This article presents a set of evaluation guidelines — developed from the author's 20 years of experience demonstrating inductively coupled plasma–optical emission spectrometry (ICP-OES) and ICP–mass spectrometry (MS) instrumentation and running customer samples — to help laboratory scientists make the right decision when selecting an ICP-MS instrument. It focuses on the evaluation process and the most important factors to consider rather than on how to compare the analytical performance of the instruments being evaluated.
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So you have read the chapter in my book (1) on comparing inductively coupled plasma–mass spectrometry (ICP-MS) with other atomic spectroscopic techniques and convinced your boss that it is the ideal technique for your laboratory. However, understanding how the instrument works doesn't necessarily give you an insight into how to compare different designs, hardware components, and the difficult-to-define intangible factors such as ease of use, reliability, and technical support; these factors are of critical importance when you have to make a decision regarding which instrument to purchase or what vendor to go with. A number of excellent commercial instruments are available on the market that all look very similar and have very similar specifications, but how do you know which instrument is the best for your application needs or which company will take care of you the best? This article presents some guidelines on how best to evaluate the capability of the instrumentation and to assess the expertise and commitment of the ICP-MS vendor.
It is very important before you begin the selection process to decide what your evaluation objectives are. This is particularly important if you are part of an evaluation committee. It is fine to have more than one objective, but it is essential that all the members of the group begin the evaluation process with the objectives clearly defined. For example, is detection limit performance an important objective for your application, or is it more important to have an instrument that is easy to use? If the instrument is being used on a routine basis, good reliability may be very critical. On the other hand, if the instrument is being used to generate revenue, perhaps sample throughput and cost of analysis are of greater importance. Every laboratory's scenario is unique, so it is important to prioritize before you begin the evaluation process. So, in addition to looking at performance, instrument features, and hardware components, you should make the comparison with your evaluation objectives in mind, based on your particular application needs.
Although price can be considered a valid evaluation guideline, especially if you only have limited funds to purchase an instrument, it will not be discussed in this article. However, you will probably own the instrument for 10 years or more. For that reason, you should purchase the instrument that is best suited for your needs and not the instrument with the lowest price tag. If you are interested in the financial side of the evaluation process, it is presented in greater detail in my book (1). With that in mind, let's take a look at the three most common selection criteria used in the evaluation process.
They typically include
Let's examine these in greater detail.
Analytical performance can mean different things to different people. The major reason that the trace-element community was attracted to ICP-MS almost 30 years ago was its extremely low multielement detection limits. Other multielement techniques, such as ICP-optical emission spectrometry (OES), offered very high throughput but just could not get down to ultratrace levels. Although electrothermal atomization (ETA) offered much better detection capability than ICP-OES, it did not offer the sample throughput capability that many applications demanded. In addition, ETA was predominantly a single-element technique and so was impractical for carrying out rapid multielement analyses. These limitations quickly led to the commercialization and acceptance of ICP-MS as a tool for rapid ultratrace-element analysis. However, there are certain areas where ICP-MS is known to have weaknesses. For example, dissolved solids for most sample matrices must be kept below 0.2%; higher levels can lead to serious drift problems and poor precision.
Polyatomic and isobaric interferences, even in simple acid matrices, can produce unexpected spectral overlaps that will have a negative impact on your data. High-resolution instrumentation and collision–reaction cell and interface technology are helping to alleviate these spectral problems, but they also have their limitations. Depending on the types of samples being analyzed, matrix components can dramatically suppress analyte sensitivity and affect accuracy. These potential problems can all be reduced to a certain extent, but different instruments approach and compensate for these problem areas in different ways. With a novice, it is often ignorance or a basic lack of understanding of how a particular instrument works that makes the selection process more complicated than it really should be. So, any information that can help you prepare for the evaluation will put you in a much stronger position.
It should be emphasized that these evaluation guidelines are based on my personal experience and should be used in conjunction with other material in the open literature that has presented broad guidelines to compare figures of merit for commercial instrumentation (2–4). In addition, you should talk with colleagues in the same industry or application segment as yourself. If they have gone through a lengthy evaluation process, they can give you valuable pointers or even suggest an instrument that is better suited to your needs. Finally, I strongly suggested that you narrow the actual evaluation to two or three commercial products. By carrying out some pre-evaluation research, you will gain a better understanding of what ICP-MS technology or instrument to focus on. For example, if funds are limited and you are purchasing an ICP-MS system for the very first time to perform high-throughput environmental testing, it is probably more cost-effective to focus on quadrupole technology. On the other hand, if you are investing in a second system to enhance the capabilities of your quadrupole instrument, it might be worth taking a look at magnetic sector or triple-quadrupole collision–reaction cell instruments. Or, if fast multielement transient peak analysis is your major reason for investing in ICP-MS, time-of-flight (TOF) or Mattauch-Herzog simultaneous sector systems should be given serious consideration. Alternatively, if your instrument is going to be used to characterize nanoparticles using the single-particle ICP-MS technique, the speed of data acquisition and the response time of the ICP-MS quadrupole and detector electronics must be fast enough to capture the time-resolved nanoparticles pulses, which typically last only a few milliseconds or less.
