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Comprehensive water analysis: combining titration, IC, and direct measurement in one setup

Comprehensive water analysis: combining titration, IC, and direct measurement in one setup

If you perform water analyses on a regular basis, then you know that analyzing different parameters for drinking water can be quite time-consuming, expensive, and it requires significant manual labor. In this article, I’d like to show you an example of wider possibilities in automated sample analysis when it comes to combining different analytical techniques, especially for our drinking water.

Water is the source and basis of all life. It is essential for metabolism and is our most important foodstuff.

As a solvent and transporting agent it carries not only the vital minerals and nutrients, but also, increasingly, harmful pollutants, which accumulate in aquatic or terrestrial organisms.

Within the context of quality control and risk assessment, there is a need in the water laboratory for cost-effective and fast instruments and methods that can deal with the ever more complex spectrum of harmful substances, the increasing throughput of samples, and the decreasing detection limits.

Comprehensive analysis of ionic components in liquid samples such as water involves four analytical techniques:

  • Direct measurement
  • Titration
  • Ion chromatography
  • Voltammetry

Each of these techniques has its own particular strengths. However, applying them one after the other on discrete systems in the laboratory is a rather complex task that takes up significant time.

Back in 1998, Metrohm accepted the challenge of combining different analytical techniques in a single fully automated system, and the first TitrIC system was introduced.

What is TitrIC?

The TitrIC system from Metrohm combines direct measurement, titration, and ion chromatography in a fully automated system.

Direct measurements include temperature, conductivity, and pH. The acid capacity (m and p values) is determined titrimetrically. Major anions and cations are quantified by ion chromatography. Calcium and magnesium, which are used to calculate total hardness, can be determined by titration or ion chromatography.

The results are displayed in a common table, and a shared report is given out at the end of the analysis. All methods in TitrIC utilize the same liquid handling units and a common sample changer.

For more detailed information about the newest TitrIC system, which is available in two predefined packages (TitrIC flex I and TitrIC flex II), take a look at our informative brochure:

Efficient: Titrations and ion chromatography are performed simultaneously with the TitrIC flex system.

Figure 1. Flowchart of TitrIC flex II automated analysis and data acquisition.

How does TitrIC work?

Each water sample analysis is performed fully automated at the push of a button—fill up a sample beaker with the sample, place it on the sample rack, and start the measurement. The liquid handling units transfer the required sample volume (per measurement technique) for reproducible results. TitrIC carries out all the work, and analyzes up to 175 samples in a row without any manual intervention required, no matter what time the measurement series has begun. The high degree of automation reduces costs and increases both productivity and the precision of the analysis.

Figure 2. The Metrohm TitrIC flex II system with OMNIS Sample Robot S and Dis-Cover functionality.

To learn more about how to perform comprehensive water analysis with TitrIC flex II, download our free application note AN-S-387:

Would you like to know more about why automation should be preferred over manual titration? Check out our previous blog post on this topic:

Calculations with TitrIC

With the TitrIC system, not only are sample analyses simplified, but the result calculations are performed automatically. This saves time and most importantly, avoids sources of human error due to erroneously noting the measurement data or performing incorrect calculations.

Selection of calculations which can be automatically performed with TitrIC: 

  • Molar concentrations of all cations
  • Molar concentrations of all anions
  • Ionic balance
  • Total water hardness (Ca & Mg)
  • … and more

Ionic balances provide clarity

The calculation of the ion balance helps to determine the accuracy of your water analysis. The calculations are based on the principle of electro-neutrality, which requires that the sum in eq/L or meq/L of the positive ions (cations) must equal the sum of negative ions (anions) in solution.

TitrIC can deliver all necessary data required to calculate the ion balance out of one sample. Both anions and cations are analyzed by IC, and the carbonate concentration (indicative of the acid capacity of water) is determined by titration.

If the value for the difference in the above equation is almost zero, then this indicates that you have accurately determined the major anions and cations in your sample.

