General comments
This paper describes improvements in the multi-scheme chemical ionization inlet (Rissanen et al., 2019) which apparently have led to detection limits using bromide CIMS comparable to those of the standard Eisele nitrate CIMS inlet. The paper discusses the calibration of the nitrate and bromide chemical ionization units and then investigates the dependence of the bromide method on humidity and instrument settings. Finally, the paper discusses potential ambiguities in the detection of iodic acid that may be caused by reactions of iodine oxides with the reagent ions in the instrument inlet.
This paper presents valuable research that should be published after mayor revisions are undertaken.
I’m struggling to understand what is this paper exactly about in view of the emphasis given in the tittle to the inlet characterization and the mainly Br CIMS-related material presented. The title states that it deals with the characterization of the MION2 inlet, but throughout the paper the experiments refer to the characterization of a particular (optimized) configuration of this inlet for Br- as reagent, using NO3- as a reference. Certain modifications pertaining to the inlet as such, as the new design of the source electrodes and flows, are described in section 2.1, but the actual characterization of the inlet stops there. From this point on, it is the new inlet what it is actually used to characterize and optimize the bromide CIMS method. I think that the authors have done a good job on that and therefore the emphasis should be there. The water dependence of the Br-CIMS signals and the possible strategies to reduce it are relevant for any type of atmospheric pressure ionization inlet, so this is not really a characterization of MION2.
Finally, some material is presented related to the detection of HIO3 by nitrate and bromide CIMS and potential interferences by IxOy. A significant fraction of this material has already been presented by Finkenzeller et al. 2022 and I don’t think it is necessary to repeat it here, especially qualitative or semi-quantitative theoretical discussions. I do feel that this section needs to be reworked to make it fit better into the general context of the paper, e.g. a section about potential interferences in any instrument’s inlet. I see a problem with the fact that the interferences are mostly related to the nitrate CIMS system, while the paper is very Br-centered. Nevertheless, the emphasis should be on the new experimental data that has been obtained, which seems to indicate that the nitrate and bromide CIMS signals attributed to HIO3 are linearly related, which supports the conclusion of the authors about the absence of IxOy interferences under atmospherically relevant conditions.
Specific comments:
Lines 241-251. Please indicate uncertainties in the iodine output rate of the permeation tube.
Line 209. Actually section 2.2.2 refers mainly to the development of an iodine source and quantification of its output rate, rather than calibration of the instrument as such, so I would suggest calling this section something in the line of “Development of an iodine source”.
Line 276. There is a statement above saying that to quantify the concentrations of H2SO4, HOI, and HO2, a model was developed (line 192), but there is no description of why such model may be necessary. I think the authors could have mentioned briefly radial diffusion, wall losses and secondary reactions of the precursor species that may interfere in the determination of the concentration of the analyte.
Line 276. The term “chemical dynamics” is confusing in this context and does not represent what the code does, which appears to be chemical kinetics and transport rather than actual reaction dynamics.
Line 381. Please add an appropriate MESMER reference. I notice that these calculations were already reported by Finkenzeller et al 2022, and hence a reference to that paper should be enough.
Section 3.1. What is the difference between the H2SO4 concentration calculated directly from initial OH and from the model? Figure 2 suggests that the losses of OH are minimal at the sampling axis. Does the MARFORCE model help to reduce uncertainty significantly? Similarly, the I2 calibration scheme appears to be well designed to produce full conversion of OH into HOI in a large excess of I2. Does the model reveal any significant loss of OH that is worth considering?
Line 397. The readers of this paper will be most likely familiar with these “normalized ratios”, but for a more general audience please explain briefly what is the measured quantity that you are calibrating and why and how you normalize it.
Table 1. What is the value in reporting detection limits for iodine oxides if they are based in mere estimated calibration factors as indicated in the table footnote? Where do these calibration factors come from?