So depending on your application requirements, several major performance criteria should be evaluated:
It is beyond the scope of this article to go into the evaluation of all these performance criteria, because it would require more detail than can be conveyed in a magazine article. There are many ways to compare performance, particularly when it comes to the demands of different application areas. However, it will be easier to compare the capabilities of each instrument being evaluated by using exactly the same set of evaluation samples and calibration standards. The samples can include unknowns, your own quality control (QC) standards, and certified reference materials, but it is important that you supply these samples already prepared; you should take all the necessary precautions in preparing the samples for an ultratrace-element technique like ICP-MS (1). In this way, you are assessing the capability of the instrument and not the expertise of the vendor to carry out dissolution and preparation of the sample or making up the calibration standards and blanks. It's certainly valid to evaluate the expertise of the vendor's analytical chemist, but try to separate that evaluation from the performance of the instrument.
It's also important to emphasize that in today's ICP-MS marketplace, all commercially available instruments are of the highest quality. Despite what each vendor might tell you, they will all do an excellent job for you. There will clearly be subtle differences in the capability of each instrument, based on your application requirements. More-detailed information is available from my textbook and the short course that I teach at the Pittsburgh Conference every year (1,5).
But even after you have run a set of evaluation samples, it might not be possible to declare a clear winner. So the final decision will often come down to factors such as ease of use, reliability, and technical support from the vendor. The rest of this article will therefore focus on these intangible factors, which are sometimes extremely difficult to compare.
In most applications, analytical performance is a very important consideration when deciding what instrument to purchase. However, the vast majority of instruments being used today are being operated by technician-level chemists. They usually have had some experience in the use of trace-element techniques such as atomic absorption (AA) spectroscopy or ICP-OES, but in no way could they be considered experts in ICP-MS. Therefore, a system's usability aspects might be competing with its analytical performance as the most important selection criteria, particularly if the application does not demand the ultimate in detection capability. Although usability is in the eye of the user, there are some general considerations that need to be addressed. They include but are not limited to the following aspects:
First, you need to determine the skill level of the operator who is going to run the instrument. If the operator is a PhD-level scientist, then maybe ease of use is not such an important factor. However, if the instrument is going to be used in a high-workload environment and possibly be operated around the clock, there is a strong possibility that the operators will be less qualified. Therefore, you should be looking at how easy the software is to use and how similar it is to other trace-element techniques that are used in your laboratory. Ease of use will definitely have an impact on the time it takes to fully train a person to use the instrument. Another issue to consider is whether the person who runs the instrument on a routine basis is the same person who will be developing the methods. Correct method development is critical because it impacts the quality of your data; therefore it usually requires more expertise than just running routine methods.
This article will not discuss software features or operating systems, because they are complicated to evaluate and decisions tend to be based more on a personal preference or comfort level than on the actual functionality of ICP-MS software features. Instrument software is also a moving target, because it is continually being modified and updated. However, there are differences in the way software feels. For example, if you have come from an MS background, you are probably comfortable with more-sophisticated software. Alternatively, if you come from a trace-element background and have used AA or ICP-OES, you are probably used to more routine software that is relatively straightforward to use. You will find that different vendors have come to ICP-MS from a variety of different analytical chemistry backgrounds, which is often reflected in the way they design their software. Depending on the way the instrument will be used, an appropriate amount of time should be spent looking at software features that are specific to your application needs. For example, if you are working in a high-throughput environmental laboratory, you might be interested in turnkey methods that are used to run a particular United States Environmental Protection Agency (EPA) methodology, such as Method 200.8 for the determination of elements in water and wastes. In addition, maybe you should also be looking very closely at all the features of the automated QC software, or if you do not have the time to export your data to an external spreadsheet to create reports, you might be more interested in software with comprehensive reporting capabilities.
In some highly regulated industries, the operating and reporting software needs to be compliant with a set of regulated standards and guidelines. For example, the pharmaceutical and food manufacturing industries are affected by federal regulations set down by the Food and Drug Administration (FDA) in 21 CFR Part 11, which specifies detailed requirements that computerized systems need to fulfill to allow electronic signatures and records in lieu of handwritten signatures on paper records. There are other industries that are highly regulated, so it is very important that any ICP-MS system used in a regulated environment has all the necessary software to be compliant.
As mentioned previously, optimized method development is absolutely critical in ICP-MS. Factors such as torch alignment, plasma and nebulizer gas flows, ion lens voltages, and collision–reaction cell gas conditions are all variables than can potentially impact the sensitivity, detection limits, interference reduction capabilities, and precision of your analysis. You should set aside enough time in your evaluation to carefully consider these factors and understand how different instruments compare with regard to ease of method development.
This is most definitely the case with collision–reaction cells and interfaces, especially with a new method. It can take a great deal of time and effort to select the best gases, gas flows, and cell parameters to maximize the reduction of interferences for certain analytes in a new sample matrix. Using a single gas in a simple collision cell can be beneficial to setting up a method, but can it determine your full suite of elements at the detection limits you require in all your sample matrices? And does the use of a collision cell degrade the detection capability of the analytes that don't actually need it? On the other hand, using reaction chemistry typically offers the best interference reduction capabilities and lowest detection limits, but it can be quite time-consuming, particularly if more than one reaction gas is required. Reaction mechanisms are very well understood nowadays because vendors have been investigating the optimum reaction gases for different sample matrices for almost 15 years, since collision–reaction cells were developed. As a result, a large amount of application data is available in the public domain.
