column the analyte ions are retained and subsequently injected for analysis. Typical application: Heavy metal removal from galvanic samples. |
| Inline Dialysis |
MISP Method to remove particles and large molecules inline from the sample solution prior to the injection. Patented by Metrohm. More efficient than inline ultrafiltration. Typical applications: heavy loaded wastewater, diary products, fruit juices, emulsions. |
| Inline Dilution |
MIDT: It allows to automatically dilute the sample according to a set dilution factor. Liquid handling is performed with a Dosino. Works with MagIC Net™. |
| Inline Eluent Preparation |
E-Pod:Automatic preparation of eluents for uninterrupted IC analyses for several weeks. Dosino and Level Sensor are used to prepare the eluent as soon as required «on demand». |
| Inline Extraction |
MISP Method for automated sample extraction e.g. extraction of ions from (bio)-diesel. |
| Inline Matrix Elimination |
MISP method to remove the matrix (disturbing components in the sample) from the analytes. The sample is injected into a stream of transfer solution (typically ultra pure water). The analytes are retained on the preconcentration column and the matrix subsequently removed by additional transfer solution. After this the injection of the purified analytes takes place. |
| Inline Neutralization |
MISP method to neutralize or remove excess of counter ions from the sample. The sample is injected into a stream of transfer solution (typically ultra pure water). In the sample prep module (same reaction like in suppression) the sample gets neutralized. On the preconcentration column the analyte ions are retained and subsequently injected for analysis. Typical application: trace anions in NaOH solutions. |
| Inline Preconcentration |
Preconcentration is the technology to retain the analyte on a short column (preconcentration column), which is mounted on the injector instead of the sample loop. By switching the injector, the preconcentrated analytes are introduced to the separation column. Preconcentration is mainly used for very low concentration (ppt to low ppb range). It allows to collect analytes from large volumes. |
| Inline Spiking |
MISP Method to add a known amount of ions into a sample during preconcentration. |
| Inline Ultrafiltration |
MISP Method to filtrate sample solutions inline prior to injection. If the samples are too contaminated inline dialysis might be a alternative. Typical applications: Any sample that requires filtration e.g. natural waters (surface, ground, wastewater etc.). |
| Metrohm intelligent Partial Loop Technology |
MiPT: Partial loop injection technique making use of Dosino liquid handling. Multi-point-calibration out of one standard solution, sample volume adjustment. Sample concentration range 1:10'000 in ppb/ppm concentrations. |
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Columns
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What is important when using IC columns?
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- Use in flow direction
- Precolumn should be used and replaced frequently (PR Guard can be exchanged)
- Analytical column: How can life time be increased? E.g. check the quality of chemicals, water and sample preparation (e.g. filtrated or dialyzed samples)
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What means «separation efficiency» and how do I check for it?
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The attainable quality of analyses with a Metrohm Compact IC depends to a large extent on the separation efficiency of the column used. When purchasing an IC column you should ensure that the separation efficiency suffices for the analysis problems at hand. Ascertain the characteristic data of the IC column on the standard chromatogram enclosed with the column such as capacity factors, selectivity, plate number and resolution and check these data with your own measurements. If any difficulties arise, you should always first check the quality of the column by recording a standard chromatogram.
You will find additional general tips on handling IC separating columns in the 8.732.2003 Metrohm Monograph "Ion chromatography" and in the 8.792.2013 Metrohm Monograph "Practical ion chromatography", as well as detailed information on the separating columns available from Metrohm in the leaflets supplied and in the special Application Notes and Bulletins available free of charge from your nearest Metrohm agency.
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How do I protect the column against particles and unwanted components
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To protect the column against foreign particles which could have an adverse influence on the separation efficiency, we advise you to subject both the eluents and all samples to microfiltration (0.45 µm filter) and to siphon the eluent through the 6.2821.090 Aspirating filter.
To avoid contamination by abrasive particles arising from piston seals of the high-pressure pump, it is advantageous to install an in-line filter between the pump and the injection valve.
The use of readily interchangeable precolumns serves to protect the actual separating columns and increase their service life appreciably.
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How do I store the IC column when it is not in use?
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Always store the separating columns closed when not in use and filled in accordance with the manufacturer's specifications. |
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Is there a regeneration procedure for IC columns?
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If the separation properties of the column have deteriorated, it can be regenerated in accordance with the column manufacturer's specifications. With the separating columns available from Metrohm, the instructions for regeneration can be found on the leaflet enclosed with every column.
Regenerate a column only if extended rinsing with a strong eluent did not improve the resolution.
In the case of separating columns with carrier material based on silica, only solutions with pH 2...7 may be used for regeneration, otherwise the columns could be damaged.
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Suppressor Modules
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How do I work properly with the Metrohm Suppressor Module (MSM and MSM-HC)?
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- MSM Suppressor
- PTFE capillaries are soft, don't close the screws too tight; if the capillaries are squeezed, cut off the first millimeter using a capillary cutter.
- Don't step the suppressor under dry conditions!
- In case the background conductivity is too high check the flow rates of the sulfuric acid and ultrapure water.
Protection
To avoid contamination of the suppressor module by foreign particles or bacterial growth, the two 6.2821.120 Inline Filter 2 µm supplied must be installed between peristaltic pump and inlet capillaries of the suppressor module.
Operation
The Metrohm Suppressor Module MSM comprises a total of 3 suppressor units which are in turn used for suppression, regenerated with sulfuric acid and rinsed with water. To record every new chromatogram under comparable conditions, work is normally carried out with freshly regenerated suppressor. Switching takes place automatically together with the valve switching.
For operation of the suppressor module, a two-channel peristaltic pump is needed which conveys the regeneration solution (normally 50 mmol/L H2SO4) and the rinsing solution (normally dist. H2O) to the suppressor units (flow rate of 0.5 mL/min).
The suppressor units must never be regenerated with H2SO4 in the same flow direction used for the eluent. You should thus always install the inlet and outlet capillaries.
The suppressor module must never be switched in the dry state as there is a danger of blocking. Before every switching operation of the suppressor module, the three suppressor units must have been rinsed for at least 1/2 h with eluent, regeneration and rinsing solution.
The capacity of the suppressor units is exhausted after approx. 2 h or less, depending on the eluent and the flow rate. With longer interruptions between the individual measurements it is recommended that, depending on the separating column used, that a method is started that steps the MSM e.g. every 20 min during the pauses.
Maintenance
In the event of reduced capacity or high counter-pressure the suppressor module must be regenerated, cleaned or exchanged.
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How do I use the MCS?
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The Metrohm CO2 Suppressor (MCS) requires CO2-free air therefore:
- Water and CO2 absorber cartridges have to be used.
- Water absorber material can be regenerated by heating (<140°C -> see color indicator)
- CO2 absorber material has to be replaced frequently (see color indicator)
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Is there a hazardous color indicator used in the absorption cartridges?
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No, the color indicator used is free from the previously used cobalt chloride. |
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