In general no, the volume is not conserved. To take an extreme example, consider a shell of particles surrounding the Earth. As they freely fall, their volume will definitely decrease!
EDIT: my example is extreme, of course. Baez at https://math.ucr.edu/home/baez/einstein/node5.html points out that the volume of a "small" sphere of test particles in vacuum does not change, and I'm sure he's right about that. But in my example there's a mass at the center, so the whole volume is not in vacuum.
EDIT: to put some numbers on this, I'll calculate the volume of a 1 km thick shell falling near the Earth's surface (so the inner radius is about the same as Earth's radius, 6372000 meters, and the outer radius is 6373000 meters). Near Earth's surface Newton's equations are an excellent approximation for gravity, so the radius of a falling shell as a function of time is given by the differential equation $r'' = \frac{GM}{r^2}$, where $GM$ is approximately $4 \times 10^{14} m^3 / s^2$ for Earth. Unfortunately there isn't a nice closed form solution for this equation, but we can solve it numerically using Wolfram Alpha with something like
solve [y'' + (4*10^14) / (y-6372000)^2 = 0, y(0)=0, y'(0)=0] from 0 to 10 using r k f
That is for the inner surface of the shell, and gives a delta of -492.569, which is reasonable (we know gravitational acceleration is about 9.8 m/s^2 near earth's surface, so we expect an answer near 490 m for a 10 second fall).
Doing the same for the outer surface gives a delta of -492.415, which again is reasonable (it falls slightly less because it starts further away).
Finally, calculating the volumes gives us a starting volume of
$4/3 * \pi * 1.21826269 * 10^{17}$ and a final volume (after 10 seconds) of $4/3 * \pi * 1.21826197641753715846882634 * 10^{17}$, so the volume of the shell has indeed decreased as expected.