ICP–MS systems are complex pieces of equipment that, if not maintained correctly, have the potential to fail when you least expect them to. For that reason, a major aspect of instrument usability is how often routine maintenance has to be performed, especially if complex sample matrices are being analyzed. You must not lose sight of the fact that your samples are being aspirated into the sample introduction system and the resulting ions generated in the plasma are steered into the mass analyzer via the interface and ion optics. In other words, the sample, in one form or another, is in contact with many components inside the instrument. Modern instruments require much less routine maintenance than older-generation equipment, but it is still essential to find out which components need to be changed and at what frequency to keep the instrument in good working order. You should be asking the vendor which components need to be replaced or inspected on a regular basis and what type of maintenance should be done on daily, weekly, monthly, or yearly intervals. In other words, determine the tasks required to keep the instrument in good working order. I also encourage you to talk to real-world users of the equipment to make sure you get their perspective of these maintenance issues. This step is particularly important if you are investing in a brand new instrument that hasn't been on the market long. There won't be a large number of users in the field, so it's important you talk to them to get their real-world perspective of the routine maintenance issues.
Alternative sample introduction techniques are becoming more necessary because ICP-MS is being utilized to analyze more complex sample types. Therefore, it is important to know if a particular sampling accessory is made by the ICP-MS instrument company or by a third-party vendor. Obviously, if it has been made by the same company, compatibility should not be an issue. However, sampling accessories made by a third party may work much better with some instruments than with others. It might be that the physical connection of coupling the accessory to the ICP-MS torch has been better thought out, or that the software "talks" to one system better than another. A good example of this is in the coupling of liquid or gas chromatographic techniques with ICP-MS for the separation and detection of different elemental species. There are many excellent commercially available chromatography systems that are capable of performing low-level speciation determinations, but the chromatography system must connect relatively seamlessly to the ICP-MS system. In addition, not all chromatography data handling software is the same, so make sure you fully evaluate its capabilities, flexibility, and ease of use, because it will have a direct impact on the time required to develop and run a speciation method on a routine basis.
You should also understand how much routine maintenance a sampling accessory needs. The benefits of a rugged ICP-MS system that requires very little maintenance is negated if the sampling accessory needs to be cleaned every 5–10 samples. (See reference 1 for more details about the suitability of sampling accessories such as laser ablation for the analysis of solid materials, high performance liquid chromatography for trace-element speciation studies, or field-flow fractionation for the characterization of nanoparticles.) And if a sampling accessory is required, software–hardware compatibility should be one of your evaluation factors.
However, sampling-accessory compatibility is not the same factor as how the sampling accessory impacts the performance of the instrument. For example, when a dry sample aerosol generated by a laser ablation system is introduced into an instrument, how do the ablated particles affect the torch, interface cones, and ion optic system? A liquid sample aerosol might not cause any problems, but dry particles ablated from a solid surface could possibly be deposited on components in the interface region and have a negative impact on the instrument's sensitivity or signal stability.
Installation of the instrument and where it is going to be located does not seem to be an obvious evaluation consideration at first, but it could be important, particularly if space is limited. For example, is the instrument freestanding or bench-mounted? Maybe you have a bench available but no floor space, or vice versa. It could be that the instrument requires a temperature-controlled room to ensure good stability and mass calibration. If this is the case, have you budgeted for this kind of expense? If the instrument is being used for ultratrace detection levels, does it need to go into a class 1, 10, or 100 clean room? If it does, what is the size of the room and do the roughing pumps need to be placed in another room? In other words, it is important to fully understand the installation requirements for each instrument being evaluated and where it will be located (for more details, see reference 1).
Technical and application support is a very important consideration, especially if you have no previous experience with ICP-MS. You want to know that you are not going to be left on your own after you make the purchase. Therefore, it is important to know not only the level of expertise of the specialist who is supporting you, but also whether they are local to you or located in the manufacturer's corporate headquarters. In other words, can the vendor give technical help whenever you need it? Another important aspect related to application support is the availability of application literature. Is a wide selection of material available to help you develop your methods, either in the form of Web-based application reports or references in the open literature? Also, find out if there are active users or Internet-based discussion groups, because they will be an invaluable source of technical and application help. One excellent source of help in this area can be found on the PlasmaChem Listserver, a plasma spectrochemistry discussion group out of Syracuse University (6).
Find out what kind of training course comes with the purchase of the instrument and how often it is run. Most instruments come with a 2–3 day training course for one person, but most vendors will be flexible regarding the number of people who can attend. Some manufacturers also offer application training, where they teach you how to optimize methods for major application areas such as environmental, clinical, and semiconductor analysis. Talk to other users about the quality of the training they received when they purchased their instruments and also ask them what they thought of the operator's manuals. You will often find that this is a good indication of the importance a vendor places on customer training.
To a certain degree, instrument reliability is impacted by routine maintenance issues and the types of samples being analyzed, but it is generally considered more of a reflection of the design of an instrument. Most manufacturers will guarantee a minimum uptime percentage for their instrument, but this number (which is typically ~95%) is almost meaningless unless you really understand how it is calculated. Even when you know how it is calculated, it is still difficult to make the comparison. But at least you should understand the implications if the vendor fails to deliver the uptime they promise. Good instrument reliability is taken for granted nowadays, but it has not always been the case. When ICP-MS was first commercialized in , the instruments were a little unpredictable, to say the least, and were quite prone to frequent downtime. However, as the technique became more mature, both the quality of instrument components and overall reliability improved. You should therefore be aware of the instrument components that are more problematic than others. This is particularly true when the design of an instrument is new or a model has had a major redesign. You will therefore find that in an instrument's design life cycle, instruments that are "more mature" in age will have a known track record, particularly when being used in a high-sample-throughput environment. For this reason, it is very important that you talk to real users in your application field to get their input.
