Not sure what's up with your code. Here's some code borrowed from Tushar Meta for 1D array..
Function StdDev(Arr)
Dim i As Integer
Dim avg As Single, SumSq As Single
Dim k1 As Long, k2 As Long
Dim n As Long
k1 = LBound(Arr)
k2 = UBound(Arr)
n = 0
avg = Mean(Arr)
For i = k1 To k2
n = n + 1
SumSq = SumSq + (Arr(i) - avg) ^ 2
Next i
StdDev = Sqr(SumSq / (n - 1))
End Function
You could trial it like this...
For i = 1 To 5
subsetStDev(i) = StdDev(subsets(i))
' Output standard deviation to Immediate Window for debugging
Debug.Print "Subset " & i & " Standard Deviation: " & subsetStDev(i)
Next i
Good luck. Dave