The details of how to measure degree of hydration with TGA in cementitious materials are given in this recently-published book:

Scrivener, K., Snellings, R. and Lothenbach, B. eds., 2016. A Practical Guide to Microstructural Analysis of Cementitious Materials. Crc Press.

We are using TGA and isothermal calorimetry also on mortars. If you want to measure on concrete, TGA will be problematic because of the large amount of aggregates (it "dilutes" the mass loss) and the difficulty of obtaining a representative sample - you would need to crush the whole concrete including the coarse aggregates.

Isothermal calorimetry could be used (with some loss of accuracy) if you have a large cell (some calorimeters have it). We managed to do measurements in concrete/mortars with up to 8 mm aggregate size in a TAM Air calorimeter.

Using image analysis might be close to impossible on concrete. You will have to analyze a huge number of high-resolution images and the presence of aggregates will complicate the segmentation of the unhydrated cement.

This is a very interesting discussion topic, perhaps some good ideas will emerge from this forum!

The details of how to measure degree of hydration with TGA in cementitious materials are given in this recently-published book:

Scrivener, K., Snellings, R. and Lothenbach, B. eds., 2016. A Practical Guide to Microstructural Analysis of Cementitious Materials. Crc Press.

We are using TGA and isothermal calorimetry also on mortars. If you want to measure on concrete, TGA will be problematic because of the large amount of aggregates (it "dilutes" the mass loss) and the difficulty of obtaining a representative sample - you would need to crush the whole concrete including the coarse aggregates.

Isothermal calorimetry could be used (with some loss of accuracy) if you have a large cell (some calorimeters have it). We managed to do measurements in concrete/mortars with up to 8 mm aggregate size in a TAM Air calorimeter.

Using image analysis might be close to impossible on concrete. You will have to analyze a huge number of high-resolution images and the presence of aggregates will complicate the segmentation of the unhydrated cement.

This is a very interesting discussion topic, perhaps some good ideas will emerge from this forum!

I do not test cement concret materials

Degree of hydration can be tested with the help of shrinkage and concrete electrical resistivity meter

If you are trying to correlate degree of hydration with the strength development, it may not give you the correct results. As there are many phases which bind high amount of water but don't contribute to the strength, though they are the products of cement hydration, like AFt and AFm phases. The best is to combine TGA with XRD quantitative analysis. the first mass loss between 50 to ~250 is for CSH, Gypsum, AFm and AFt phases. Quantify Gypsum, AFm and AFt phases with the help of XRD, work out the chemically bound water and deduct it from the mass loss 50 to ~250 range. Similarly, you can compare portlandite and calcite contents separately, among your various mix designs.

I agree with Pietro Lura's suggestion, about Karen Scrivener's book. Their group has done quite impressive work on cementitious materials using various techniques, like TGA, XRD, image analysis etc 

A considerably more simple method,  less precise though, is the measurement of the water bound until~600°C, it should give you good semi-quantitative indication of the degree of hydration and you can use bigger /and more representative concrete sample: you quantify most of the binding water hydrates without decarbonating eventual limestone filler or aggregates.

The mentioned book is a reference that you can follow!

degree of hydration is usually centered on calcium hydroxide generation from cement. Sometimes i think there is little emphasis on other products such as CSH and CASH, AFm and AFt. if the hydration process is extended beyond CaOH2 generation trends, then I think one can use solid state Al and Si Nuclear Magnetic Resonance (NMR). It is gaining grounds slowly even though the determination processes is time consuming using the equipment. I also agree with Mishra that shrinkage(total and autogeneous) could be explored to know the hydration behavior

good papers on degree of hydration ?

Hi Siraj,

You can get detailed methodology in the following papers:

"A quantitative study on the effect of nano SiO2, nano Al2O3 and nano CaCO3 on the physicochemical properties of very high volume fly ash cement composite"

"Micro and Nano Engineered High Volume Ultrafine Fly Ash Cement Composite with and without Additives"

Feel free to contact me if you have any query