Out: 220 xx ESMTP
In:  EHLO yy
Out: 250-xx
Out: 250-SIZE 1024000000
Out: 250-VRFY
Out: 250-ETRN
Out: 250 8BITMIME
In:  MAIL FROM:<a at b.com 
<http://lists.freebsd.org/mailman/listinfo/freebsd-questions>> SIZE=13414
Out: 452 Insufficient system storage
Out: 221 Bye

Okay, so the disk is filling up.

This happens, if there's less than 2*message_size_limit free space on /var/mail. Check /var/log/mail

box# df -hl
Filesystem    Size   Used  Avail Capacity  Mounted on
/dev/ar0s1a  1008M    45M   882M     5%    /
/dev/ar0s1d    27G    23G   1.9G    92%    /jails
/dev/ar0s1h  1008M    20M   908M     2%    /home
/dev/ar0s1g  1008M  10.0K   927M     0%    /tmp
/dev/ar0s1f   3.9G   1.2G   2.4G    34%    /usr
/dev/ar0s1e   2.0G   148M   1.7G     8%    /var
procfs        4.0K   4.0K     0B   100%    /proc
procfs        4.0K   4.0K     0B   100%    /jails/xxx/proc

Okay, we are at 92%. We should clean some things up, but we do still have
1.9GB of free space. (And we often linger around this anyway.)

Postfix is set to accept mail as long as there is 25MB of free space:

main.cf:queue_minfree = 25000000

That doesn't matter. Check your main.cf. What message_size_limit have you defined? I guess, your /var is getting temporarly quit full due to some cronjobs e.g. backup-scripts which need a lot of temp-space to zip big directories like /home.

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