the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Quality assurance and quality control of atmospheric organosulfates measured using hydrophilic interaction liquid chromatography (HILIC)
Abstract. As a crucial constituent of fine particulate matter (PM2.5), secondary organic aerosols (SOA) influence public health, regional air quality, and global climate patterns. This paper highlights the use of Hydrophilic interaction liquid chromatography (HILIC) which effectively retains strongly polar analytes that might exhibit incomplete or no retention in reverse chromatography, resulting in superior separation efficiency.
A HILIC column was used to analyze 7 standards, environmental standards (1648a and 1649b), and samples collected in urban environments in the Pearl River Delta region of Guangzhou. That serve as valuable reference points for evaluating the organic composition of the atmospheric environment. The results indicate a high degree of accuracy in the analytical method, sodium octyl-d17 sulfate serves as the internal standard, with a linear correlation coefficient of the 7 standards, boasting a linear correlation coefficient R ranging from 0.987–0.999 and a slope, k, of the linear equation from 0.9662–2.2927. The instrument detection limit (IDLs) is established at 0.0026–0.0300 μg mL-1, while the method detection limit (MDLs) falls within the range of 0.0077–0.2300 ng m-3, demonstrating the method's exceptional sensitivity.
Since isoprene sulphates are highly polar due to containing a hydrophilic bond to the hydroxyl group and a hydrophobic bond to the sulphate, and as such showed strong retention using this method. This technique employs Sodium ethyl sulfate and Sodium octyl sulfate standards for semi-quantitative compound analysis isoprene-derived OSs, the error in sample analysis (EA) ranged from 12.25–95.26 % and the two standards maintaining a consistent recovery rate between 116 %–131 % and 86 %–127 %. These findings indicate a high level of precision when semi-quantifying compounds with similar structural characteristics, affirming the analysis method's minimal relative error and underscoring its repeatability, process stability, and the reliability of its results for isoprene OSs. To enhance the method's reliability assessment, the study analyzed polar organic components of standard particulate matter samples (1648a and 1649b), providing precise determinations of several isoprene OSs using this method. Methyltetrol sulfate (m/z 215) is the highest concentration in the ambient samples, up to 67.33 ng m-3 at daytime. These results serve as valuable reference points for assessing the organic composition of the atmospheric environment.
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RC1: 'Comment on amt-2023-250', Anonymous Referee #1, 09 Feb 2024
Please see detailed comments in the attached file
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AC1: 'Reply on RC1', Ping Liu, 27 Mar 2024
We sincerely appreciate your valuable comments, which have substantially enhanced the quality of the manuscript and improved the manuscript. Below, we provide point-by-point responses to the reviewers' comments.
Comments 1-4:
Reply: See the supplement file "Response to reviews".
Comment 5: Figure 1. The specific value for m/z HSO4- should keep same. m/z 96.9 and m/z 97.1 can not be assigned to the same fragment ion in high resolution MS.
Reply: We revised, see the new Fig. 4, line 293.
Comment 6: Figure 1 and throughout the manuscript: The m/z values and concentration values must report the same correct number of significant figures.
Reply: We revised, see the new Fig. 4, line 293 and markup section.
Comment 7: “m/z” and “k” should be italic. Line 239: “SO4-”should be “·SO4-”; Line 269:“5.24.6.07” should be “5.24, 6.07”. Authors should also carefully check and correct other typos and grammar errors that are not listed here.
Reply: We revised, for “·SO4-”, see new line 286, for “5.24, 6.07”, see new line 314, and we also checked the full text and made changes, as detailed in the markup revised section.
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AC1: 'Reply on RC1', Ping Liu, 27 Mar 2024
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RC2: 'Comment on amt-2023-250', Anonymous Referee #2, 03 Mar 2024
General Comments:
This manuscript uses Hydrophilic Interaction Liquid Chromatography (HILIC) to analyze isoprene-derived organosulfates in the Pearl River Delta. The results show that the relative error is extremely small, the experimental reproducibility is high, the analysis procedure is stable, and the results are reliable. The research content aligns with the publication scope of the Atmospheric Measurement Techniques journal, and publication is recommended after revisions.
Specific Comments:
1) The full name of the abbreviations should be given at the first time the abbreviations appear. For example, “OSs” in Line 31, “ACN” in Line 114, etc.
2) Some figures and tables in the manuscript have not been referenced in the text, such as Table 3 and Figure 1. All figures and tables should be cited and introduced in the text.
3) Line 269: the dot between “5.24” and “6.07” should be a comma.
4) Line 289: the comma in this line should be a dot.
5) In Table 9, the column “retention time” is sometimes aligned with “daytime” and sometimes positioned between “daytime” and “nighttime”. Is this a formatting issue? If not, it should be explained in the manuscript.
Citation: https://doi.org/10.5194/amt-2023-250-RC2 -
AC2: 'Reply on RC2', Ping Liu, 27 Mar 2024
We greatly appreciate the time and effort you dedicated to thoroughly reviewing our manuscript. We have carefully considered each point and have made revisions accordingly. We believe that your input has significantly improved the manuscript. Below are our responses to each comment.
