I would wash with water then the solvent the column is going to be run in as per:

http://www.dow.com/assets/attachments/business/process_chemicals/amberlite_xad/amberlite_xad4/tds/amberlite_xad4.pdf

As is is essentially a polymeric reverse phase, I wash with methanol (or whatever I use to elute my compound) followed by water or the solvent system I'll initially use in the column. This is in accordance with the procedure link in Dr. Levison's post above.

Thank you! I don't need to let it swell overnight or anything that normally you do with packing your own columns? Also, how do I know how much to add if my column is 2.5x15cm? 

I usually didn't, but please note the link Bruce posted, where I read it can swell 20% when washed with the organic solvent; it probably takes some time. I let it sit an hour or two. I would do the solvent wash outside of a column.

It depends how clean should be your resin. When we needed it for accurate measurements and fine experiments we simply put XAD-2 resin in 250 x 10 mm stainless steel column or bigger, then put this column in HPLC instrument and wash with methanol at low flow rate until stable base line at 254 nm on UV detector. It took for a while to get a stable baseline.

Add the resin as a slurry in water.  Fill the column to only 50 - 60%, to allow room for backwash.  Drain water level to 2 - 5 cm above the top of the bed. Start by backwashing the resin, to remove air pockets and any fines.  To do so, pump water from bottom to top at a rate sufficient to expand the bed.(see Figure 4 of the link Bruce sent).  Allow the bed to expand to the top of the column, then stop water flow, allow the bed to resettle, then again drain until the level is 2 - 5 cm above the top of the bed. Next rinse with ethanol (or other suitable polar solvent) for 90 minutes at 2 - 2.5 bed volumes (BV) per hr (top to bottom).  Displace the ethanol with water (30 minutes, 2 - 2.5 BV/hr), then rinse with water for one hour at 8 - 10 BV/hr.  Repeat these steps twice (total of three), then do a final backwash.  Now your column is free of preservatives, residual monomer, fines and air pockets, and it's ready to go.

Add the resin as a slurry in water.  Fill the column to only 50 - 60%, to allow room for backwash.  Drain water level to 2 - 5 cm above the top of the bed. Start by backwashing the resin, to remove air pockets and any fines.  To do so, pump water from bottom to top at a rate sufficient to expand the bed.(see Figure 4 of the link Bruce sent).  Allow the bed to expand to the top of the column, then stop water flow, allow the bed to resettle, then again drain until the level is 2 - 5 cm above the top of the bed. Next rinse with ethanol (or other suitable polar solvent) for 90 minutes at 2 - 2.5 bed volumes (BV) per hr (top to bottom).  Displace the ethanol with water (30 minutes, 2 - 2.5 BV/hr), then rinse with water for one hour at 8 - 10 BV/hr.  Repeat these steps twice (total of three), then do a final backwash.  Now your column is free of preservatives, residual monomer, fines and air pockets, and it's ready to go.

for making resin slurry, how much solvent must be add to how many resin? it isn't important the slurry concentration?

It's not critical - about 10-15% is fine

Thank you a lot

I want to prepare Amberlite XAD-7 HP for measuring plant hormones. I can’t find any protocols about it. I bought it from sigma and it’s a powder. How can I prepare it?

Hi Leila

The comments I wrote previously on XAD-4 are applicable.  Also, take a look at this and let me know if you have any questions: http://msdssearch.dow.com/PublishedLiteratureDOWCOM/dh_08d2/0901b803808d2eff.pdf?filepath=liquidseps/pdfs/noreg/177-03082.pdf&fromPage=GetDoc

Regards

Alan

Thanks for attention and answer, but unfortunately your attached link doesn't work and browser in my computer showed below messages.

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Hi Leila

I have attached the document.

Regards

Alan

Thanks a lot, dear Alan

I have to prepare XAD7HP resin column for adsorption of fulvic acid. Can anyone guide me what should be the procedure for making column of XAD7HP?

Looking forward for a fruitful answer.

Thanks

Hi Jawad

take a look at this attached file.

Thanks a lot Leila Aslani for your support. I will go through it.

Thanks again.

Hi Leila Aslani

Do you have any idea that what solvent should be used to make solution of XAD7-HP to pack the column?

Thanks

You mean a slurry, not solution. Just use water.

Thanks Alan Gabelman for your guidance. in our methodology they didn't explain the detail about "how should use the resin dry or wet? but i saw most of the people used it in solution or make slurry. so im confused that what should i do.

if you can guide me in this regard, my problem will be solved.

Thanks

Jawad

This procedure is for a 25 mm diameter x 70 cm tall column. You should adjust the amounts and bed height for whatever size column you're using. Leave about 1/3-1/2 of the column height as headspace to allow for expansion during backwash.

1.1. Open the stopcock at the bottom of the column, and place a 500 mL beaker (or other suitable container) underneath.

1.2. In another 500 mL beaker, prepare about 250 mL of a slurry of 10 – 15% v/v hydrophobic resin in water.

1.3. Using a spatula or glass rod, mix the slurry to uniformly suspend the resin, then immediately pour the slurry into the top of the column. Allow the column to drain.