So when it comes to instrument reliability, it is important to understand whether it is related to the samples being analyzed, the inexperience of the operator, a failed or unreliable component, or an inherent weakness in the design of the instrument. For example, how does the instrument handle highly corrosive chemicals such as concentrated mineral acids? Some sample introduction systems and interfaces will be more rugged than others and will require less maintenance. On the other hand, if an operator is not aware of the dissolved solids limitation of the instrument, he or she might attempt to aspirate a sample, which will slowly block the interface cones, causing signal drift and, in the long term, possible instrument failure. Or, it could be something as unfortunate as the failure of a major component such as the radio frequency (RF) generator power amplifier tube, detector, or turbomolecular pump. Although this scenario is extremely unlikely, all these components have a finite lifetime and as the instrument approaches retirement, the likelihood of a component failure will increase.
Instrument reliability is very difficult to assess at the evaluation stage, so you have to look very carefully at the kind of service support offered by the vendor. For example, how close is a qualified support engineer to you? What is the maximum amount of time you will have to wait to get a support engineer at your laboratory or at least to call you back to discuss a problem? Ask the vendor if they have the capability for remote diagnostics, where a service engineer can remotely run the instrument or check the status of a component by "talking to" your system computer via the Internet. Even if this approach does not fix the problem, at least the service engineer can come to your laboratory with a very good indication of what the problem could be.
You should know up front what a service visit is going to cost you, irrespective of what component has failed. Also find out which routine maintenance jobs you can do and which ones require an experienced service engineer. If a maintenance task does require a service engineer, how long will it take them to complete the service? Most vendors charge an hourly rate for a service engineer but when travel time or an overnight stay is required, fully understand what you are paying for. Some companies might even charge for mileage between the service engineer's base and your laboratory. If you work in a commercial laboratory and cannot afford the instrument to be down for any length of time, find out what it is going to cost for 24–7 service coverage.
You can take a chance and just pay for each service visit, or you might want to budget for an annual preventative maintenance contract, where the service engineer checks out all the important instrumental components and systems frequently to make sure they are all working correctly. This might not be as critical if the instrument is in an academic or research environment, but it is absolutely critical if it is being used in a commercial or contract laboratory to generate revenue. Also find out what is included in the service contract, because some cover the cost of consumables or replacement parts in addition to service visits, whereas others just cover the service visits. These annual preventative maintenance contracts typically make up about 10–15% of the cost of the instrument, but they are well worth it if you do not have the expertise in-house or if you just feel more comfortable having an insurance policy to cover instrument breakdowns.
Once again, talking to existing users will give you a very good perspective of the quality of the instrument and the service support offered by a manufacturer. There is no absolute guarantee that the instrument of choice is going to perform to your satisfaction 100% of the time, but if you work in a high-throughput, routine laboratory, make sure it will be down for the minimum amount of time. Fully understand what it is going to cost you to maximize the uptime of all the instruments being evaluated.
As mentioned earlier, it was not my intention to compare instrument designs and features in this article, but to give you some general guidelines as to what are the most important factors to take into consideration. Besides being a framework for your evaluation process, these guidelines should be used in conjunction with the other materials and references mentioned in this article.
However, if you want to find the best instrument for your application needs, be prepared to spend a few months evaluating the marketplace. Don't forget to prioritize your objectives and give each of them a weighting factor based on their degree of importance for the types of samples you analyze. Be careful to take the evaluation in the direction you want to go and not where the vendor wants to take it. In other words, it is important to compare apples with apples and not to be talked into comparing an apple with an orange that looks like an apple. However, be prepared that there might not be a clear-cut winner at the end of the evaluation. So talk to as many users in your field as you possibly can — not only ones given to you as references by the vendor, but ones chosen by yourself. This approach will give you a very good indication of the real-world capabilities of the instrument, which can often be overlooked at a demonstration.
Never forget that it is a very competitive marketplace, and that your business is extremely important to all of the ICP-MS vendors. You may be pulled in many different directions by your own colleagues, external people who are advising you, and the vendors who want to influence your choice. Good luck with your evaluation!
(1) R. Thomas, Practical Guide to ICP-MS: A Tutorial for Beginners, Third Edition (CRC Press, Boca Raton, Florida, ).
(2) K. Nottingham, Anal. Chem., 35–38A (January 1, ). http://pubs.acs.org/subscribe/journals/ancham-a/76/i01/toc/toc_i01.html.
(3) Royal Society of Chemistry, Report by the Analytical Methods Committee, The Analyst122, 393–408 ().
(4) Inductively Coupled Plasma Mass Spectrometry: An Introduction to ICP Spectrometries for Elemental Analysis, A. Montasser, Ed. (Wiley-VCH, Weinheim, Germany, ), pp. 16–28, Chapter 1.4.