Advantages of a combined system like TitrIC

  • Utmost accuracy: all results come from the same sample beaker

  • Completely automated, leaving analysts more time for other tasks

  • One shared sample changer saves benchtop space and costs

  • Save time with parallel titration and IC analysis

  • Flexibility: use titration, direct measurement, or IC either alone or combined with the other techniques

  • Single database for all results and calculation of the ionic balance, which is only possible with such a combined system, and gives further credibility to the sample results

Even more possibility in sample analysis

TitrIC has been developed especially for automated drinking water analysis but can be adapted to suit any number of analytical requirements in food, electroplating, or pharmaceutical industries. Your application determines the parameters that are of interest.

If the combination of direct measurement, titration, and IC does not suit your needs, perhaps a combination of voltammetry and ion chromatography in a single, fully automatic system might be more fitting. Luckily, there is the VoltIC Professional from Metrohm which fulfills these requirements.

Check out our website to learn more about this system:

As you see, the possibility of combining different analysis techniques is almost endless. Metrohm, as a leading manufacturer of instruments for chemical analysis, is aware of your analytical challenges. For this reason, we offer not only the most advanced instruments, but complete solutions for very specific analytical issues. Get the best out of your daily work in the laboratory!

Discover even more

about combined analytical systems from Metrohm

Post written by Jennifer Lüber, Jr. Product Specialist Titration/TitrIC at Metrohm International Headquarters, Herisau, Switzerland.

Measuring herbicides in drinking water

Measuring herbicides in drinking water

It’s springtime in the northern hemisphere, and with rising temperatures comes increased use of herbicides on agricultural crops and in public spaces. In March 2015, the International Agency for Research on Cancer (IARC) published a report which stated that one such herbicide, glyphosate, was «probably carcinogenic to humans». Ever since, the use of this chemical has been highly controversial. In some countries, including the USA, there are already limit values in effect for the weed killer.

Carcinogenic or not?

Glyphosate is a broad-spectrum herbicide used globally in agriculture. Alongside farming, the chemical is also used to kill weeds in domestic gardens and in public and private spaces kept free from «vegetal invasion», such as railway tracks.

Glyphosate has been used since the 1970s in pesticides and was previously thought to be harmless at typical levels of exposure. However, since the International Agency for Research on Cancer (IARC) – the specialized cancer-research agency of the WHO – found that glyphosate was «probably carcinogenic to humans» (Group 2A) in a report published in March 2015, the chemical repeatedly made headlines [1].

Experts were then divided over whether glyphosate should be reapproved after the expiry of its EU market approval on June 30, 2016. This is because the European Food Safety Authority (EFSA) only recently arrived at the opposed conclusion that it is unlikely that glyphosate is genotoxic or poses a carcinogenic threat [2]. The approval of glyphosate was initially extended by 18 months, but is now allowed to remain in use in the EU until at least the end of 2022 [3].

Determination of glyphosate in drinking water

Because chemicals used in farming can seep through the ground and enter the ground water, limit values are in effect in some countries concerning the concentration of glyphosate in drinking water.

Glyphosate and its metabolite AMPA (aminomethylphosphonic acid) are usually determined by HPLC with post-column derivatization and subsequent fluorescence detection (EPA Method 547), or alternatively by ion chromatography coupled with a mass-selective detector.

Methodology using IC

The following segments explain the initial results of the determination of glyphosate and AMPA in drinking water in the low µg/L range using ion chromatography (IC) with pulsed amperometric detection. The detection limits for glyphosate and AMPA previously attained with pulsed amperometric detection were around ≥ 50 µg/L [4].

Given this improvement in terms of sensitivity, the method outlined here represents a promising approach to the screening of water and food samples for glyphosate and AMPA.

Instrumentation

All determinations were performed with an IC system consisting of a 940 Professional IC Vario ONE with an IC Amperometric Detector and an 858 Professional Sample Processor for automatic sample injection (Figure 1).

Figure 1. Glyphosate and AMPA were determined with the ProfIC IC Vario 1 Amperometry system.