Figure 3. Regarding the curvature of the HOI calibration plots, I do not find the response to the previous reviewers or the modifications introduced in the manuscript very helpful. First of all, there is no mention to the curved calibration curves in the modified text. If the authors believe that this is a result of the sensitivity to water of HIO detection by Br- CIMS, they should explain how does this actually reflect in the curvature of the calibrations for Tower 1 and 2. Also, does it make sense to fit straight lines through the HIO log-log data? Why not a quadratic dependence?
Line 638. Reaction (5) does not involve breaking multiple I-O and N-O bonds. It simply requires breaking a terminal I-O of I2O3 and forming a new I-O with halogen bonding character with the NO3 moiety, so I am not so sure why this should be less likely than proton transfer. Please rephrase or provide a more compelling argument.
Line 647. The main piece of evidence for reactions (5) and (6) is the recurrent observation of the conspicuous IONO2.NO3- signal (m/z=250.9), which has been reported in all previous field, laboratory and chamber nitrate CIMS work, but is not mentioned in this study. While in field studies (e.g. Baccarini et al. 2020) this signal could be indicative of ambient IONO2, in laboratory and chamber experiments it has been observed in the absence of NO2 (all the works cited by the authors). What is the origin of this ion? This paper deals with a thorough experimental characterization of CIMS instruments, and therefore an investigation of such “measurement artefact” (Finkenzeller et al. 2022) could be expected in this section, not least because this signal could prove useful as method to detect IONO2 in the atmosphere. I would be interested in seeing a plot of IONO2.NO3- vs IO3- as those presented in figure 9. That could shed some light into the origin of that signal (whose IONO2.Br- analogue is not observed in the Br- case, according to Finkenzeller et al. 2022).
Lines 650-653. The molecular parameters employed in this calculation are not provided by the authors, so I cannot reproduce it. Anyway, Finkenzeller et al. 2022 has reported this result already, and therefore I do not think it should be reported here again, specially considering that the uncertain PES does not enable a reliable determination of branching ratios using MESMER. For saying something meaningful from a theoretical point of view a more in-depth analysis of the PES of this process is needed. I would just ignore this or refer to Finkenzeller et al. 2022.
Lines 663-665. Finkenzeller et al. 2022 argues that HIO3 originates from I2O2+O3+H2O, so please rephrase to indicate I2Oy with y>2.
Lines 668-670. The authors say that they capitalise on the fact that IO is a good indicator of the intensity of atmospheric iodine activities (please reconsider the term “activities”) and that it influences the ratio of iodine oxides to oxoacids. But then they don’t mention IO again. Please clarify. Have you used IO to tune the iodine concentration in the laminar flow tube experiments? Do you have evidence that from a certain IO concentration IxOy formation starts to dominate the signals? In general I think the description of the experiments could be better and that more juice could be extracted from the analysis of the data obtained.
Figure 9. The top right panel is an important figure that shows a linear dependence between the IO3- signal measured by nitrate CIMS and the HIO3.Br- signal measured by bromide CIMS. This would indicate in principle that both signals have the same origin and in that sense is very compelling. I would focus the discussion of this section mainly on these measurements.
Why do the bromide CIMS signals stop at Norm. IO3- signal = 0.015 cps cps-1? Where are the bromide CIMS data corresponding to the highest ozone nitrate CIMS data in the top left panel?
Lines 680-683. The water-mediated reactions producing oxoacids may go at a faster rate than the iodine oxide recombination reactions for very low iodine concentrations. But still, HIO3 nucleation is not very favourable energetically and the authors have proposed in previous work “a critical role of HIO2” in stabilizing the HIO3 clusters (Zhang et al. 2022). HIO2, which has an uncertain originin the atmosphere as HIO3, is measured at very low concentrations by CIMS, but of the same order of magnitude than those of I2O3 and I2O4. Can we then rule out that I2O3 and I2O4 affect the formation of particles under boundary layer conditions even though they are at low concentrations? Admittedly, this discussion goes beyond the scope of the paper, but I would suggest the authors to smooth their statement if they choose to keep this section.