1.4. Prepare additional slurry, then again transfer to the column and allow the column to drain.

1.5. Repeat step 1.4 until the bed height is 48 – 50 cm, but do not allow the column to drain completely. Close the stopcock when the liquid level is 2 – 4 cm above the top of the bed.

Thanks a lot Alan Gabelman for your detailed guidance. Definitely, this will help me a lot.

Regards

Hi all especially Alan Gabelman. Can anyone guide me that;

1. For how much long/how many times we can use the resin in a column?

2. From which indicators we can assure that resin is fit for use?

3.What is meant by enrichment zone of resin in adsorption process?

Thanks in advance.

Jawad

1. There is no set number or length of time. Most resins last many adsorption/elution cycles, typically for a period of years. Usually the end of the useful life of the resin is indicated by a deterioration in performance. In some cases this is due to fouling, which may be reversible with aggressive cleaning. Another problem may be attrition, i.e., breakup of resin particles into fines.

2. It's fit for use if the resin performance meets your process objectives. These usually include selectivity, capacity, ease of regeneration, repeatability and cost. That is, does the resin adsorb what you want to keep and reject what you don't want? Is the capacity (expressed different ways, e.g., mg/kg of resin) sufficient? Can the resin be regenerated in an economical way, or are the adsorbates too tightly held?

3. I think you mean "mass transfer zone." For an explanation of this concept, take a look at the attached article.

Hope this helps,

Alan

Soak in methanol to wet up the resin. Then rinse with distilled water to remove the methanol. These is most easily done in a large beaker (4L) in bulk mode. Then load the resin into your column and acidify with dilute HCl (8 ml in total 1L). Measure the pH of the effluent. When pH of effluent = pH of influent start rising away the excess acid with DI H2O. when the electrical conductivity of the effluent = EC of the influent you have remove the excess acid. The resin is now ready. You will desorb the XAD-4 resin acids with 0.1M NaOH or KOH. So to regenerate wash the resin with DI H2O to remove and NAOH/KOH then repeat the treatment process (no need to treat with methanol again).

When displacing water with a solvent such as ethanol, methanol, isopropanol or acetonitrile, the solvent is introduced at the top of the column, and effluent removed from the bottom. The solvent chases out the water in a nearly plug flow manner (although some back-mixing does occur). When displacing solvent with water, the displacement is more efficient (less back-mixing) if the heavier water is introduced at the bottom. However, allowing for both feed and effluent at each end of the column is complicated in an industrial setting, requiring more valves and complex piping. For this reason, typically water is introduced at the top also, and the greater back-mixing (leading to longer time for displacement) is accepted.

Alan,

Our procedure indicates to rinse the Amberlite with water until conductivity of the eluent is less than 2 μS/cm. The water we are using does not have a conductivity that low even though it is USP grade. Will this harm the performance of the Amberlite.

No you're fine

Alan Gabelman Our contractor mentioned that this might impact the efficiency of the Amberlite to remove small molecules and thus result in having to run the column twice. Do you have any experience with this?

I have not run into that, but if you describe what you're trying to do in as much detail as possible (specific resin, column diameter, bed height, approximate composition of feed, target molecule(s)), and also share any additional info on your contractor's concern, I may be able to comment further

Cary see this paper and references therein for good info on the use of XAD-4 resin. It would be nice to know what purpose you are using it for.

Malcolm, R. L., & MacCarthy, P. (1992). Quantitative evaluation of XAD-8 and XAD-4 resins used in tandem for removing organic solutes from water. Environment International, 18(6), 597–607.doi:10.1016/0160-4120(92)90027-2 

Richard and Alan,

The amberlite we are using is IR120 Na form. We are preparing in water and rinsing until conductivity is reduced. The column is used to remove small molecules from a polymer preparation. We have used this for a 400 g column and are now scaling up to a 4000 g column. Our initial use indicates that if you soak the column in water, then the conductivity will reduce more quickly. Do either of you have experience with this? At this point we are using large volumes of water and still not getting conductivity measurements that we desire.

To be clear, do you mean soak or rinse? Rinsing is better. I assume you're referring to reducing the conductivity after each regeneration. At the end of regeneration, rinse with two bed volumes of water at two bed volumes per hour, then continue at 10 bed volumes per hour until your conductivity target is reached ( usually 5-10 bed volumes, but could be more). Of course the conductivity of the water you're using matters. Usually deionized water (by RO or softening resin) is sufficient, but if you have a particularly low conductivity requirement, you may need to use distilled water. Piping and vessel materials may also matter. Deionized water should be handled using glass or polymeric materials, not metal. The same may also be needed for your polymer product.

Alan,

I really appreciate your input. I will check with the speed at which they are rinsing the column. It is possible that they are moving too fast. My chemist found that after he let the column sit overnight in water that the conductivity came down faster. That is what I was referring to with 'soaking'.

Kind Regards, Cary

I may have missed a switch in this discussion. But, the original question was about prep of an XAD-4 resin. You now say you are using an IR 120 Na form resin which is a cation exchange resin. The prep and regeneration of these two resins is totally different. Which resin are you interested in?