Glyphosate and AMPA were separated on the high-capacity anion separation column Metrosep Carb 2 – 150/4.0, and subsequently detected via flexIPAD (FLEXible Integrated Pulsed Amperometric Detection) using a gold working electrode as a measuring mode in the amperometric detector. The profile of the potential curve produced in one measuring cycle in flexIPAD mode is presented in Figure 2.

Figure 2. Pulse profile of the flexIPAD method: A measuring cycle lasts 0.9 s; measurement of the current is performed during the phase shown in red.

Experiment

The Metrosep Carb 2 column is used mainly for separating and determining carbohydrates, sugar alcohols, alcohols, etc. Its high column capacity, combined with the high pH value of the eluent (approximately pH 10), results in a large difference in retention time for AMPA and glyphosate. This is because, with a pH value of 10, all three acid groups are deprotonated in part of the glyphosate, meaning that it is partially present as a trivalent anion while the metabolite AMPA, which is missing the carboxyl group, is present as a divalent anion.

Results

Figure 3 shows the chromatogram of the determination of AMPA and glyphosate under the conditions used in this application. An aqueous standard solution was injected containing 10 µg/L each of both components.

Figure 3. Separation of AMPA and glyphosate: a standard solution containing 10 µg/L of each component in ultrapure water was analyzed.

The detection limits for both components were determined using the signal/noise (S/N) ratio, i.e., the ratio of the peak height to the baseline noise. At the detection limit, the S/N ratio is 3; with smaller values, secured detection is not possible. The detection limit found for AMPA was considerably lower than 1 µg/L, while the limit for glyphosate was approximately 1 µg/L.

Figure 4 shows a chromatogram of a drinking water sample mixed with 2 µg/L glyphosate and AMPA.

Figure 4. Determination of AMPA and glyphosate in drinking water which was mixed with 2 µg/L of each component.

Summary

For the first time, glyphosate and its primary metabolite AMPA were determined in drinking water in the low µg/L range using ion chromatography with pulsed amperometric detection (flexIPAD). This puts at our disposal a reliable and – compared with HPLC with a mass-selective detector – very inexpensive method for determining the glyphosate and AMPA content in water and foodstuffs. With a detection limit of approximately 1 µg/L, the adherence to limit values for glyphosate can be verified in the USA, Canada, and Australia, among others.

If you want to learn even more about how to measure glyphosate and AMPA via ion chromatography and amperometric detection, download our free white paper «Glyphosate and AMPA in drinking water».

Curious to learn even more?

Check out our webinar:

«Glyphosate and AMPA analysis»

References

[1] IARC Monographs Volume 112 (2015). Retrieved from http://monographs.iarc.fr/ENG/Monographs/vol112/mono112-09.pdf on June 27, 2016.

[2] EFSA press news, 151112 (2015). Retrieved from http://www.efsa.europa.eu/en/topics/factsheets/glyphosate151112 on June 27, 2016.

[3] European Commission: Status of glyphosate in the EU. Retrieved from https://ec.europa.eu/food/plant/pesticides/glyphosate_en on May 25, 2020.

[4] F. Sanchez-Bayo, R. V. Hyne, and K. L. Desseille (2010) Anal. Chim. Acta, 675 125–131.

Post written by Dr. Alyson Lanciki, Scientific Editor at Metrohm International Headquarters, Herisau, Switzerland.

To automate or not to automate? Advantages of PAT: Part 1

To automate or not to automate? Advantages of PAT: Part 1

I have to admit that the technological world of process analysis seemed foreign for me for a while. When I first heard about process automation, I imagined futuristic robots that do the work, similar to modern science fiction films. Perhaps many people might have the same impression.

There is often a great deal of uncertainty about what the expression «we automate your process» actually means. In this blog series, I want to show you that process analytical technology (PAT) is less complicated than expected and offers several advantages for users.

What does process analytical technology (PAT) mean? 