Summary. Rather than changing the name of the section following the comment by a previous reviewer, I think the authors should try to draw some conclusions from their work. The final summary section is very similar to the abstract.
Table A1. Replace the equal signs by arrows.
Figure A8. I don’t find this figure particularly useful for a paper in AMT. Remove? |
In "Characterisation of the multi-scheme chemical ionisation inlet-2 and the detection of gaseous iodine species", authors Xu-Cheng He and co-workers describe a new version of an inlet (MION) for chemical ionization mass spectrometry (CIMS) that allows for switching between multiple schemes and reaction times. Overall, they are presenting careful work that employed scientifically sound and appropriate methodology. Its findings will be very interesting for the CIMS community, especially of course if using a MION inlet or similar. Unfortunately, the manuscript itself was not prepared as carefully.
General positive points are the abstract, which I believe provides a good summary (except for some ambiguities noted below), as well as the figures, which are of mostly easy to read and of high quality and well-chosen by their relevance to the presented research.
However, for an AMT paper introducing a new CIMS inlet, its description is confusing and substantially lacking important details, as I try to elaborate in my detailed comments. This deficiency is most apparent in Section 2 (Methods), but found also in some parts of Section 3 ("Results") where additional experimental and analytical methodology are described.
In addition, the text will need some proofreading/copy-editing to deal with numerous grammatical errors. Some semantic errors disrupt the reading as well. Nonetheless, the text is in principle understandable.
For these reason, I suggest to reconsider the manuscript only after major revisions.
[Disclaimer: I do not feel qualified to judge the various methods used for the DFT calculations (Section 2.4).]
Specific comments:
Title: Much of this study deals with the Br- ionization scheme, and indeed provides useful insights into that specific scheme in particular, applicable also beyond the MION inlet systems. NO3-, for the most part, is rather used as a reference. Anyway, I would point that out already in the title. E.g., "... using Br- as reagent", or "... using Br- and NO3- as reagents".
Abstract: I suggest disclosing somewhere near the beginning that MION inlets operate (or are at least designed to operate) at atmospheric pressure.
L4 (abstract): "generally more robust operation" ... please be more specific.
L20 (abstract): Should specify if the detection limit for H2SO4 is achieved via Br- or NO3- reagents (or both).
L22 (abstract): again, "generally more robust" is too vague.
L95-102: Somewhat confusing description of the MION inlet. Not the only issue, but also: is "reaction time" the same as "ionisation time"? Most critically maybe: how does MION2 allow for two CI methods with same reaction time, and why was that not possible with the MION1? Please clarify.
After also checking Fig. 1, I think I get it. But now I wonder why only two CI at the same time (and same reaction time) (L101), and not three? (Or even six, if the polarity can be switched quickly as well, which remains unclear. And does "two or more (up to six)" simply mean "up to six" or something more elaborate, possibly including limitations regarding reaction time choice as in MION1?)
Fig. 1: I suggest to indicate the directions of the various flows, to make the drawing easier to comprehend.
L108: How was the sample flow provided?
L110-122: What are typical/required/desired reagent flows, reagent concentrations, and purge flow(s!)?
Also, how are the reagent concentrations facilitated?
Fig. A1 is missing the "purge flow" (and L119-122).
L124-125: How is that "operational stability" manifest or determined? If elaborated on later, please state so. If not, be more specific.
L125-127: How have the ion optics been upgraded? I am not expecting much details, but at least some indication of what type of effort was undertaken and required to increase "reagent ion transmission" (by which the authors might actually mean the amount of reagent ions ending up being detected?)?
Section 2.2.1: What exactly is the "calibration source"? It is referred to multiple times, but never actually specified what it is, except that OH radicals are generated "in it", or how it connects to other parts of the setup. (For example, are the OH radicals actively mixed into that SO2- and I2- containing gas mixture, or is the gas mixture going through a region where OH radicals is generated, and the "source" is the sum of something like that?)
