# Characterizing a new MOF

> A new framework is only as good as its evidence. Solvent has to leave the pores without the crystal collapsing; then the powder pattern shows the bulk is the phase solved from the crystal structure, a nitrogen isotherm at 77 K shows the pores are open (a type I curve for a microporous MOF, with the BET area taken from the low-pressure range that meets the consistency criteria), and thermogravimetry shows the composition. Drawn here for UiO-66.

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- Open in the LabCanvas editor (LabCanvas account): https://www.labcanvas.com/editor.html?template=mof-characterization
- Updated: 2026-10-14
- Category: Metal–organic frameworks
- Method: Characterization, bottom-up
- Starting materials: An as-made MOF with solvent in its pores (here UiO-66, made in DMF)
- Product: An activated, characterized framework: phase purity, porosity and composition
- Key result: Report what supports permanent porosity: PXRD after activation, the isotherm with its BET range, and TGA
- Figure: 1920 × 1080 px, 75 editable layers (10 generated objects with settings)

## Steps

1. **Solvent exchange**: High-boiling synthesis solvent (DMF) replaced by a volatile one over several soaks
2. **Activation**: Solvent removed by heating under vacuum, or by supercritical CO₂ drying for fragile frameworks (Howarth et al. 2017)
3. **PXRD**: Measured powder pattern compared with the one calculated from the crystal structure; UiO-66: 111 at 7.4°, 200 at 8.5° 2θ (Cu Kα)
4. **N₂ at 77 K**: Type I isotherm for micropores; BET area from the low-pressure range that meets the consistency criteria (Walton & Snurr 2007; Thommes et al. 2015)
5. **TGA**: In air: solvent loss, then the linkers burn to ZrO₂; for Zr₆O₆(BDC)₆ the plateau is 2.20 × the residue

## Strengths

- Three quick measurements cover structure, porosity and composition
- Calculated patterns and formula masses make the checks quantitative

## Limitations

- BET areas of microporous MOFs depend on the pressure range chosen
- Collapse on activation can hide behind a good as-made pattern

## Uses

- Any new or newly made MOF
- Batch-to-batch quality control

## References

1. Howarth et al., “Best Practices for the Synthesis, Activation, and Characterization of Metal–Organic Frameworks”, Chem. Mater. 2017. https://doi.org/10.1021/acs.chemmater.6b02626 (review)
2. Thommes et al., “Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report)”, Pure Appl. Chem. 2015. https://doi.org/10.1515/pac-2014-1117 (method origin)
3. Walton & Snurr, “Applicability of the BET Method for Determining Surface Areas of Microporous Metal−Organic Frameworks”, J. Am. Chem. Soc. 2007. https://doi.org/10.1021/ja071174k (further reading)
4. Valenzano et al., “Disclosing the Complex Structure of UiO-66 Metal Organic Framework: A Synergic Combination of Experiment and Theory”, Chem. Mater. 2011. https://doi.org/10.1021/cm1022882 (further reading)

Credit: After Howarth et al., Chem. Mater. 2017 (doi:10.1021/acs.chemmater.6b02626), Thommes et al., Pure Appl. Chem. 2015 (doi:10.1515/pac-2014-1117) and Walton & Snurr, JACS 2007 (doi:10.1021/ja071174k). Pattern computed; isotherm and TGA schematic.

## Questions

**What does the “Characterizing a new MOF” template show?** A new framework is only as good as its evidence. Solvent has to leave the pores without the crystal collapsing; then the powder pattern shows the bulk is the phase solved from the crystal structure, a nitrogen isotherm at 77 K shows the pores are open (a type I curve for a microporous MOF, with the BET area taken from the low-pressure range that meets the consistency criteria), and thermogravimetry shows the composition. Drawn here for UiO-66.

**What are the steps shown in “Characterizing a new MOF”?** 1. Solvent exchange: High-boiling synthesis solvent (DMF) replaced by a volatile one over several soaks. 2. Activation: Solvent removed by heating under vacuum, or by supercritical CO₂ drying for fragile frameworks (Howarth et al. 2017). 3. PXRD: Measured powder pattern compared with the one calculated from the crystal structure; UiO-66: 111 at 7.4°, 200 at 8.5° 2θ (Cu Kα). 4. N₂ at 77 K: Type I isotherm for micropores; BET area from the low-pressure range that meets the consistency criteria (Walton & Snurr 2007; Thommes et al. 2015). 5. TGA: In air: solvent loss, then the linkers burn to ZrO₂; for Zr₆O₆(BDC)₆ the plateau is 2.20 × the residue.

**What are the starting materials and the product?** Starting materials: An as-made MOF with solvent in its pores (here UiO-66, made in DMF). Product: An activated, characterized framework: phase purity, porosity and composition.

**Which papers is “Characterizing a new MOF” based on?** Howarth et al., “Best Practices for the Synthesis, Activation, and Characterization of Metal–Organic Frameworks”, Chem. Mater. 2017 (doi:10.1021/acs.chemmater.6b02626); Thommes et al., “Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report)”, Pure Appl. Chem. 2015 (doi:10.1515/pac-2014-1117); Walton & Snurr, “Applicability of the BET Method for Determining Surface Areas of Microporous Metal−Organic Frameworks”, J. Am. Chem. Soc. 2007 (doi:10.1021/ja071174k); Valenzano et al., “Disclosing the Complex Structure of UiO-66 Metal Organic Framework: A Synergic Combination of Experiment and Theory”, Chem. Mater. 2011 (doi:10.1021/cm1022882).

**Can I edit the “Characterizing a new MOF” template?** Yes. Open it in the LabCanvas editor: all 75 layers are editable, including 10 generated objects (structures, plots, equipment) with their own settings. Change the text, colours and layout, then export PNG, TIFF, SVG or PDF.

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