I was once told in conversation:

«Process analytics is for everyone who believes that they don’t need it.»

There is definitely truth in this statement, and it certainly shows the abundance of application possibilities. At the same time, it should be considered that in the future, users of process analytical technology will not only invest in conventional measurement technologies (e.g., direct measurement, TDLAS, GC), but also increasingly in the determination of substance properties and material compositions.

Pollution (gases and aerosols) in ambient air are especially harmful to human health. These substances can continuously and reliably be monitored by process analyzers.

PAT serves to analyze, optimize, and ultimately control processes and their critical parameters. This control makes a major contribution to quality assurance and the overall process reliability at the manufacturer. Thinking back to some well-known chemical disasters (e.g. Minamata, Toulouse, or Tianjin) in which poisonous substances were released, causing immense damage to people and the environment, the importance regarding regular monitoring of critical parameters becomes abundantly clear. The list of analytes that can and must be monitored is long, ranging from contamination in wastewater due to municipal or industrial wastewater treatment plants, to pharmaceutical agents, to gases and aerosols in the ambient air.

From Lab to Process

Considering the history of manufacturing and other industrial processes, it is clear that the ultimate goal is to increase throughput in ever-shorter timeframes, with an eye on safety measures and minimization of costs where possible. Independence through automation and fast, reliable data transfer is a high priority.

In order to make the process economically viable along the entire value chain, the resulting products should be manufactured at the highest quality in a short time and with minimal raw material and energy usage. For 24/7 operations in particular, knowledge of the composition of the starting materials and intermediate products (or rather, any impurities) is essential for optimal process control and reliability.

How can reliable process monitoring be ensured around the clock? Very few companies have company laboratories with an actual 3-shift operation, and often send their samples to external laboratories. Additionally, the samples are sometimes taken with longer time intervals between them. This carries various risks.

On one hand, the time lost between the sampling event and receiving the results from the analysis is enormous. It is only possible to react to fluctuations and deviations from target concentrations or limit values ​​with a certain delay. On the other hand, working and environmental conditions are not comparable and can lead to changes in the sample. Oxidation, pressure or temperature changes, introduction of moisture, and many other factors can change a sample’s original properties during transport, waiting periods, and manual laboratory analysis.

Example trend graph comparing process deviations mitigated by manual control (grey) and fully automatic process control (orange) via PAT.

Process analyzers: automated operation around the clock

Analyses, which are usually carried out manually, are automated by using industrial process analyzers. The samples are automatically removed from critical points in the production process and processed further. The information obtained is used to control the process without any delay, as the data can be transferred immediately to a central computing system at the plant. Automated analysis right at the sample point allows for increased accuracy and reproducibility of the data.

In practice, this entails rerouting a partial stream from the process in question to be fed to the analyzer by means of valves, peristaltic pumps, or bypass lines. Each sample is therefore fresh and correlates to the current process conditions. Probes can also be integrated directly into the process for continuous inline measurement.

The analysis is performed using common titration, spectroscopy, ion chromatography, or electrochemical methods known from the laboratory, which are optimally integrated into the process analyzer for each individual application requirement. The methods can be used in combination, allowing several measuring points to be monitored in parallel with one system. Thanks to the process analyzers that are specifically configured and expandable for the application, the optimal conditions for stable process control are obtained.

Spectroscopic methods have become particularly well-established in recent years for process analysis and optimization purposes. In contrast to conventional analysis methods, near-infrared (NIR) spectroscopy shows a number of advantages, especially due to the analysis speed. Results can be acquired within a few seconds and transferred directly to the chemical control system so that production processes can be optimized quickly and reliably. Samples are analyzed in situ, completely without the use of chemicals, in a non-destructive manner, which means further added value for process safety.