Similarly, Fig. A2 simply refers to a mysterious "calibration box".
Section 2.2.2: 1st paragraph is a general introduction to the problem that may fit better to the Introduction section.
Section 2.2.2: Unclear what was done why, and how the I2 was ultimately supplied during the MION calibration experiments. For example, was the permeation tube output used directly, and the process from dissolution in hexane to quantifying a concentrated solution of the derivative was only to gain knowledge of the I2 permeation tube output rate? (Which is presented as the conclusion of the main paragraph.)
Eq. 1: Q is not defined.
Table 1, Section 3.1: Detection limits are given for MION2/T1, MION2/T2 and Eisele inlets. But for H2SO4, either NO3- or Br- were used on MION2/T1, so, which reagent ion do the reported detection limits correspond to? And the Eisele inlet presumably used NO3-? If so, is there a reason that the NO3- scheme with MION2 was not tested for HIO3, as the Eisele inlet was?
Also, it is unclear at this stage what is meant by "APi1" and "APi2".
~L344: Is fragmentation at atmospheric pressure (as opposed to only in the ion optics) responsible for the HO2 cal factors for T1 vs T2 being only a factor of 2.3 apart?
L360: I am not following the final sentence. As the authors just pointed out, they found (experimentally) that more strongly fragmenting instrument settings reduced sensitivity to HOI, agreeing with somewhat weaker binding between reagent and analyte, compared to the H2SO4 case, expected theoretically. So, why would one anyway blame "iodine chemistry schemes" or "differences in experimental conditions"? As those terms are rather vague, I may just misunderstand what is being pointed at. (Oh, is it differences in chemistries between the cited studies and this study?)
L383: Please provide a reference to that "earlier study".
L420: I disagree with the implication of the first half of this sentence. I agree that, for instance, within a typical day, ambient absolute humidity often does not vary by very much. But within, say, a week, one would expect substantial variations. And more so the longer of a time period is being considered...
Section 3.4: Figure A9 needs some more explanation, maybe via annotations in the figure (photo). Unclear what is what.
Section 3.5: I appreciate that experiments were carried out using two independent detectors and sample sources. But the discussion of the respective differences is awfully short. (And merely from a statistics point of view, a sample size of two is not that much better than a sample size of one.) Hence, is there anything useful to say about differences between APi1 and APi2 (or APi3 for that matter), beyond time since service? E.g., details on tunings, or purity of gas or calibrant supplies, etc.?
~L553: How was DeltaV50 determined? The shapes of the signal-remaining curves (Fig. 6) indicate that for several species the maximum is not obtained at the lowest tested DeltaV. The clearest case is H2O, for which the signal-remaining drops to 50% at ~3-4V, but the curve is steep and a higher reference value (signal-remaining = 1) would likely be obtained at yet "softer" settings (e.g., DeltaV < 2V). Correspondingly, if dV50 is simply the 50% point from Fig. 6, I expect several points in Fig. 7 being "too high".
Fig. 7: It would be very useful if the same color coding was used in Figs. 6 and 7, i.e., same color for same species.
Section 3.7: L568 vs L580 appear to contradict each other, even though using same reference. Is Reaction 4 exo- or endothermic?
Section 4 ("Conclusions"): This Section is really a summary of the results and the major discussion points presented in Section 3. With the exception of one or two sentences, it does not provide any new discussion nor actual conclusions. Consequently, it should be named accordingly. (Whereas Section 3 would be more aptly named "Results and Discussion".)
Technical comments:
L14: More correct, I believe, to write "We calibrated for [...]"
L34: "spectrometer" -> "spectrometry" (for grammar)
L38: missing article ("forming a relatively")
[I will stop commenting on grammatical errors (or semantical errors or typos). Some proofreading/copy-editing service will be more suitable.]
L81: I assume the authors mean the LOD is higher (hence worse), not lower
Fig. A2: stain -> stainless
L150: "calibrator" or "calibration"?
L238-239: I am counting three ways, not two.