(5) "How to Select an ICP Mass Spectrometer: The Most Important Analytical Consideration," Pittcon, Short Course. http://ca.pittcon.org/Technical+Program/tpabstra14.nsf/SCoursesByCat/FEAD9A9CEBFBECC03?opendocument.
(6) PlasmaChem Listserver: A discussion group for plasma spectrochemists worldwide, Syracuse University, New York. http://www.lsoft.com/scripts/wl.exe?SL1=PLASMACHEM-L&H=LISTSERV.SYR.EDU.
Robert Thomas is a consultant and science writer specializing in trace element analysis. This installment was printed with permission and adapted from reference 1.
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Robert Thomas
The following article is adapted from a chapter in the author’s textbook, Practical Guide to ICP-MS and Other AS Techniques: A Tutorial for Beginners, published by CRC Press (ISBN: ). More information about the book can be found at the following link: https://www.routledge.com/Practical-Guide-to-ICP- MS-and-Other-Atomic-Spectroscopy-Techniques-A-Tutorial/Thomas/p/ book/#
The components of an inductively coupled plasma (ICP) mass spectrometer are generally more complex than other atomic spectroscopic techniques, and as a result, more time is required to carry out routine maintenance to ensure that the instrument is performing to the best of its ability. Some tasks involve a simple visual inspection of a part, whereas others involve cleaning or changing components on a regular basis. However, routine maintenance is such a critical part of owning an ICP-mass spectroscopy (MS) system that it can impact both the performance and the lifetime of the instrument, particularly with complex samples.
The fundamental principle of ICP-MS, which gives the technique its unequalled isotopic selectivity and sensitivity, also unfortunately contributes to some of its weaknesses. The fact that the sample “flows into” the spectrometer and is not “passed by it,” such as flame atomic absorption (AA) and radial inductively coupled plasma optical emission spectroscopy (ICP-OES), means that the potential for thermal problems, corrosion, chemical attack, blockage, matrix deposits, and drift is much higher than with the other atomic spectrometry (AS) techniques. However, being fully aware of this fact and carrying out regular inspection of instrumental components can reduce and sometimes eliminate many of these potential problem areas. There is no question that a laboratory which initiates a routine maintenance schedule stands a much better chance of having an instrument ready and available for analysis whenever it is needed, compared to a laboratory that basically ignores these issues and assumes the instrument will look after itself.
Let us now look at the areas of the instrument that a user needs to pay attention to. I will not go into great detail but just give a brief overview of what is important, so you can compare it with maintenance procedures of other trace element techniques you are more familiar with. These areas should be very similar with all commercial ICP-MS systems but depending on the design of the instrument and the types of samples being analyzed, the regularity of changing or cleaning components might be slightly different (particularly if the instrument is being used for solid sampling techniques such as laser ablation work). The main areas that require inspection and maintenance on a routine or semi-routine basis include the following:
Other areas of the instrument require less attention, but nevertheless the user should also be aware of maintenance procedures required to maximize their lifetime. They will be discussed at the end of this section.
Note: It is not the intent to go into the fundamental principles of these instrumental components. However, this article will discuss the factors that impact their routine use. It’s also worth emphasizing that the instrument manufacturer should always be consulted with regard to recommendations for specific tasks related to the design of their technology. You might also consider a preventative maintenance (PM) plan, which is basically an insurance policy in the case of any major or catastrophic failures (more details later in the article).
The sample introduction system, comprising the peristaltic/pneumatic pump, nebulizer, spray chamber, and drain system, takes the initial abuse from the sample matrix, and as a result, is an area of the ICP mass spectrometer that requires a great deal of attention. Brennan and associates published a very informative article on how best to maintain the sample introduction system (1). Let us now examine what kind of routine maintenance it requires.
If the instrument uses a peristaltic pump, the sample is pumped at about 1 mL/min into the nebulizer. The constant motion and pressure of the pump rollers on the pump tubing, which is typically made from a polymer-based material, ensures a continuous flow of liquid to the nebulizer. However, over time, this constant pressure of the rollers on the pump tubing has the tendency to stretch it, which changes its internal diameter, and, therefore, the amount of sample being delivered to the nebulizer. The impact could be a change in the analyte intensity, and therefore, a degradation in short-term stability.
Therefore, the condition of the pump tubing should be examined every few days, particularly if your laboratory has a high sample workload or if extremely corrosive solutions are being analyzed. The peristaltic pump tubing is probably one of the most neglected areas, so it is absolutely essential that it be a part of your routine maintenance schedule. Here are some suggested tips to reduce pump tubing–based problems:
A very useful tool to diagnose any problems associated with the peristaltic pump tubing (or the nebulizer) is a digital thermoelectric flow meter. By inserting this device in the sample line, you always know the actual rate of sample uptake to your nebulizer. This enhances the day-to-day reproducibility of your results and reduces the need to repeat measurements due to a blocked nebulizer, worn pump tubing or incorrect clamping of the pump tube. In addition, the borosilicate glass sample path ensures that there is no memory effect or sample contamination. A commercially-available digital thermoelectric flow meter is shown in Figure 1.
The frequency of nebulizer maintenance will primarily depend on the types of samples being analyzed and the design of nebulizer being used. For example, in a cross-flow nebulizer, the argon gas is directed at right angles to the sample capillary tip, in contrast to the concentric or microflow nebulizer, where the gas flow is parallel to the capillary. This can be seen in Figures 2 and 3, which show schematics of a conventional concentric and cross-flow nebulizer, respectively.