The many advantages of PAT

Automation in the context of process analysis technology does not always have anything to do with futuristic robots. Instead, PAT offers companies a number of advantages:

 

  • Fully automatic, 24/7 monitoring of the process
  • Timely and automatic feedback of the analysis results to the system control for automatic process readjustment
  • Reduction in fluctuations of product quality
  • Increased process understanding to run production more efficiently
  • Independent of your own laboratory (or contract lab)
  • Complete digital traceability of analysis results
  • Total solution concepts including sample preconditioning, saving time and increasing safety

What’s next?

In our next post in this series, you will discover the role process analysis technology plays in digital transformation with regard to «Industry 4.0».

Want to learn more about the history of process analysis technology at Metrohm? Check out our previous blog post:

Read what our customers have to say!

We have supported customers even in the most unlikely of places⁠—from the production floor to the desert and even on active ships!

Post written by Dr. Kerstin Dreblow, Product Manager Wet Chemical Process Analyzers, Deutsche Metrohm Prozessanalytik (Germany), with contributions from Dr. Alyson Lanciki, Scientific Editor at Metrohm International Headquarters (Switzerland).

Tips and Tricks for IC Columns

Tips and Tricks for IC Columns

Monitoring and maintaining column performance

One of the basic requirements for ensuring reliable chromatographic analyses is a high-performance separation column. Ion chromatography (IC) users should regularly check the performance of their column. This way, if a drop in performance becomes apparent, steps can be taken in good time to restore or maintain the proper functioning of the column, reducing downtimes in sample throughput. In this blog post, we explain how you can assess column performance, which parameters you should monitor, and which measures you can take to ensure excellent column performance.

 

First-time use of a new separation column

When you use a column for the very first time, we recommend that you check its initial performance. The Certificate of Analysis (CoA), which you receive with every purchase of a Metrohm column, is your source of reference here. Record a chromatogram and use the analysis conditions specified in the CoA: these include flow rate, temperature, eluent (mobile phase), analyte concentration, sample loop size, and suppression.

You can evaluate the column’s performance by comparing some of the result parameters with the values listed in the CoA (e.g. retention time, theoretical plates, asymmetry, resolution, and peak height).

Regular monitoring of column performance

Columns that are already in use should be monitored regularly, too! We recommend carrying out these tests with check standards under the application conditions you normally use, because performance varies depending on the type of analysis and associated analysis conditions as well as the instrumental setup. If a reduction in performance is observed, the requirements of the application are crucial to determine whether it can still be used.

Below, we explain how to determine your column performance based on five performance indicators. You will also find out how you can prevent or rectify a decline in performance.

Click to jump directly to a topic:

 

Backpressure

Monitor the backpressure: When you use your new column for the first time, save the backpressure value under the analysis conditions of your application as a reference («common variable» in MagIC Net). Then use the user-defined results to monitor the difference between the initial backpressure and the one displayed during the current determination.

If you identify an increase in the backpressure in comparison with the saved initial value, this indicates that particles have been deposited in either the guard column or separation column. If the measured increase is greater than 1 MPa, action must be taken. First, you should check which of the columns is affected (guard vs. separation). If the guard column is contaminated, it should be replaced, as this is its primary function. If the separation column is affected, remove it from the system, turn it around and reinstall, and then rinse it for several hours in this reversed flow direction. If this doesn’t help, we strongly recommend that you consider replacing the column. This will be essential if the maximum permitted backpressure for the column is reached.

Retention time

To track changes in the retention time (which signal a decrease in column performance), the retention time of the last analyte peak is monitored in the chromatogram. Sulfate, for example, is suitable for this, as it usually elutes right at the end of standard anion chromatograms. Here too, work with a common variable in MagIC Net to save the initial value.

Unstable retention times can be caused by carbon dioxide introduced from the ambient air or from air bubbles present in the eluent. Luckily, these problems can be resolved easily (see Table 1).

Table 1. Preventing and correcting performance loss in IC columns (click to enlarge).

The column may also have lost some capacity. This capacity loss can be caused by the presence of high-valency ions which are difficult to remove due to their strong attraction to the stationary phase. The column should then be regenerated in accordance with the column leaflet to remove any contamination. If this doesn’t lead to any improvement, then consider replacing the column depending on the requirements of the application, particularly in the event of progressive capacity loss.

