Analysis

Overview

You can use the ZIF Phase Analysis app to analyse the X-ray diffraction (PXRD) data from your sample.

There ZIF Phase Analysis app provides with two alternative analyses. The two analyses have two different purposes, require two different types of samples and call for different inputs from the user.

Multi-phase analysis

• Purpose: to quantify the relative amount of the phases (e.g. sodalite, diamondoid, ZIF-CO3-1, ZIF-EC-1, U12 and/or ZIF-L) that are likely to be present in the studied sample
• Sample: an internal standard is NOT required
• User Input: the user can select the desired range of 2θ values for analysis; we recommend using the 6°-28° range as it includes all the reference peaks of the detectable crystal phases (the entire 6°-39° range should be used if ZrO2 and/or ZnO are of interest as well)

Single-phase analysis

• Purpose: to estimate the percentage of crystalline and amorphous material present in the studied sample (currently, only one phase can be investigated at a time)
• Sample: a sample with a constant amount of ZrO2 as internal standard (i.e. sample/internal standard mixture) is required; see “Preparation of ZIF-based sample with internal standard” below
• User Input: the user is required to indicate:
  1. the crystalline phase to study;
  2. the weight proportion of the ZIF-based material in the sample/internal standard mixture.

NOTE: Accuracy depends on the precision used for the preparation of the sample/internal standard mixture and calibrations. Thus, we recommend to double-check your results if you are using this app for the first time.

Preparation of ZIF-based sample with internal standard

The single-phase analysis requires the investigated sample to contain a constant amount of an internal standard. This results in a sample/internal standard mixture.

The internal standard to use is ZrO2. ZrO2 was purchased from Sigma Aldrich (powder, 5 µm, 99 % trace metal basis, product number: 230693).

To prepare the sample/internal standard mixture, the following procedure is required: 5 mg of ZrO2 powder are suspended in 150 µl de-ionised water, sonicated for 15 minutes and added to 5 mg of ZIF-based sample.¹ The suspension is vortexed for 1 minute to ensure a homogeneous mixture. From the suspension mixture 50 µl are drop-cast on a 1,5 cm x 1,5 cm piece of Si and air-dried for 48 h at room temperature (23° C). Triplicates should be made from the same mixture.

The detailed procedure can be found here: https://doi.org/10.1039/D2CE00073C

If you use the app, please cite us

We have invested time and effort in the ZIF Phase Analysis app. Your citation to our paper (https://doi.org/10.1039/D2CE00073C) means a lot to us.