The larger diameter of the liquid capillary and longer distance between the liquid and gas tips of the cross-flow design make it far more tolerant to dissolved solids and suspended particles in the sample than the concentric design. On the other hand, aerosol generation of a cross-flow nebulizer is far less efficient than a concentric nebulizer, and therefore it produces droplets of less optimum size than that required for the ionization process. As a result, concentric nebulizers generally produce higher sensitivity and slightly better precision than the cross-flow design but are more prone to clogging.
So, the choice of which nebulizer to use is usually based on the types of samples being aspirated and the data quality objectives of the analysis. However, whichever type is being used, attention should be paid to the tip of the nebulizer to ensure it is not getting blocked. Sometimes, microscopic particles can build up on the tip of the nebulizer without the operator noticing, which, over time, can cause a loss of sensitivity, imprecision, and poor long-term stability. In addition, O-rings and the sample capillary can be affected by the corrosive solutions being aspirated, which can also degrade performance. For these reasons, the nebulizer should always be a part of the regular maintenance schedule. Some of the most common things to check include the following:
The digital thermoelectric flow meter is also very useful to diagnose problems with the nebulizer, even if you are using a self-aspirating nebulizer, because you are concerned about imprecision from the pulsing of a peristaltic pump. By placing the device inline, you always know what your sample uptake is and can take immediate corrective action if there is any change. You can also record your sample flow in order to check that you are using the same flow from day to day.
If the flow meter indicates a blocked nebulizer tip, there are also nebulizer-cleaning devices offered by most of the third-party consumables/accessories companies. Traditionally if particulate matter from the sample lodges itself in the end of the nebulizer, cleaning wires or ultrasonic baths were the only way to remove the obstruction, which often resulted in permanent damage. These new cleaning devices are designed to efficiently deliver a pressurized cleanser through the nebulizer capillary to safely dislodge particle build-up and thoroughly clean the nebulizer, without fear of damage.
The most common type of spray chambers used in commercial ICP-MS instrumentation are the double-pass and cyclonic designs.
The Scott design is the most commonly used double-pass S/C, which selects the small droplets by directing the aerosol into a central tube. The larger droplets emerge from the tube, and by gravity, exit the spray chamber via a drain tube. The liquid in the drain tube is kept at positive pressure (usually by way of a loop), which forces the small droplets back between the outer wall and the central tube; they emerge from the spray chamber into the sample injector of the plasma torch. Scott double-pass spray chambers come in a variety of shapes, sizes, and materials, but are generally considered the most rugged design for routine use. Figure 4 shows a double-pass spray chamber (made of a polymer material) coupled to a cross-flow nebulizer.
The cyclonic spray chamber operates by centrifugal force, where droplets are discriminated according to their size by means of a vortex produced by the tangential flow of the sample aerosol and argon gas inside the chamber. Smaller droplets are carried with the gas stream into the ICP-MS, whereas the larger droplets impinge on the walls and fall out through the drain. It is generally accepted that a cyclonic spray chamber has a higher sampling efficiency, which for clean samples translates into higher sensitivity and lower detection limits. However, the droplet size distribution appears to be different from a double-pass design, and for certain types of samples can give slightly inferior precision. Beres and coworkers published a very useful study describing the capabilities of a cyclonic spray chamber (2). Figure 5 shows a cyclonic spray chamber with a concentric nebulizer.
The most important maintenance task with regard to the spray chambers is to make sure that the drain is functioning properly. A malfunctioning or leaking drain can produce a change in the spray chamber backpressure, producing fluctuations in the analyte signal, resulting in erratic and imprecise data. Less frequent problems can result from degradation of O-rings between the spray chamber and sample injector of the plasma torch. Typical maintenance procedures regarding the spray chamber include the following:
Not only is the plasma torch/sample injector exposed to the sample matrix and solvent, but they also have to sustain the analytical plasma at approximately -10,000 K. This combination makes for a very hostile environment and therefore is an area of the system that requires regular inspection and maintenance. A plasma torch positioned in the RF coil is shown in Figure 6.
As a result, one of the main problems is staining and discoloration of the outer tube of the quartz torch because of heat and the corrosiveness of the liquid sample. If the problem is serious enough, it has the potential to cause electrical arcing. Another potential problem area is blockage of the sample injector due to matrix components in the sample. As the aerosol exits the sample injector, desolvation takes place, and the sample changes from small liquid droplets to minute solid particles prior to entering the base of the plasma. Unfortunately, with some sample matrices, these particles can deposit themselves on the tip of the sample injector over time, leading to possible clogging and drift. In fact, this can be a potentially serious problem when aspirating organic solvents, because carbon deposits can rapidly build up on the sample injector and cones unless a small amount of oxygen is added to the nebulizer gas flow. Some torches also use metal plates or shields to reduce the secondary discharge between the plasma and the interface. These are consumable items, because of the intense heat and the effect of the RF field on the shield. A shield in poor condition can affect instrument performance, so the user should always be aware of this and replace it when necessary.
Some useful maintenance tips with regard to the torch area include the following:
It’s also worth emphasizing that based on the design of the RF generator, the power amplifier (PA) tube is considered a consumable. There is no question that depending on the instrument’s age and the frequency of operation, the life of the PA tube could be seriously impacted. These components are not inexpensive and if one should unexpectedly fail, you will be faced with the cost of a service engineer’s time in addition to the cost of the tube, not to mention the downtime of the instrument.