Capacity loss can also occur if the functional groups are permanently detached from the stationary phase. In such a case, the column cannot be regenerated and must be replaced.

Resolution

Monitor the chromatographic resolution by comparing measurements from a predefined check standard with an initial reference value. If the resolution is R > 1.5, the signal is considered baseline-separated (see illustration below). However, in cases involving highly concentrated matrices and for peaks that are more widely spread, the resolution value must be higher to ensure baseline separation.

If a loss of resolution occurs, first make sure that it is not caused by the eluent or the IC system. Once these have been ruled out, it is possible that the adsorptive effect of contaminations in the guard column or separation column may be responsible. A contaminated guard column should be replaced. If the cause of the problem is found to be the separation column, this should be regenerated in accordance with the column leaflet to free it from any organic or inorganic contamination. If the loss of resolution progresses, a column replacement is inevitable.

Theoretical plates

Save the initial number of theoretical plates in MagIC Net as a common variable, as mentioned earlier for other parameters. Usually, the last eluting peak is used – in anion chromatograms, sulfate would yet again prove to be a suitable candidate. Theoretical plates also depend on the analyte concentration. Therefore, it is ideal to monitor this parameter during check standard measurements and not during sample measurements. You can track the development of any changes to the number of theoretical plates via the user-defined results in MagIC Net.

A decrease in the theoretical plates can suggest dead volume in the IC system (see Table 1). A low number of theoretical plates may also be observed if the column has been overloaded by a high salt concentration in the sample matrix, for instance. If the theoretical plates decrease by more than 20%, this indicates that column performance is declining. Depending on the requirements of the application, action may need to be taken.

If the guard column is the reason for the drop in performance, it should be replaced. If the problem is with the separation column, we recommend regenerating the column in accordance with the column leaflet to eliminate any organic or inorganic contamination. If this doesn’t help, you should consider replacing the column, particularly if a trend toward lower theoretical plates is observed.

Asymmetry

Determine the initial asymmetry of the analytes by measuring a predefined check standard under the analysis conditions of your application. Save it as a common variable, then track the user-defined results to observe the development of asymmetry over time. The maximum acceptable values for the asymmetry vary depending on the analyte. For example, calcium and magnesium peaks initially present relatively high asymmetry values.

Asymmetry is defined as the distance from the centerline of the peak to the descending side of the peak (B in the figure below) divided by the distance from the centerline of the peak to the ascending side of the peak (A in the figure below), where both distances are measured at 10% of the peak height. Some pharmacopoeia may use other figures – please check to be sure of the requirements in your country.

AS > 1 means a peak has tailing, and AS < 1 equates to peak fronting. Optimum chromatography is achieved with peak asymmetries as close as possible to 1. As a general rule, column performance is considered in decline when the asymmetry is AS > 2 or AS < 0.5. Depending on the requirements of the application, measures have to be taken in this case in order to improve symmetry and to enable better integration.

The reason for high asymmetry values may be down to the ion chromatograph – due to dead volume, for example. If this is not the case, it is important to find out whether the asymmetry is caused by problems with the guard column or with the separation column. If the guard column causes the asymmetry, it should be replaced. If it is the separation column, it should first be regenerated in accordance with the column leaflet to remove any organic or inorganic contamination. If this doesn’t help, you should consider replacing the column. If a trend toward higher asymmetry values can be observed, replacement is unavoidable.

In summary, there are many ways in which you can estimate the performance of the column and track concrete figures over its lifetime. Proper maintenance can extend the lifetime of the separation column, as well as always using a guard column for extra protection.

Need help choosing the right column for your application?

Look no further!

Try the Metrohm Column Finder here:

For further guidance about IC column maintenance, you can watch our tutorial videos here:

Post written by Dr. Alyson Lanciki, Scientific Editor at Metrohm International Headquarters, Herisau, Switzerland. Primary research and content contribution done by Stephanie Kappes.