Comment 1: The full name of the abbreviations should be given at the first time the abbreviations appear. For example, “OSs” in Line 31, “ACN” in Line 114, etc.
Reply: We revised, see new lines 28 and 115, and we also checked the full text, see revision with markup for more details.
Comment 2: Some figures and tables in the manuscript have not been referenced in the text, such as Table 3 and Figure 1. All figures and tables should be cited and introduced in the text.
Reply: We revised, see new lines 213-216 and 290-292.
Comment 3: Line 269: the dot between “5.24” and “6.07” should be a comma.
Reply: We revised, see new line 314.
Comment 4: Line 289: the comma in this line should be a dot.
Reply: We revised, see new line 333.
Comment 5: In Table 9, the column “retention time” is sometimes aligned with “daytime” and sometimes positioned between “daytime” and “nighttime”. Is this a formatting issue? If not, it should be explained in the manuscript.
Reply: We are sorry, it's a formatting issue. We revised it, see new Table 10.
Citation: https://doi.org/10.5194/amt-2023-250-AC2
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AC2: 'Reply on RC2', Ping Liu, 27 Mar 2024
Status: closed
-
RC1: 'Comment on amt-2023-250', Anonymous Referee #1, 09 Feb 2024
Please see detailed comments in the attached file
-
AC1: 'Reply on RC1', Ping Liu, 27 Mar 2024
We sincerely appreciate your valuable comments, which have substantially enhanced the quality of the manuscript and improved the manuscript. Below, we provide point-by-point responses to the reviewers' comments.
Comments 1-4:
Reply: See the supplement file "Response to reviews".
Comment 5: Figure 1. The specific value for m/z HSO4- should keep same. m/z 96.9 and m/z 97.1 can not be assigned to the same fragment ion in high resolution MS.
Reply: We revised, see the new Fig. 4, line 293.
Comment 6: Figure 1 and throughout the manuscript: The m/z values and concentration values must report the same correct number of significant figures.
Reply: We revised, see the new Fig. 4, line 293 and markup section.
Comment 7: “m/z” and “k” should be italic. Line 239: “SO4-”should be “·SO4-”; Line 269:“5.24.6.07” should be “5.24, 6.07”. Authors should also carefully check and correct other typos and grammar errors that are not listed here.
Reply: We revised, for “·SO4-”, see new line 286, for “5.24, 6.07”, see new line 314, and we also checked the full text and made changes, as detailed in the markup revised section.
-
AC1: 'Reply on RC1', Ping Liu, 27 Mar 2024
-
RC2: 'Comment on amt-2023-250', Anonymous Referee #2, 03 Mar 2024
General Comments:
This manuscript uses Hydrophilic Interaction Liquid Chromatography (HILIC) to analyze isoprene-derived organosulfates in the Pearl River Delta. The results show that the relative error is extremely small, the experimental reproducibility is high, the analysis procedure is stable, and the results are reliable. The research content aligns with the publication scope of the Atmospheric Measurement Techniques journal, and publication is recommended after revisions.
Specific Comments:
1) The full name of the abbreviations should be given at the first time the abbreviations appear. For example, “OSs” in Line 31, “ACN” in Line 114, etc.
2) Some figures and tables in the manuscript have not been referenced in the text, such as Table 3 and Figure 1. All figures and tables should be cited and introduced in the text.
3) Line 269: the dot between “5.24” and “6.07” should be a comma.
4) Line 289: the comma in this line should be a dot.
5) In Table 9, the column “retention time” is sometimes aligned with “daytime” and sometimes positioned between “daytime” and “nighttime”. Is this a formatting issue? If not, it should be explained in the manuscript.
Citation: https://doi.org/10.5194/amt-2023-250-RC2 -
AC2: 'Reply on RC2', Ping Liu, 27 Mar 2024
We greatly appreciate the time and effort you dedicated to thoroughly reviewing our manuscript. We have carefully considered each point and have made revisions accordingly. We believe that your input has significantly improved the manuscript. Below are our responses to each comment.
Comment 1: The full name of the abbreviations should be given at the first time the abbreviations appear. For example, “OSs” in Line 31, “ACN” in Line 114, etc.
Reply: We revised, see new lines 28 and 115, and we also checked the full text, see revision with markup for more details.
Comment 2: Some figures and tables in the manuscript have not been referenced in the text, such as Table 3 and Figure 1. All figures and tables should be cited and introduced in the text.
Reply: We revised, see new lines 213-216 and 290-292.
Comment 3: Line 269: the dot between “5.24” and “6.07” should be a comma.
Reply: We revised, see new line 314.
Comment 4: Line 289: the comma in this line should be a dot.
Reply: We revised, see new line 333.
Comment 5: In Table 9, the column “retention time” is sometimes aligned with “daytime” and sometimes positioned between “daytime” and “nighttime”. Is this a formatting issue? If not, it should be explained in the manuscript.
Reply: We are sorry, it's a formatting issue. We revised it, see new Table 10.
Citation: https://doi.org/10.5194/amt-2023-250-AC2
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AC2: 'Reply on RC2', Ping Liu, 27 Mar 2024
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