As the name suggests, the interface is the region of the ICP mass spectrometer where the plasma discharge at atmospheric pressure is “coupled” to the mass spectrometer at 10−6 torr by way of two or three interface cones—a sampler and skimmer (and sometimes a hyper skimmer). This coupling of a high-temperature ionization source such as an ICP to the metallic interface of the mass spectrometer imposes demands on this region of the instrument that can be very challenging. When this is combined with matrix, solvent, and analyte ions together with particulates and neutral species being directed at high velocity at the interface cones, the result is an extremely harsh environment. The most common types of problems associated with the interface are blocking or corrosion of the sampler cone and, to a lesser extent, the skimmer cone. A schematic of the interface cones showing potential areas of blockage are shown in Figure 7.
A blockage is not always obvious, because often the buildup of material on the cone or corrosion around the orifice can take a long time to reveal itself. For that reason, the sampler and skimmer interface cones have to be inspected and cleaned on a regular basis. The frequency will often depend on the types of samples being analyzed and also the design of the ICP mass spectrometer. Neufeld and coworkers wrote an excellent article on maintaining the cones and interface area to maximize productivity and uptime (3). For example, it is well documented that a secondary discharge at the interface can prematurely discolor and degrade the sampler cone, especially when complex matrices are being analyzed or if the instrument is being used for high sample throughput. Note: More information about the impact of a secondary discharge were described in an earlier chapter of the book.
Besides the cones, the metal interface housing itself is also exposed to the high-temperature plasma. Therefore, it usually needs to be cooled by water, either from a continuous water supply or a recirculating system, containing some kind of antifreeze or corrosion inhibitor (Note: Some of the new designs using proprietary RF technology are not water cooled). Recirculating systems are probably more widely used because the temperature of the interface can be controlled much better. There is no real routine maintenance involved with the interface housing, except maybe to check the quality of the coolant from time to time, to make sure there is no corrosion of the interface cooling system. If for any reason the interface gets too hot, there are usually built-in safety interlocks that will turn the plasma off. Some useful hints to prolong the lifetime of the interface and cones include the following:
Note: There are many different cone materials and inserts used nowadays, including nickel, platinum, copper, aluminum, and stainless steel.
The ion optic system is usually positioned just behind or close to the skimmer cone to take advantage of the maximum number of ions entering the mass spectrometer. There are many different commercial designs and layouts, but they all have one attribute in common, and that is to transport the maximum number of analyte ions while allowing the minimum number of matrix ions, particulates and neutral species through to the mass analyzer.
The ion-focusing system is not traditionally thought of as a component that needs frequent inspection, but because of its proximity to the interface region, it can accumulate minute particulates and neutral species that over time can dislodge, find their way into the mass analyzer, and affect instrument performance. Signs of a dirty or contaminated ion optic system are poor stability or a need to gradually increase lens voltages over time. For that reason, no matter what design of ion optics is used; inspection and cleaning every 3–6 months (depending on workload and sample type) should be an integral part of a preventative maintenance plan. Some useful maintenance tips for the ion optics to ensure maximum ion transmission and good stability include the following:
Typically, two roughing pumps are used in commercial instruments. One pump is used on the interface region, and the other is used as a backup to the turbomolecular pumps on the main vacuum chamber. They are usually oil-based rotary or diffusion pumps, where the oil needs to be changed on a regular basis, depending on the instrument usage. The oil in the interface pump will need changing more often than the one on the main vacuum chamber because it is pumping for a longer period. A good indication of when the oil needs to be changed is the color in the “viewing glass.” If it appears dark brown, there is a good chance that heat has degraded its lubricating properties, and it needs to be changed. With the roughing pump on the interface, the oil should be changed every 1–2 months, and with the main vacuum chamber pump, it should be changed every 3–6 months. These times are only approximations and will vary depending on the sample workload and the time the instrument is actually running. Some important tips when changing the roughing pump oil:
Most of the electronic components, especially the ones in the RF generator, are air-cooled. Therefore, the air filters should be checked, cleaned, or replaced on a fairly regular basis. Although this is not carried out as routinely as the sample introduction system, a typical time frame to inspect the air filters is every 3–6 months, depending on the workload and instrument usage.
It is also important to emphasize that other components of the ICP mass spectrometer have a finite lifetime and will need to be replaced or at least inspected from time to time. These components are not considered a part of the routine maintenance schedule, and usually require a service engineer (or at least an experienced user) to clean or to change them. The following area that might require cleaning from time to time.
Depending on the usage and levels of ion signals measured on a routine basis, the electron multiplier should last about 12 months. A sign of a failing detector is a rapid decrease in the “gain” setting despite attempts to increase the detector voltage. The lifetime of a detector can be increased by avoiding measurements at masses that produce extremely high ion signals, such as those associated with the argon gas, solvent or acid used to dissolve the sample (for example, hydrogen, oxygen, and nitrogen), or any mass associated with the matrix itself. It is important to emphasize that the detector should be replaced by an experienced person wearing gloves, to reduce the possibility of contamination from grease or organic/water vapor from the operator’s hands. It is advisable that a spare detector be purchased with the instrument.