Increase productivity and profitability in environmental analysis with IC

Increase productivity and profitability in environmental analysis with IC

Nearly every chemist begins his or her path under the guidance of trained professionals, learning the correct way to implement the scientific method and to handle themselves safely in the laboratory. I am no different; I obtained my doctorate in Analytical and Environmental Chemistry in 2010. Since 2003, I worked in the environmental analysis sector, investigating soil contamination due to heavy metals and chemical spills, water quality analysis, and especially performing studies relating to atmospheric chemistry. During these years, I’ve been exposed to several analytical technologies, varied laboratory sizes, and different sample preparation procedures.

A common theme runs throughout these different places—the hunt for more time and a bigger budget. However, with the right tools at your disposal, you can have your cake and eat it, too.

Environmental chemical analysis

The focus of environmental analysis lies in these three major sectors:

  • Air
  • Water
  • Soil

It is in our best interest to study these interconnected areas as thoroughly as possible, considering how our health and the future of our species heavily relates to and relies upon them.

Authorities and regulations

With that in mind, local and governmental authorities have developed and enforced several regulations for the good of public health.

One of the more well-known authorities on the subject is the United States Environmental Protection Agency (EPA). Under the Clean Air Act (enacted in 1970) and Clean Water Act (1972), as well as the requirement to report the use and disposal of toxic chemical substances (TRI reporting), several norms and standards have been developed over the intervening years to meet the stringent guidelines brought forth in these and other regulations.

In the world of water analysis, one of the most common methods you will hear about is EPA Method 300. The methods 300.0 and 300.1 give detailed instructions to chemical analysts regarding measurement of common anions (Part A) and inorganic disinfection byproducts (Part B) in water via ion chromatography.

Meet the family! The Metohm 940 Professional IC Vario TWO/SeS/PP, 930 Compact IC Flex Oven/SeS/PP/Deg, and Eco IC.

Heavier workloads = less time per sample

A growing list of aqueous contaminants and increasingly stringent regulatory requirements require labs to process more samples in less time, without sacrificing accuracy.

The nature of the samples measured in environmental laboratories is such that sample preparation is required—this always involves filtering the samples, and in many cases diluting them as well. This procedure is the only way to prevent damage to the analysis system and to achieve accurate results.

However, sample preparation is an expensive step, as it involves a significant amount work as well as costly consumables.

Time to crunch the numbers!

A 30 day study was performed on a Metrohm IC system with automatic ultrafiltration and dilution by an environmental analysis laboratory in the US. This lab, like many others, processes a high volume of samples, including some with a limited shelf life. Reliability is therefore a particularly important criterion when it comes to buying a new system.

Economic considerations also play a key role: a new system should pay for itself as quickly as possible; it needs to be generating a return on investment after a year at the latest.

So, how did we perform in the study? We tested several parameters, including:

(Click to jump directly to the relevant section.)

(Ultra)filtration

All aqueous environmental samples must be filtered prior to analysis. This prevents particles from the sample contaminating or blocking the separation column, significantly extending its lifetime. The high volume of samples at the lab involved in this study drove material cost down to only $1 USD per syringe filter. However, since each individual sample requires a new filter, with 14,300 samples a year this still amounts to $14,300 – just for filtration materials!

The integrated ultrafiltration in the ion chromatography system from Metrohm only needs one filter change per day, saving this laboratory over $12,000 per year. What’s more, the ultrafiltration process is fully automated.

Compared to manual filtration, this saves three minutes of working time per sample. With labor costs of $18 per hour, this again corresponds to savings of around $13,000 per year.

The Metrohm inline ultrafiltration cell.
Overall, using ultrafiltration saves over $25,000 in annual expenditure – a significant return on investment (ROI).
Yearly cost savings estimated by switching from manual filtration to automatic inline ultrafiltration (click to enlarge).
For even more information about this time-saver, read our earlier blog post about how to determine when it is time to exchange the ultrafiltration membrane:

Suppression

Suppression reduces the conductivity of the eluent, resulting in a more sensitive conductivity detection of the analyte. This makes it possible to achieve particularly low limits of detection and quantification.

