Best practices for precipitation sample storage for offline studies of ice nucleation in marine and coastal environments

Ice-nucleating particles (INPs) are efficiently removed from clouds through precipitation, a convenience of nature for the study of these very rare particles that influence multiple climate-relevant cloud properties including ice crystal concentrations, size distributions and phase-partitioning processes. INPs suspended in precipitation can be used to estimate in-cloud INP concentrations and to infer their original composition. Offline droplet assays are commonly used to measure INP concentrations in precipitation samples. Heat and filtration treatments are also used to probe INP composition and size ranges. Many previous studies report storing samples prior to INP analyses, but little is known about the effects of storage on INP concentration or their sensitivity to treatments. Here, through a study of 15 precipitation samples collected at a coastal location in La Jolla, CA, USA, we found INP concentration changes up to > 1 order of magnitude caused by storage to concentrations of INPs with warm to moderate freezing temperatures (−7 to −19 ∘C). We compared four conditions: (1) storage at room temperature (+21–23 ∘C), (2) storage at +4 ∘C, (3) storage at −20 ∘C and (4) flash-freezing samples with liquid nitrogen prior to storage at −20 ∘C. Results demonstrate that storage can lead to both enhancements and losses of greater than 1 order of magnitude, with non-heat-labile INPs being generally less sensitive to storage regime, but significant losses of INPs smaller than 0.45 µm in all tested storage protocols. Correlations between total storage time (1–166 d) and changes in INP concentrations were weak across sampling protocols, with the exception of INPs with freezing temperatures ≥ −9 ∘C in samples stored at room temperature. We provide the following recommendations for preservation of precipitation samples from coastal or marine environments intended for INP analysis: that samples be stored at −20 ∘C to minimize storage artifacts, that changes due to storage are likely an additional uncertainty in INP concentrations, and that filtration treatments be applied only to fresh samples. At the freezing temperature −11 ∘C, average INP concentration losses of 51 %, 74 %, 16 % and 41 % were observed for untreated samples stored using the room temperature, +4, −20 ∘C, and flash-frozen protocols, respectively. Finally, the estimated uncertainties associated with the four storage protocols are provided for untreated, heat-treated and filtered samples for INPs between −9 and −17 ∘C.

Best practices for precipitation sample storage for offline studies of ice nucleation

Ice nucleating particles (INPs) are efficiently removed from clouds through precipitation, a convenience of nature for the study of these very rare particles that influence multiple climate-relevant cloud properties including ice crystal concentrations, size distributions, and phase-partitioning processes. INPs suspended in precipitation can be used to estimate in-cloud INP concentrations and to infer their original composition. Offline droplet assays are commonly used to measure INP concentrations in precipitation samples. Heat and filtration treatments are also used to probe INP composition and size ranges. Many previous studies report storing samples prior to INP analyses, but little is known about the effects of storage on INP concentration or their sensitivity to treatments. Here, through a study of 15 precipitation samples collected at a coastal location in La Jolla, CA, USA, we found significant changes caused by storage to concentrations of INPs with warm to moderate freezing temperatures (−7 to −19 ºC). We compared four conditions: 1.) storage at room temperature (+21–23 ºC), 2.) storage at +4 ºC 3.) storage at −20 ºC, and 4.) flash freezing samples with liquid nitrogen prior to storage at −20 ºC. Results demonstrate that storage can lead to both enhancements and losses of greater than one order of magnitude, with non-heat-labile INPs being generally less sensitive to storage regime, but significant losses of INPs smaller than 0.45 μm in all tested storage protocols. No correlation was found between total storage time (1–166 days) and changes in INP concentration. We provide the following recommendations for preservation of precipitation samples from coastal environments intended for INP analysis: that samples be stored at −20 ºC to minimize storage artifacts, that changes due to storage are likely and an additional uncertainty in INP concentrations, and that filtration treatments be applied only to fresh samples. Average INP losses of 72 %, 42 %, 25 % and 32 % were observed for untreated samples stored using the room temperature, +4 ºC, −20 ºC, and flash frozen protocols, respectively. Finally, correction factors are provided so that INP measurements obtained from stored samples may be used to estimate concentrations in fresh samples.

UNCERTAINTY ASSESSMENT AND QUALITY CONTROL FOR ENVIROMENTAL MEASUREMENTS OF TRITIUM IN WATER SAMPLES

The main aim of this paper was to evaluate uncertainty for low level tritium measurements in monthly precipitation collected at PC NFS site and to clarify quality control procedures which provide reasonable assurance that the analytic results obtained are valid and accurate. Determination of tritium concentration in precipitation sample was conducted using liquid scintillation counter Quantulus 1220. The most important sources of uncertainty are discussed. Four different internal quality control methods have been presented and explained in detail.

Freezing nucleation apparatus puts new slant on study of biological ice nucleators in precipitation

For decades, drop-freezing instruments have contributed to a better understanding of biological ice nucleation and its likely implications for cloud and precipitation development. Yet, current instruments have limitations. Drops analysed on a cold stage are subject to evaporation and potential contamination. The use of closed tubes provides a partial solution to these problems, but freezing events are still difficult to be clearly detected. Here, we present a new apparatus where freezing in closed tubes is detected automatically by a change in light transmission upon ice development, caused by the formation of air bubbles and crystal facets that scatter light. Risks of contamination and introduction of biases linked to detecting the freezing temperature of a sample are then minimized. To illustrate the performance of the new apparatus we show initial results of two assays with snow samples. In one, we repeatedly analysed the sample (208 tubes) over the course of a month with storage at +4 °C, during which evidence for biological ice nucleation activity emerged through an increase in the number of ice nucleators active around −4 °C. In the second assay, we indicate the possibility of increasingly isolating a single ice nucleator from a precipitation sample, potentially determining the nature of a particle responsible for a nucleation activity measured directly in the sample. These two seminal approaches highlight the relevance of this handy apparatus for providing new points of view in biological ice nucleation research.