Most of the instruments running today use two turbomolecular pumps to create the operating vacuum for the main mass analyzer/detector chamber and the ion optic region. However, some of the newer instruments use a single, twin-throated turbo pump. The lifetime of turbo pumps, in general, is dependent on a number of factors, including the pumping capacity of the pump (usually expressed as liters per second), the size (or volume) of the vacuum chamber to be pumped, the orifice diameter of the interface cones (in mm), and the time the instrument is running. Although some instruments still use the same turbo pumps after 5–10 years of operation, the normal lifetime of a pump in an instrument that has a reasonably high sample workload is on the order of 3–4 years. This is an approximation and will obviously vary depending on the make and design of the pump (especially the type of bearings used). As the turbomolecular pump is one of the most expensive components of an ICP-MS system, this should be factored into the overall running costs of the instrument over its operating lifetime.
It is worth pointing out that although the turbo pump is not generally included in routine maintenance, most instruments use a “Penning” (or similar) gauge to monitor the vacuum in the main chamber. Unfortunately, this gauge can become dirty over time and lose its ability to measure the correct pressure. The frequency of this is almost impossible to predict but is closely related to types and numbers of samples analyzed. A sudden drop in pressure or fluctuations in the signal are two of the most common indications of a dirty Penning gauge. When this happens, the gauge must be removed and cleaned. This should be performed by an experienced operator or service engineer because removing the gauge, cleaning it, maintaining the correct electrode geometry, and reinstalling it correctly into the instrument is a fairly complicated procedure. It is further complicated by the fact that a Penning gauge is operated at high voltage.
Under normal circumstances, there is no need for the operator to be concerned about routine maintenance of the mass analyzer or collision/reaction cell. With modern turbomolecular pumping systems, it is highly unlikely there will be any pump contamination problems associated with the quadrupole, magnetic sector, or time-of-flight (TOF) mass analyzer. And very few sample matrix components ever make it into the mass spectrometer region, which dramatically reduces the frequency of routine maintenance tasks. This certainly was not the case with some of the early instruments that used oil-based diffusion pumps, because many researchers found that the quadrupole and pre-filters were contaminated by oil vapors from the pumps. Today, it is fairly common for turbomolecular-based mass analyzers to require no maintenance of the analyzer or the collision/reaction cell quadrupole rods over the lifetime of the instrument, other than an inspection carried out by a service engineer on an annual basis. However, in extreme cases, particularly with older instruments, removal and cleaning of the quadrupole assembly might be required to get acceptable peak resolution and abundance sensitivity performance.
The overriding message I would like to leave you with on this subject is that routine maintenance cannot be overemphasized in ICP-MS. Even though it might be considered a mundane and time-consuming chore, it can have a significant impact on the uptime of your instrument. Read the routine maintenance section of the operator’s manual and understand what is required. It is essential that time be scheduled on a weekly, monthly, and quarterly basis for preventative maintenance on your instrument. In addition, you should budget for an annual preventative maintenance contract under which the service engineer checks out all the important instrumental components and systems on a regular basis to make sure they are all working correctly. This might not be as critical if you work in an academic environment, where the instrument might be down for extended periods, but in my opinion, it is absolutely critical if you work in commercial laboratory, which is using the instrument to generate revenue. Although the cost of a PM contract might seem daunting, it typically includes one PM visit per year, and unlimited technical support, on-site repair visits and the price of replacement parts. You should check with your specific vendor/supplier for more detailed information.
There is no question that spending the time to keep your ICP mass spectrometer in good working order can mean the difference between owning an instrument whose performance could be slowly degrading without your knowledge or one that is always working in “peak” condition. And one of the ways to ensure this is to have a highly skilled operator, who knows how to keep the instrument optimized and working to its full potential.
And finally, I must give credit to the instrument designers and accessories suppliers in making today’s instrumentation extremely easy to maintain and keep clean. The technique is over 40 years old, and its commercial success has been built on acceptance by the analytical community for applying it to truly routine, real-world analysis. The only areas that need cleaning on a regular basis are the sample introduction system and interface cones, depending on usage and sample matrices being aspirated. And many of today’s instruments have alarms which can be set to remind the operator when it’s time for the few preventative maintenance tasks that are required, such as oil changes and tubing replacement. Some systems will even display how many hours various components have been used and when they might need attention. So even though routine maintenance is very important, instrument vendors and sampling accessories companies have put a great deal of time and effort into making this as straightforward and seamless as possible. Besides the major ICP-MS instrument vendors, here is a partial list of some of the companies that supply interface/torch/sample introduction/sampling accessories for the ICP-MS marketplace. Please contact them for more detailed support and troubleshooting information.
(1) Neufeld, L. ICP-MS Interface Cones: Maintaining the Critical Interface Between the Mass Spectrometer and the Plasma Discharge to Optimize Performance and Maximize Instrument Productivity. Spectroscopy , 34 (7), 12–17. https://www.spectroscopyonline.com/view/icp-ms-interface-cones-maintaining-critical-interface-between-mass-spectrometer-and-plasma-discharge
(2) Beres, S. A.; Bruckner, P. H.; Denoyer, E. R. Performance Evaluation of a Cyclonic Spray Chamber for ICP-MS. At. Spectrosc. , 15(2), 96–99. https://url.us.m.mimecastprotect.com/s/Oq57CKrR2RiP9x6ouMf0C5cU1h?domain=scientificsolutions1.com
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