The instrument previously used at this laboratory (from a different supplier) employed membrane-based suppressors. These suppressors have to be replaced every three months, costing approximately $1,200 each time. The Metrohm Suppressor Module (MSM), on the other hand, is a one-off purchase because it utilizes ion exchanger particles in a robust micro-packed bed for suppression instead of membranes. The three suppression cartridges of the MSM alternate between suppression, rinsing, and regeneration, thereby ensuring continuous suppression at all times.

The regeneration reagents are inexpensive, averaging $52 per 1,000 samples, resulting in total annual costs of $750 for 14,300 samples. This is much cheaper than the cost of replacing a membrane suppressor multiple times!

The Metrohm Suppressor Module (MSM) high-capacity version.
Yearly cost savings estimated by switching from membrane suppressors to the packed bed MSM. (click to enlarge).
Want to learn even more about suppression in anion chromatography? Download our free brochure here:

Separation Columns

With Metrohm columns, the environmental laboratory in this study achieved better separation of the analytes and a much longer column service life – on average, 7,000 injections compared to 1,200 with the previous columns. There appear to be two factors that are key to the reduced wear on the separation column:

1. The Metrohm ion chromatograph provides measuring signals that are four to five times stronger. This makes it possible to reduce the injection volume by a factor of five.

2. Additionally, Metrohm Inline Ultrafiltration removes particles down to a size of 0.2 μm, whereas manual filtration with syringe filters can only remove particles down to 20 μm.

Selection of Metrohm separation columns in various lengths with intelligent chips (top) and protective guard columns (bottom).
Overall, using Metrohm separation columns saves nearly $18,000 in one year for a high-throughput environmental analysis laboratory.
Yearly cost savings estimated by switching from using Metrohm separation columns compared to the competition (click to enlarge).
Looking for a specific column for your analysis challenges? Check out our Column Finder here!

Dilution

If the determination indicates that the analyte concentration is too high, i.e., outside the permissible determination range, the sample must be diluted and reanalyzed.

This is the situation for around 30% of the samples at the laboratory involved in this study. Manual dilution takes the lab staff at least three minutes per sample. With labor costs of approximately $18 USD per hour, this adds up to annual costs of $3,800.

Automatic Inline Dilution eliminates this expense: the analysis system dilutes the relevant samples fully automatically and then measures them again. This makes the laboratory much more efficient: the daily sample throughput increases, and samples with a limited shelf life are always analyzed in good time.

Yearly cost savings estimated by switching from manual dilution practices to automatic inline dilution from Metrohm (click to enlarge).
Find out more about the many different Metrohm Inline Sample Preparation options available here:

Robustness

Significant cost savings weren’t the only benefit of the Metrohm analysis system – the 30 day comparison study also revealed a number of other advantages. The company was impressed with the robustness of the instrument and with its ability to measure the entire range of samples processed in their laboratory.

Its stable calibration also made it possible to reduce the calibration frequency: the new system only needs calibrating every two to three weeks instead of every two to three days.

The most impressive features, though, were the high measuring sensitivity and the large linear range of the detector. Thanks to the latter, only 2% of the samples remain outside the measuring range and have to be diluted – compared to 30% with the old system.

Final Results

The 30 day test proved to the lab in question that the Metrohm IC with the integrated automatic inline sample preparation techniques saves both material and labor costs. Furthermore, it also offers a number of improvements in terms of analysis performance compared to the systems previously used on site.

The most significant savings are those for labor and material costs as a result of using ultrafiltration, followed by those resulting from the longer service life of the separation column.

 

For the final savings calculation over an entire year, download our white paper on the subject below.

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High productivity and profitability in environmental IC analysis

Post written by Dr. Alyson Lanciki, Scientific Editor at Metrohm International Headquarters, Herisau, Switzerland.