XAD-8 & XAD-4
Resin Cleaning Procedure (New Resin)
* This procedure is for cleaning new XAD-8 and XAD-4 resin which is often stored in methanol
Supplies needed
 1 L erlenmeyer flasks
 ~ 0.1 N NaOH (enough to match the amount of resin to be cleaned)
Procedure
1) Rinse resin several times with hot deionized water (~60 oC) to drive off methanol
2) Place resin in a 1 L flask
3) Add 0.1 N NaOH in excess, swirl and let sit for at least 12 hours.
4) Swirl and decant NaOH
 Allow fines to be decanted since you want to end up with a uniform range of resin size
5) Add fresh NaOH and repeat procedure 3 & 4 for at least 3 days (six decants)
6) Decant NaOH and rinse with MQ water several times
7) Store in MQ water
Resin Cleaning Procedure (Used Resin)
* This procedure is for cleaning used XAD-8 and XAD-4 resin
* If resin is dried out, discard and do not clean
Equipment & Supplies needed
 2 – 1 L erlenmeyer flasks
 Methanol (HPLC grade)
 Acetonitrile (HPLC grade)
 Cleaning apparatus
(Soxhlet extractor)
Condenser
Clamp 1
Resin cleaning vessel
Clamp 2
Resin holding sleeve
Cleaning agent holding vessel
Heater
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Figure 1
Cleaning Procedure
1) Remove any contaminants and resin that is of the other kind (this can also be done after
cleaning)
2) If resin has significant sorbed humic substances (brown color), wash with 0.1 N NaOH.
3) Loosen “Clamp 1”, raise the “Condenser”, re-clamp
4) Loosen “Clamp 2” and remove “Resin Cleaning Vessel”
5) Fill “Cleaning Agent Holding Vessel” with methanol to just below the white oval (Figure 2)
Fill line
Figure 2
6) Clean “Resin Cleaning Vessel” and “Resin Holding Vessel” with methanol squirt bottle.
7) Transfer resin to “Resin Holding Thimble” Check resin level by inserting “Resin Holding
Thimble” into the “Resin Cleaning Vessel”. Do not fill the “Resin Holding Thimble” so
level is above bubble in glass (Figure 3).
8) Rinse “Resin Holding Thimble” 2-3 times with methanol squirt bottle and reinsert.
Liquid fill line
Max. resin fill line
Resin holding sleeve
Overflow/siphon
tube
Cleaning agent holding vessel
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Figure 3
9) Reassemble “Cleaning Agent Holding Vessel”, “Resin Cleaning Vessel” and “Condenser”
Make sure the seals are a tight fit.
10) Make sure water is running through the “Condenser”. This should be at a low flow rate to
conserve water. The flow may change slightly after a few minutes, so be sure to recheck it.
11) Turn heater to 3.5-4.0 units and wait 10 min. for methanol to be heated
12) Adjust heat so drip rate out of the “Condenser” is ~1 drop/sec.
13) Make sure methanol rises up to the “Liquid fill line”, thus saturating the resin (Figure 3).
The liquid level of methanol should be at the top of the overflow/siphon tube. If this does
not occur, see if the methanol is condensing in the top corners of the “Resin Cleaning
Vessel” and dripping down the larger outside tube. If it is, rotate the setup so the methanol
misses the outside tube as it drips down the side.
14) Clean with methanol for at least 48 hours
15) Discard methanol at end of cleaning
16) Repeat steps 2 – 14 with acetonitrile instead of methanol
17) Rinse resin in “resin holding vessel” several times with MQ
18) Transfer resin to an erlenmeyer flask and rinse several times with hot MQ water (~60 oC)
19) Store cleaned resin in MQ water
20) Wash resin cleaning apparatus with methanol to prepare for next run
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